CN103771614A - Treatment method of high-acid crude oil electro-desalting wastewater for up-to-standard discharge and reusing - Google Patents
Treatment method of high-acid crude oil electro-desalting wastewater for up-to-standard discharge and reusing Download PDFInfo
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- CN103771614A CN103771614A CN201210416372.3A CN201210416372A CN103771614A CN 103771614 A CN103771614 A CN 103771614A CN 201210416372 A CN201210416372 A CN 201210416372A CN 103771614 A CN103771614 A CN 103771614A
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Abstract
The invention provides a treatment method of high-acid crude oil electro-desalting wastewater for up-to-standard discharge and reusing. The method comprises the processing steps of flocculation, activated charcoal adsorption and ion exchange. Firstly, suspended matters and part of colloid or dissolved organic matters in effluent obtained through electro-desalting biochemical treatment of high-acid crude oil are removed in the step of flocculation, then colloid and dissolved organic matters are removed in the step of activated charcoal adsorption, and finally, ionic organic matters including naphthenic acid and the like are removed in the step of ion exchange, and wastewater is softened. According to the invention, the removal ratio of COD of the effluent obtained through electro-desalting biochemical treatment of high-acid crude oil is not less than 80 percent, and the COD of effluent after treatment is not greater than 55 mg/L, which meets the strict local discharge standard (COD is not greater than 60 mg/L), and the wastewater can be reused by a circulating water system or an electro-desalting device, so as to achieve dual purposes of water saving and emission reduction.
Description
Technical field
The invention belongs to technical field of waste water processing, relate to advanced treatment and the process for reclaiming of high acid crude oil electric desalting wastewater.
Background technology
At present, traditional oil removal-flotation-biochemical process the processing of the general employing of desalting in oil refinery waste water, when this art breading high acid crude oil electric desalting wastewater, the COD of water outlet, usually above 200 mg/L, far exceedes national wastewater discharge standard (COD≤100 mg/L).Along with the increase year by year of China's high-acid crude oil amount of finish inferior, and the stricter local wastewater discharge standard (COD≤60 mg/L) of some areas execution, the qualified discharge contradiction of high acid crude oil electric desalting wastewater will be more outstanding.The refinery of China is much positioned at water-deficient area, and water-saving and emission-reducing is the only way of its Sustainable development.On existing treatment facility basis, supplement and improve advanced treatment step, make high acid crude oil electric desalting wastewater biochemical treatment water outlet qualified discharge or reuse, be the good terms of settlement of technology and economic feasibility.
Organism in high acid crude oil electric desalting wastewater is mainly naphthenic acid, lower fatty acid and phenol compound, wherein the content of naphthenic acid is far above ordinary crude oils electric desalting waste water, because naphthenic acid is difficult to biochemical degradation, in biochemical treatment water outlet, residual concentration is higher, is to cause high acid crude oil electric desalting wastewater COD to be difficult to major cause up to standard.
Naphthenic acid is that alkyl replaces complex mixture acyclic or that alkyl-substituted alicyclic carboxylic acid forms, is the natural constituents of oil.Its molecular weight is generally 100～1300, contains monobasic～quaternary carboxyl, and wherein monobasic naphthenic acid is more common, and molecular weight is 100～600, and general molecular formula is C
nh
2n+Zo
2, in formula, n is carbon number, and Z is hydrogen degree of unsaturation, is 0 or negative even number, and-Z/2 is the quantity of ring.The difficult volatilization of naphthenic acid, acid close with longer chain fatty acid, its sodium salt is soluble in water, has surfactivity, can cause waste water emulsification or foam.The corrodibility of naphthenic acid is a difficult problem for puzzlement field produces and high-acid crude oil processing always.High molecular naphthenic acid interfacial activity is stronger, and its metal-salt easily deposits, and affects the normal operation of water-and-oil separator.Naphthenic acid is one of component that refinery water toxic is the strongest, toxic to hydrobiont, and lower molecular weight naphthenic acid toxicity is stronger.
In high acid crude oil electric desalting wastewater, Refractory organic compounds is mainly naphthenic acid, and existing naphthenic acid method of wastewater treatment generally adopts the preconditioning techniques such as extraction, absorption and flocculation.US5976366 adopts two-stage oily water separation-air lift-charcoal absorption-flocculation process to process electric desalting waste water, this technical process complexity, and working cost is high, has no its high acid crude oil electric desalting wastewater treatment effect.CN1078567C is with tertiary amine and diesel oil mixed extractant solvent naphthenic acid waste water, and extraction liquid sodium hydroxide lye back extraction, isolates extraction agent and reuse, and the reagent consumption of the method is larger, and cost is higher, and extraction process easily produces emulsification.CN1209302C provides a kind of flocculation electro multiphase catalysis to process the method for naphthenic acid waste water, and the method technical process is more complicated, and energy consumption is high, and naphthenic acid treatment effect is limited.US5395536 adopts flocculation-solvent extraction technology to process organic acid in water, and flocculation agent is polymerize aluminum chloride and cationic polyelectrolyte (as Poly Dimethyl Diallyl Ammonium Chloride), and extraction agent is diesel oil equal solvent oil, and this extraction process easily produces emulsification.Oil adsorbent for US5922206 (polyorganosilicate, acidifying calcium-base bentonite etc.) removes the oil in oil field extracted water, then macroporous adsorbent resin (as vinylbenzene-divinylbenzene polymer resin) absorption carbon number exceedes 6 carboxylic acid or naphthenic acid, if uncomfortable joint oil field extracted water is acid, naphthenic acid adsorption effect is poor, if regulate the pH value of oil field extracted water, the consumption of soda acid is larger.US7575689 adds solvability calcium salt (as nitrocalcite, calcium chloride etc.) in naphthenic acid waste water, promotes the charcoal absorption of naphthenic acid, the method calcium salt large usage quantity, and expense is higher.Refinery coke absorption pre-treatment oil-sand processing wastewater middle and high concentration naphthenic acid for US7638057, refinery coke and waste water pulpous state be mixed to be separated more difficultly, and absorption bubble point oil Jiao is secondary pollutant, need further process.
Common wastewater through organic matter advanced treatment technology comprises advanced oxidation (as electrochemical oxidation, photochemical catalysis, Fenton oxidation etc.), membrane technique (reverse osmosis, nanofiltration etc.) and adsorption technology (gac, activated carbon fiber, macroporous adsorbent resin etc.) etc.Its Trends of Advanced Oxidation Process Methods cost is higher, and many places are in the laboratory study stage, and technology maturity is lower; Membrane technique is had relatively high expectations to water inlet, and film easily stops up; Active carbon adsorption technology is relatively ripe, generally need with other treatment technology optimum combination, to improve treatment effect and to reduce processing cost.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of deep treatment method of high acid crude oil electric desalting wastewater, be mainly used in qualified discharge or the Treatment for Reuse of high acid crude oil electric desalting wastewater oil removal-flotation-biochemical treatment water outlet.
The qualified discharge of high acid crude oil electric desalting wastewater of the present invention and the concrete scheme of process for reclaiming are as follows: first high-acid crude oil electric desalting biochemical treatment water outlet removes suspended substance and part colloid or dissolved organic matter by flocculation step, then remove colloid and dissolved organic matter through charcoal absorption step, finally remove naphthenic acid plasma type organism by ion-exchange step, finally make to process COD≤55 mg/L of water outlet.Process water outlet and can meet strict local emission standard (COD≤60 mg/L), also can reuse to circulating water system or electric desalting apparatus etc.
In the inventive method, intake as the processing water outlet of high acid crude oil electric desalting wastewater after conventional oil removal-flotation-biochemical treatment.
In the inventive method, flocculation step adds inorganic flocculating agent, cationic organic polymer coargulator or composite flocculation agent in waste water, suspension, emulsification and colloidal organic matter in waste water is agglomerated into compared with large particle and settles down, and separates with water.Inorganic flocculating agent used comprises polymerize aluminum chloride (PAC), polyaluminium sulfate (PAS), bodied ferric sulfate (PFS), poly-sulphur aluminum chloride (PPAC), poly-sulphur iron(ic) chloride (PFCS), poly-phosphorus aluminum chloride (PPAC), one or more in PPFS (PFPS) etc., organic floculant comprises quaternaries cation polyelectrolyte, poly-ammonium salt class and cationic polyacrylamide etc., composite flocculation agent is multiple inorganic flocculating agent combination, multiple cationic organic polymer coargulator combination or inorganic flocculating agent and the combination of cationic organic polymer coargulator.
In the inventive method flocculation treatment, wastewater pH is 6～8; Flocculant concentration is 10～150 mg/L, and the best is 60～80 mg/L; Flocculation and settling time are 20～120 min, and the best is 60～70 min.
In the inventive method, flocculation water outlet is further processed through fixing or suspension activated carbon filter bed.Suspension filter bed adopts Powdered Activated Carbon, after having adsorbed, by sedimentation or filtering separation waste water and gac.The filler of fixing gac filter bed is particle or columnar activated carbon, and the best is 2～3 groups of fixing gac filter bed parallel connections, can realize the alternate operation of absorption and regeneration (or renewal).Gac used is any type, can use commercial goods, and specific surface area is higher than 300 m
2/ g, preferably higher than 500 m
2/ g.The granularity of particles used gac is 5～60 orders, and the best is 20～40 orders.The diameter of columnar activated carbon used is 0.8～2 mm, and length is 2～5 mm.PH value the best of waste water is 5～7, and service temperature is 10～30 ℃, activated-carbon filter bed height 1～2 m, be 5～25 min(filtering velocity 5～10 m/h an empty duration of contact), the best is 15～20 min.
In the inventive method, activated carbon treatment water outlet contacts with anion-exchange resin column with cation exchange resin column successively.
First activated carbon treatment water outlet contacts with cation exchange resin column by fixed bed or floating bed, is sodium ion by cation replacements such as the calcium magnesium in waste water, softening waste water, and prevent that these positively charged ions from precipitating on follow-up anionite-exchange resin.
Cation exchange resin column is single-column, multicolumn series connection or multicolumn parallel connection, and the best is 2～3 groups of resin column parallel connections, and every group of 1～3 resin column connected, and can realize the alternate operation of absorption and regeneration.Operation flow velocity 10～50 m/h, best 20～30 m/h.
Zeo-karb is cross-linked styrene-divinylbenzene interpolymer acidic cation-exchange resin, and the best is with sulfonic group [SO on cross-linked styrene-divinylbenzene interpolymer
3h] storng-acid cation exchange resin.The ionic type of Zeo-karb is sodium-ion type or hydrogen ion type, and the best is sodium-ion type.Zeo-karb is macropore or equal hole, and the best is equal hole.Resin particle diameter is 0.3～1.3 mm, and the best is 0.4～0.6 mm.
The service temperature of cationic exchange is 10～50 ℃.Be 5～30 min an empty duration of contact, and the best is 10～15 min.
The regenerated liquid of sodium-ion type Zeo-karb is sodium chloride solution, concentration 5%～10% (mass percent), 1～3 times of bed volume of consumption, regenerated liquid flow velocity 4～6 m/h.The regenerated liquid of hydrogen ion type Zeo-karb is hydrochloric acid soln, concentration 3%～5% (mass percent), and 2～4 times of bed volume of consumption, the best is 3 times of bed volume, regenerated liquid flow velocity 4～6 m/h.
Above-mentioned storng-acid cation exchange resin is the domestic equal pass strongly acidic styrene type cation exchange resin of D072, D061 large hole strong acid styrene system cation exchange resin, 001 × 7,001 × 7 × 7 strongly acidic styrene type cation exchange resins, JK008, or the similar resin of the corresponding U.S. Rohm & Haas Amberlite of company series, the U.S. Dowex of DOW chemical company series, the Diaion of Mitsubishi chemical company series storng-acid cation exchange resin and domestic or other national production with it.
Cationic exchange is processed water outlet and is contacted with anion-exchange resin column by fixed bed or floating bed, and the negatively charged ion on the negatively charged ion such as naphthenic acid and resin exchanges, and is removed from waste water.
Anion-exchange resin column is single-column, multicolumn series connection or multicolumn parallel connection, and the best is 2～3 groups of resin column parallel connections, and every group of 1～3 resin column connected, and can realize the alternate operation of absorption and regeneration.Operation flow velocity 10～50 m/h, best 20～30 m/h.
Anionite-exchange resin is cross-linked styrene-divinylbenzene interpolymer basic anion exchange resin, and the best is with quaternary ammonium group [N (CH on cross-linked styrene-divinylbenzene interpolymer
3)
3oH] strongly basic anion exchange resin.The ionic type of anionite-exchange resin is chlorion type or hydroxyl type, and the best is chlorion type.Anionite-exchange resin is macropore or equal hole, and the best is equal hole.Resin particle diameter is 0.3～1.3 mm, and the best is 0.4～0.6 mm.
The service temperature of anionresin is 10～50 ℃.Be 5～30 min an empty duration of contact, and the best is 10～15 min.
The regenerated liquid of hydroxyl type anion exchange resin is sodium hydroxide solution, concentration 1%～10% (mass percent), the best is 3%～5% (mass percent), 2～5 times of bed volume of consumption, the best is 3 times of bed volume, regenerated liquid flow velocity 1～10 m/h, best 4～6 m/h.The regenerated liquid of chlorion type anionite-exchange resin is sodium-chlor and sodium hydroxide solution, sodium chloride concentration 5%～10% (mass percent), sodium hydroxide 0.1～0.5% (mass percent), 2～5 times of bed volume of consumption, the best is 3 times of bed volume, regenerated liquid flow velocity 1～10 m/h, best 4～6 m/h.
Above-mentioned strongly basic anion exchange resin is domestic D201 macroporous strong basic styrene series anionite-exchange resin, 201 × 4,201 × 7 strong-basicity styrene series anion exchange resins, the equal hole of JK206 strong-basicity styrene series anion exchange resin, or the similar resin of the corresponding U.S. Rohm & Haas Amberlite of company series, the U.S. Dowex of DOW chemical company series, the Diaion of Mitsubishi chemical company series strongly basic anion exchange resin and domestic or other national production with it.
In the inventive method, it is crude oil more than 1mg KOH/g that high acid crude oil electric desalting wastewater refers generally to acid number, the waste water producing in electric desalting process.Be applicable to all kinds of qualified discharge processing containing naphthenic acid waste water such as electric desalting waste water or polymer flooding oil field waste water of processing highly acid crude oil.
The present invention not only can remove suspension organism and colloidal organic matter in waste water, also can remove naphthenic acid plasma type organism, can remove most of inorganic salt simultaneously.While processing the biochemical treatment water outlet of refinery processing highly acid crude oil electric desalting waste water, can make the COD of waste water be down to below 55 mg/L by 150～750 mg/L, COD clearance >=80%, wherein the COD clearance of flocculation step is about 30%～50%, charcoal absorption step is about 60%～80% to the clearance of flocculation water outlet COD, ion-exchange step is about 40%～60% to the clearance of charcoal absorption water outlet COD, color is become colorless transparent by khaki color, not only can realize the qualified discharge of this type of difficult waste water, process water outlet also can reuse to electric desalting apparatus.
The present invention is directed to the characteristic of high acid crude oil electric desalting wastewater biochemical treatment water outlet, adopt suitable technical process, described processing unit has produced coordinated effect, obtain outstanding technique effect, flocculation, charcoal absorption and ion-exchange can be processed respectively suspended substance in waste water, solvability non-ionic type organism and ionic organic compound, specifically, flocculation step removes suspended substance and part colloid or dissolved organic matter, then charcoal absorption step removes colloid and dissolved organic matter, cationic exchange has removed the easy metal ions that precipitate on anionite-exchange resin such as the calcium magnesium in waste water, last anionresin removes naphthenic acid plasma type organism in waste water, and softening waste water.
Embodiment
Embodiment 1
Certain refinery processing highly acid crude oil electric desalting waste water adopts oil removal-flotation-A/O treatment process, and the COD of its A/O section water outlet is 550 mg/L, is difficult to qualified discharge.Confirm that through By Gas Chromatography-mass Spectrometry and electron spray mass spectrometry analysis the organism in bio-chemical effluent is mainly the naphthenic acid that is difficult to biochemical degradation.
Get above-mentioned waste water 5 L (pH=7.0, khaki color), waste water adds polymeric ferric sulfate flocculant 350 mg, and flocculation time is 60 min, and the COD of settlement separate rear waste water is 310 mg/L, and COD clearance is 43.6%.
Get waste water 1 L after flocculation, add 20～40 object granular carbon 1 g, vibration absorption 20 min, after sedimentation and filtering separation, the COD of waste water is 70 mg/L, COD clearance is 77.4%.
Salt acid soak 2 h of 3% (mass percent) for 001 × 7 × 7 strongly acidic styrene type cation exchange resins (Chemical Plant of Nankai Univ.), 100 g, clean extremely neutral with distilled water, and then with soaking 2 h with 6% (mass percent) sodium chloride solution, wash remaining sodium-chlor with distilled water, last elimination moisture, and at room temperature seasoning.201 × 7 strong-basicity styrene series anion exchange resins (Chemical Plant of Nankai Univ.), 100 g soak 2 h with 6% (mass percent) sodium-chlor and 0.2% (mass percent) sodium hydroxide mixing solutions, then clean to neutral with distilled water, last elimination moisture, and at room temperature seasoning.
Get waste water 200 mL after charcoal absorption, put into 500 mL flasks, add 001 × 7 × 7 strongly acidic styrene type cation exchange resin 50 g after treatment, then vibration contact 20 min on track shaking table.Upper strata clear water after settlement separate is put into another 500 mL flask, adds 201 × 7 strong-basicity styrene series anion exchange resin 50 g after treatment, then vibration contact 40 min on track shaking table.The COD of settlement separate rear upper strata clear water is 40 mg/L, and having gone of ion-exchange step COD is 42.9%.
The water outlet of A/O section is khaki color, and COD is 550 mg/L, and after above-mentioned flow processing, water sample is water white transparency, and COD is 40 mg/L, and the overall clearance of COD is 92.7%.
Embodiment 2
Pack 201 × 7 strong-basicity styrene series anion exchange resin 20 mL after treatment embodiment 1 into φ 12 × 300 mm glass columns, the MBR water outlet (COD be 220 mg/Ls) identical with embodiment 1 at room temperature, flow velocity with 2 mL/min passes through resin, water outlet approaches colourless, COD is 52 mg/L, and COD clearance is 72%.
After resins exchange is saturated, with 10% (mass percent) sodium-chlor and 0.5% (mass percent) sodium hydroxide mixing solutions at room temperature,, regenerate by resin with the flow velocity of 2 mL/min.After regeneration, resin is substantially constant to the treatment effect of waste water naphthenic acid.
Claims (10)
1. the qualified discharge of a high acid crude oil electric desalting wastewater and process for reclaiming, it is characterized in that comprising following process: first high-acid crude oil electric desalting biochemical treatment water outlet removes suspended substance and part colloid or dissolved organic matter by flocculation step, then remove colloid and dissolved organic matter through charcoal absorption step, finally remove naphthenic acid by ion-exchange step, finally make to process COD≤55 mg/L of water outlet.
2. method according to claim 1, is characterized in that: high-acid crude oil electric desalting biochemical treatment water outlet is the processing water outlet of high acid crude oil electric desalting wastewater after conventional oil removal-flotation-biochemical treatment.
3. method according to claim 1, it is characterized in that: flocculation step adds inorganic flocculating agent, cationic organic polymer coargulator or composite flocculation agent in waste water, suspension, emulsification and colloidal organic matter in waste water is agglomerated into compared with large particle and settles down, separate with water; Inorganic flocculating agent used comprises one or more in polymerize aluminum chloride, polyaluminium sulfate, bodied ferric sulfate, poly-sulphur aluminum chloride, poly-sulphur iron(ic) chloride, poly-phosphorus aluminum chloride, PPFS; Organic floculant comprises one or more in quaternaries cation polyelectrolyte, poly-ammonium salt class and cationic polyacrylamide.
4. according to the method described in claim 1 or 3, it is characterized in that: in flocculation treatment process, wastewater pH is 6～8; Flocculant concentration is 10～150 mg/L, and flocculation and settling time are 20～120 min.
5. method according to claim 1, is characterized in that: flocculation water outlet is further processed through gac filter bed, and the pH value of waste water is 5～7, and service temperature is 10～30 ℃, and be 5～30 min an empty duration of contact.
6. method according to claim 1, is characterized in that: activated carbon treatment water outlet contacts with anion-exchange resin column with cation exchange resin column successively.
7. according to the method described in claim 1 or 6, it is characterized in that: Zeo-karb is cross-linked styrene-divinylbenzene interpolymer acidic cation-exchange resin, operation flow velocity is 10～50 m/h.
8. according to the method described in claim 1 or 6, it is characterized in that: the service temperature of cationic exchange is 10～50 ℃; Be 5～30 min an empty duration of contact, and the best is 10～15 min.
9. according to the method described in claim 1 or 6, it is characterized in that: the operation flow velocity of anion-exchange resin column is 10～50 m/h.
10. according to the method described in claim 1 or 6, it is characterized in that: anionite-exchange resin is cross-linked styrene-divinylbenzene interpolymer basic anion exchange resin, and the service temperature of anionresin is 10～50 ℃, be 5～30 min an empty duration of contact.
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