CN106746101A - A kind of processing method of ethylene waste lye - Google Patents
A kind of processing method of ethylene waste lye Download PDFInfo
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- CN106746101A CN106746101A CN201510800994.XA CN201510800994A CN106746101A CN 106746101 A CN106746101 A CN 106746101A CN 201510800994 A CN201510800994 A CN 201510800994A CN 106746101 A CN106746101 A CN 106746101A
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Abstract
The invention discloses a kind of processing method of ethylene waste lye, including（1）Oil removal by air bubbling, removes entrained oil class material in ethylene waste lye；（2）High-temperature wet-oxidation treatment, the spent lye after oil removing carries out high-temperature wet-oxidation treatment；（3）Sulfuric acid treatment, to the concentrated sulfuric acid is added in the spent lye after being processed through high-temperature wet-oxidation, sulfate radical is completely converted into by hydroxyl and carbonate；（4）Charcoal absorption, the acid waste liquid after sulfuric acid treatment carries out charcoal absorption treatment；（5）Multiple-effect evaporation, to carrying out multiple-effect evaporation through the waste liquid after charcoal absorption, reclaims sodium sulfate crystal.The inventive method can efficiently remove the COD and sulfide in ethylene waste lye, the sodium sulphate of high-purity be reclaimed, so as to realize the zero-emission of ethylene waste lye.
Description
Technical field
The invention belongs to environment-protection wastewater processing technology field, and in particular to a kind of processing method of chemical plant ethylene waste lye.
Background technology
In ethylene production, at present generally using the CO in alkali wash removing cracking gas2、H2The sour gas such as S.Alkaline cleaning procedure generates substantial amounts of spent lye, in this kind of spent lye in addition to containing remaining NaOH, also contains the Na generated in alkaline cleaning procedure2S、Na2CO3Deng inorganic salts.On the other hand, due to the condensation of heavy constituent in cracking gas in alkaline cleaning procedure and diene hydro carbons, the polymerization of aldehyde material, substantial amounts of organic matter is entered in spent lye, increased the intractability of spent lye.Ethylene waste lye belongs to high concentrated organic wastewater, and COD, sulfide and salt content are high, and difficulty of governance is big.With the expansion of ethylene unit scale, spent lye discharge capacity is continuously increased, and its innoxious governance and comprehensive utilization have turned into the important topic that researcher pays close attention to.
According to the water quality characteristicses of ethylene waste lye, some patents propose processing method.CN201010526697.8 discloses a kind of method that sodium sulphate is reclaimed from waste alkali liquor of ethylene unit, after wet oxidation water outlet is carried out into neutralisation treatment, anhydrous sodium sulfate containing water entrainment is crystallized out from neutralizer using evaporative crystallization method, anhydrous sodium sulfate containing water entrainment is dried, obtain anhydrous sodium sulfate product, part evaporation mother liquor returns to neutralisation unit, the part chilled freezing mother liquor reclaimed after sal glauberi of evaporation mother liquor goes biochemical treatment, and the sal glauberi for being reclaimed returns to neutralisation unit.The method reduces the salt content in wet oxidation water outlet, it is to avoid the impact that the high-salt wastewater after being processed through wet oxidation process subsequent biochemical, while the sodium sulphate in recovery ethylene waste lye.But, COD contents are high during the step of evaporative crystallization one needs to consume substantial amounts of energy, and evaporation mother liquor, need to further be processed through biochemical process.
CN200510122185.4 discloses a kind of technique for reclaiming ethylene alkali-washing waste liquid, and its operating procedure is：Spent lye successively adds the materials such as supported solid flocculant, metal oxide therebetween by steps such as oil removing, causticization, desulfurization.The accessory substance that causticization and sweetening process are obtained, using sulfide conversion method by S2 -The sulfide of high added value is converted into, though the method simplifies ethylene waste lye processing procedure, reclaimed utility, whole process does not consider the removal to COD in ethylene waste lye, and introduces plurality of impurities, influences the recovery quality of spent lye.
CN201010205763.1 discloses a kind of method that high-temperature wet-oxidation processes spent lye, under 220 DEG C~260 DEG C with the pressure for making spent lye keep liquid phase, using inorganic sulphide and organic matter in the dioxygen oxidation spent lye in air.The method is to S2-Clearance reach the clearance of 100%, COD up to 75%~85%, but in its water outlet COD concentration in more than 20000mg/L, and containing substantial amounts of sodium salt, need to be allowed for access biochemical system after Macrodilution.
To sum up analyze, existed using current various methods treatment spent lye or improper or treatment effect is not enough or investment is big and operating cost is high or reclaims of low quality or needs for spent lye after treatment to drain into sewage disposal system, or the problems such as high slat-containing wastewater can be produced.
The content of the invention
The present invention in order to overcome the shortcomings of on existing ethylene waste lye treatment technology, and the characteristics of for ethylene waste lye, there is provided a kind of processing method of ethylene waste lye.The inventive method can efficiently remove the COD and sulfide in ethylene waste lye, reclaim sodium sulfate in high purity, realize the zero-emission of ethylene waste lye.
The processing method of ethylene waste lye of the present invention, comprises the following steps：
（1）Oil removal by air bubbling, removes entrained oil class material in ethylene waste lye；
（2）High-temperature wet-oxidation treatment, NaOH is added in the spent lye after oil removing, it is carried out high-temperature wet-oxidation treatment in the basic conditions；
（3）Sulfuric acid treatment, to the concentrated sulfuric acid is added in the spent lye after being processed through high-temperature wet-oxidation, sulfate radical is completely converted into by hydroxyl and carbonate；
（4）Charcoal absorption, the acid waste liquid after sulfuric acid treatment carries out charcoal absorption treatment；
（5）Multiple-effect evaporation, to carrying out multiple-effect evaporation through the waste liquid after charcoal absorption, reclaims sodium sulfate crystal.
In the present invention, step（1）Oil removal by air bubbling be to being passed through air in oily waste water, make to produce bubble in water, so that the oil being dispersed in water is bonded on bubble, is floated on the surface with gas and removed.Replace gravity oil-removing with oil removal by air bubbling, oil removal efficiency is greatly improved, the oil content after oil removal by air bubbling in spent lye is down to below 20mg/L, meet requirement of the high-temperature wet-oxidation technique for oil content of intaking.
In the present invention, sodium hydrate solid is added in the spent lye after oil removing.The addition of NaOH is that naoh concentration is 3.0wt%-4.0wt% in making the spent lye for enter high-temperature wet-oxidation treatment, whole wet oxidation reaction is carried out in the basic conditions, so as to imitate guarantee removal efficiency of the processing procedure for COD.When high-temperature wet-oxidation treatment, need to consume a certain amount of alkali while oxidation of organic compounds, while the acidic materials of generation can neutralize a certain amount of alkali；If alkali concn is too low, one side oxidation of organic compounds is not thorough, and on the other hand the acidic materials of generation can make the solution in reactor become acid, and corrosion is caused to reactor material.Suitable alkali concn not only makes the whole wet oxidation reaction carry out in the basic conditions, and can effectively be reclaimed in subsequent step, does not result in waste.
In the present invention, step（2）The middle reaction temperature for controlling high-temperature wet-oxidation is 240~320 DEG C, preferably 260~280℃；Reaction pressure is 6.0~20.0MPa, preferably 8.0~12.0MPa；Reaction time is 40~90 minutes.High-temperature wet-oxidation treatment can efficiently remove the sulfidion in spent lye（S2-）, organic pollution is oxidized to the materials such as small molecular organic acid, alcohol, significantly removes the COD in spent lye.S2-Clearance is up to more than 99.9%, water outlet S2-Concentration is less than 1mg/L, S2-Almost all is converted into SO4 2-, thoroughly, operating process will not produce the foul gas of pollution air for divalent oxidation.
In the present invention, step（3）According to carbonate in high-temperature wet-oxidation water outlet and concentration hydroxy, to the concentrated sulfuric acid that 98% is added in spent lye, the pH for controlling solution is 2~6.The concentrated sulfuric acid for adding can make NaOH and sodium carbonate in spent lye be completely converted into sodium sulphate, and in acid condition, small organic molecule in wet oxidation water outlet is easy to dissociate, large amount of organic exists in the form of cation, the oxy radical of activated carbon surface such as hydroxyl, carboxyl and carbonyl etc. all have stronger electrostatic adsorption to it, are favorably improved subsequent adsorbtion effect.During this, on the one hand carbanion clearance improves the concentration of sodium sulphate in solution up to more than 99% in solution, and the sodium sulphate of high concentration plays salting out to the small organic molecule in solution, increase organic matter equilibrium adsorption capacity on the activated carbon, improve the adsorption efficiency of activated carbon；On the other hand the sodium salt in solution can be made to be converted into single sodium sulphate, for the sodium sulphate for subsequently entering to reclaim high-purity provides advantage.
In the present invention, after spent lye after oil removing is through wet oxidation treatment and sulfuric acid acidification, wherein mainly containing sodium sulphate and small molecular organic acid class material, sodium sulfate concentration is up to more than 20wt%.Using the spent lye after the acidified treatment of charcoal absorption, due to the presence of solution middle and high concentration sodium sulphate, with very strong ionic strength, the interaction increase between ion and solvent can improve organic matter equilibrium adsorption capacity on the activated carbon.
In the present invention, step（4）Activated carbon used is wooden powder's shaped activated carbon, amounts of activated carbon is added in spent lye per ton for 5~15kg, after 0.2~1.0h of stirring mixing, through Filter Press, filtrate sends into follow-up multiple-effect evaporation unit, and the activated carbon isolated reuses to saturation state regeneration.
In the present invention, step（5）Multiple-effect evaporation may be selected 3~7 effect, evaporator selection falling film type.1st effective evaporator in multi-effect evaporator wherein generates indirect steam as thermal source after 2nd effect evaporator by the way of additional steam using previous effect evaporation, and the rest may be inferred.Sodium sulfate concentration is 60wt%~90wt% during multiple-effect evaporation controls solution, and sodium sulphate is obtained after the crystallized treatment of evaporation concentrated solution.
Compared with prior art, the inventive method has following prominent characteristics：
（1）The present invention removes the oily substance in spent lye first for the water quality characteristicses of ethylene waste lye, after then being processed through wet oxidation, then is acidified through sulfuric acid, most obtains the sulfate crystal of high-purity after charcoal absorption and multiple-effect evaporation afterwards.After treatment, the COD clearances of spent lye are up to more than 98%；S2-Clearance is up to more than 99.9%, S2-Oxidation is thorough, is almost completely converted into sulfate radical, and sulfide content is in below 1mg/L；And the foul odour of spent lye is stripped of completely, it is to avoid the atmosphere pollution such as hydrogen sulfide produced by being directly acidified to spent lye；COD can also be greatly lowered simultaneously.
（2）Spent lye carries out sulfuric acid treatment after being processed through wet oxidation, improves sodium sulfate concentration in solution, the efficiency of charcoal absorption organic matter is significantly improved, and reduces activated carbon usage amount.Meanwhile, the carbonate in spent lye is converted into sulfate radical, and the sulfate radical produced with wet oxidation treatment is in the lump for the sodium sulphate of subsequent recovery high-purity high-recovery provides advantage.
（3）By sodium sulfate concentration in multiple-effect evaporation raising solution, while small organic molecule remaining in solution after removal is processed through charcoal absorption, realizes that sodium sulphate is separated with other impurity substances, the sodium sulphate of high-purity can be reclaimed.
Brief description of the drawings
Fig. 1 is a kind of process chart of the inventive method；
Wherein：1- oil removal by air bubbling, the treatment of 2- high-temperature wet-oxidations, 3- sulfuric acid treatments, 4- charcoal absorptions, 5- multiple-effect evaporations.
Specific embodiment
Technical scheme is further illustrated by the following examples.In the present invention, wt% is mass fraction.
Embodiment 1
The spent lye produced in one ethylene production, wherein COD is 43000mg/L, and vulcanization na concn is 3.7wt% (S2-：16090mg/L）, concentration of sodium carbonate is 1.8wt%（19080mg/L）, naoh concentration is 2.8wt%, and oil is 320mg/L.Processed under the following conditions using the inventive method：
（1）Oil removal by air bubbling：Air is passed through in ethylene waste lye, makes to produce bubble in spent lye, the micro light oil carried secretly in spent lye is bonded on bubble, is floated on the surface with gas and is removed.After oil removal by air bubbling treatment, oil content is down to 17mg/L in spent lye.
（2）High-temperature wet-oxidation treatment：To solid sodium hydroxide is added in the spent lye after oil removal by air bubbling, naoh concentration is 3.5wt% in making spent lye.High-temperature wet-oxidation treatment is carried out in the basic conditions, and reaction temperature is 270 DEG C, and reaction pressure is 9.0MPa, and reaction time is 60min.After being processed through high-temperature wet-oxidation, S in water outlet2-Concentration is 0.3mg/L, and COD is 2980mg/L, and sodium sulfate concentration is 71380mg/L, and concentration of sodium carbonate is 44580mg/L, and naoh concentration is 1.3wt%.
（3）Sulfuric acid treatment：According to the concentration of hydroxyl and carbonate in high-temperature wet-oxidation water outlet, to the concentrated sulfuric acid that 98% is added in spent lye, regulation pH value of solution is 4.Hydroxyl and carbonate in solution are completely converted into sulfate radical, and sodium sulfate concentration is 156480mg/L in spent lye.
（4）Charcoal absorption：To wooden powdered activated carbon is added in the spent lye after acidification, activated carbon 10kg is added per 1m3 spent lyes, stirring mixing 0.5 hour, water outlet COD is 595mg/L.
（5）Multiple-effect evaporation：Enter 4 effect vapo(u)rization systems through the waste liquid after charcoal absorption, to producing, solid phase reclaims sodium sulfate crystal to the condensed rear reuse of steam after drying.Every cubic metre of recyclable purity of spent lye is 98.5% sodium sulphate 155.7kg.
Embodiment 2
The spent lye produced in one ethylene production, wherein COD is 62000mg/L, and vulcanization na concn is 6.3wt% (S2-：28430mg/l）, concentration of sodium carbonate is 2.3wt%（24380mg/L）, naoh concentration is 2.1wt%, and oil is 480mg/L.Processed under the following conditions using the inventive method：
（1）Oil removal by air bubbling：Air is passed through in ethylene waste lye, makes to produce bubble in spent lye, the micro light oil carried secretly in spent lye is bonded on bubble, is floated on the surface with gas and is removed.After oil removal by air bubbling treatment, oil content is down to 20mg/L in spent lye.
（2）High-temperature wet-oxidation treatment：Solid sodium hydroxide is added in spent lye after being processed to oil removal by air bubbling, naoh concentration is 3.5wt% in making spent lye.High-temperature wet-oxidation treatment is carried out in the basic conditions, and reaction temperature is 270 DEG C, and reaction pressure is 9.0MPa, and reaction time is 60min.After being processed through high-temperature wet-oxidation, S in water outlet2-Concentration is 0.5mg/L, and COD is 1180mg/L, and sodium sulfate concentration is 126100mg/L, and concentration of sodium carbonate is 27980mg/L, and naoh concentration is 1.8wt%.
（3）Sulfuric acid treatment：According to the concentration of hydroxyl and carbonate in high-temperature wet-oxidation water outlet, to the concentrated sulfuric acid that 98% is added in spent lye, regulation pH value of solution is 2.Hydroxyl and carbonate in solution are completely converted into sulfate radical, and sodium sulfate concentration is 163580mg/L in spent lye.
（4）Charcoal absorption：To wooden powdered activated carbon is added in the waste soda residue after acidification, activated carbon 13kg is added per 1m3 spent lyes, stirring mixing 1.5 hours, water outlet COD is 230mg/L.
（5）Multiple-effect evaporation：Enter 6 effect vapo(u)rization systems through the waste liquid after charcoal absorption, to producing, solid phase reclaims sodium sulfate crystal to the condensed rear reuse of steam after drying.Every cubic metre of recyclable purity of spent lye is 98.6% sodium sulphate 161kg.
Comparative example 1
With the identical spent lye of embodiment 1, difference is not use sulfuric acid treatment to remove carbonate and regulation pH value of solution, and spent lye directly uses charcoal absorption after being processed through high-temperature wet-oxidation for treatment.
To adding wooden powdered activated carbon in the spent lye after high-temperature wet-oxidation, add activated carbon 10kg per 1m3 spent lyes, stirring mixing 0.5 hour, because sodium sulfate concentration is low compared with spent lye after neutralizing in solution, its effect of saltouing to small organic molecule is poor, and water outlet COD is 920mg/L, after being processed through 4 effect vapo(u)rization systems, what concentrated phase was obtained after drying is carnallite sodium sulphate and sodium carbonate, it is impossible to obtain the sodium sulphate of high-purity.
Comparative example 2
Spent lye same as Example 1 is processed using the method described in CN201010526697.8.After spent lye is through wet oxidation and neutralisation treatment, the anhydrous sodium sulfate containing water entrainment is crystallized out from neutralizer using evaporative crystallization method, the anhydrous sodium sulfate containing water entrainment is dried, obtain anhydrous sodium sulfate product, its purity is 95.3%.COD is 1730mg/L in evaporation mother liquor.Part evaporation mother liquor returns to neutralisation unit, and the part chilled freezing mother liquor reclaimed after sal glauberi of evaporation mother liquor goes biochemical treatment, and COD is 1280mg/L in gained freezing mother liquor.Because an evaporation mother liquor part is back to neutralisation unit, energy consumption increases in causing evaporation and crystal process；Neutralizer is directly evaporated crystallization treatment, because COD concentration is higher, the reduction of evaporative crystallization product purity is on the one hand caused, COD concentration is higher on the other hand causing evaporation mother liquor and freezing mother liquor, and this part COD is mainly small molecular organic acid class material, it is impossible to removed by biochemical treatment.
Claims (10)
1. a kind of processing method of ethylene waste lye, it is characterised in that comprise the following steps：
（1）Oil removal by air bubbling, removes entrained oil class material in ethylene waste lye；
（2）High-temperature wet-oxidation treatment, the spent lye after oil removing carries out high-temperature wet-oxidation treatment；
（3）Sulfuric acid treatment, to the concentrated sulfuric acid is added in the spent lye after being processed through high-temperature wet-oxidation, sulfate radical is completely converted into by hydroxyl and carbonate；
（4）Charcoal absorption, the acid waste liquid after sulfuric acid treatment carries out charcoal absorption treatment；
（5）Multiple-effect evaporation, to carrying out multiple-effect evaporation through the waste liquid after charcoal absorption, reclaims sodium sulfate crystal.
2. in accordance with the method for claim 1, it is characterised in that：Step（1）Oil content after oil removal by air bubbling in spent lye is down to below 20mg/L, meets requirement of the high-temperature wet-oxidation technique for oil content of intaking.
3. in accordance with the method for claim 1, it is characterised in that：Sodium hydrate solid is added in spent lye after oil removing, addition is that naoh concentration is 3.0wt%~4.0wt% in making the spent lye for enter high-temperature wet-oxidation treatment, whole wet oxidation reaction is carried out in the basic conditions.
4. in accordance with the method for claim 1, it is characterised in that：Step（2）The middle reaction temperature for controlling high-temperature wet-oxidation is 240~320 DEG C, and reaction pressure is 6.0~20.0MPa, and the reaction time is 40~90 minutes.
5. in accordance with the method for claim 4, it is characterised in that：Step（2）The middle reaction temperature for controlling high-temperature wet-oxidation is 260~280 DEG C, reaction pressure is 8.0~12.0MPa。
6. in accordance with the method for claim 1, it is characterised in that：Step（3）According to carbonate in high-temperature wet-oxidation water outlet and concentration hydroxy, to the concentrated sulfuric acid that 98% is added in spent lye, the pH for controlling solution is 2~6.
7. in accordance with the method for claim 1, it is characterised in that：After spent lye after oil removing is through wet oxidation treatment and sulfuric acid acidification, wherein mainly containing sodium sulphate and small molecular organic acid class material, sodium sulfate concentration is up to more than 20%.
8. in accordance with the method for claim 1, it is characterised in that：Step（4）Activated carbon used is wooden powder's shaped activated carbon, and amounts of activated carbon is added in spent lye per ton for 5~15kg, and after 0.2~1.0h of stirring mixing, through Filter Press, filtrate sends into follow-up multiple-effect evaporation unit.
9. in accordance with the method for claim 1, it is characterised in that：Step（5）Multiple-effect evaporation selection 3~7 imitate, evaporator selection falling film type, the 1st effective evaporator in multi-effect evaporator using additional steam by the way of, after 2nd effect evaporator using it is previous effect evaporate wherein generate indirect steam as thermal source, the rest may be inferred.
10. in accordance with the method for claim 9, it is characterised in that：Sodium sulfate concentration is 60wt%~90wt% during multiple-effect evaporation controls solution, and sodium sulphate is obtained after the crystallized treatment of evaporation concentrated solution.
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| CN109761405A (en) * | 2019-02-01 | 2019-05-17 | 浙江科菲科技股份有限公司 | A kind of synthetical recovery of sulfate carbonate binary system nickel-containing waste water with high salt and the technique of wastewater zero discharge |
| CN112707570A (en) * | 2020-12-28 | 2021-04-27 | 江苏南大华兴环保科技股份公司 | Method for producing byproduct salt of imidazole aldehyde wastewater and application of substance for reducing surface tension in imidazole aldehyde wastewater |
| CN116081747A (en) * | 2021-10-31 | 2023-05-09 | 中国石油化工股份有限公司 | Method and device for treating ethylene waste alkali liquor |
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| CN112707570A (en) * | 2020-12-28 | 2021-04-27 | 江苏南大华兴环保科技股份公司 | Method for producing byproduct salt of imidazole aldehyde wastewater and application of substance for reducing surface tension in imidazole aldehyde wastewater |
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