CN100594189C - Method for treatment of oil-bearing waste water - Google Patents
Method for treatment of oil-bearing waste water Download PDFInfo
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- CN100594189C CN100594189C CN200710010901A CN200710010901A CN100594189C CN 100594189 C CN100594189 C CN 100594189C CN 200710010901 A CN200710010901 A CN 200710010901A CN 200710010901 A CN200710010901 A CN 200710010901A CN 100594189 C CN100594189 C CN 100594189C
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Abstract
The invention relates to a treatment method for oily wastewater, in particular to a treatment method for the oily wastewater in oil refineries and oil extraction wastewater in oil fields. The treatment method comprises launching an emulsion breaker A into the oily wastewater firstly and then plunging a flocculant B into the oily wastewater after the emulsion breaking reaction. The emulsion breakerA is a quaternary ammonium type positive ion polymer; and the flocculant B is a colloid aqueous solution taking sulfonated methyl polyacrylamide as a main ingredient. The oily wastewater, in particular the oil refinery wastewater and oil field wastewater, treated by the method of the invention can meet the requirements of process indexes of the consequent biological treatment.
Description
Technical field
The present invention relates to a kind of treatment process of oily(waste)water, particularly at the treatment process of refinery oily(waste)water, oil production waste water in oil field.
Background technology
In refining of petroleum or recovery process, can produce a large amount of oily(waste)waters, adopt processes such as gravity oil removal, dissolved air floatation to handle usually.In the oily water treatment process, generally need to add emulsion splitter, make the oily(waste)water breakdown of emulsion, reach the purpose of oil removing with this.The most frequently used emulsion splitter is polymerize aluminum chloride (abbreviating PAC as), though have breaking milk and removing oil performance preferably, but its maximum shortcoming is in the treating processes, the scum silica frost amount that produces is big, the water content of slag is up to 95%～99.5% (weight), and loose, the easy fragmentation of flco, bring difficulty for the aftertreatment of scum silica frost.
Along with the increase of the oilfield exploitation degree of depth, recover the oil and substantially all adopt water flooding regime in many oil fields, and the crude oil water content and the oil field produced water yield constantly increase, and the excessive and waste water of waste water effluxes the problem serious threat that exceeds standard ordinary production and the ecotope to the oil field.A kind of wasting of resources is not only in the discharging of oil extraction-generated waste water, and serious environment pollution.Therefore, the oil extraction-generated waste water resource utilization is the important measures that solve the oil field deterioration of the ecological environment, control ground water regime catastrophe variation.
An oil production waste water in oil field part after treatment is used as re-injection water, and a part effluxes.Therefore, provide qualified re-injection water water quality, satisfy the oil field and recover the oil, guaranteeing that oil field stable high yield has crucial meaning to requirements in water quality.For this reason, should improve the oilfield water technology level on the one hand, adopt efficient new technology, new installation, simplify sewage treatment process to greatest extent, improve effluent quality; Should select efficient oil-water separating agent for use on the other hand, guarantee the efficient operation of crude oil transmission station oily water separation, guarantee effluent quality, reduce working cost.Make oil extraction waste water be achieved resource utilization after treatment.
CN85107131 has introduced the emulsion splitter that is used to handle oily(waste)water based on inorganic aluminate, molysite, when using this agent to dispose of sewage, has produced a large amount of scum silica frost, and scum silica frost water ratio height, has brought secondary pollution.CN1451610A has disclosed a kind of oil production waste water in oil field advanced treatment and cyclic utilization method.It is to adopt the film separating system of micro-filtration or ultrafiltration to the suspended substance in the oil extraction waste water, COD
Cr, oil, polymkeric substance removes, the water outlet after the processing is removed salinity and micromolecular oil in the water through nanofiltration or reverse osmosis again, final outflow water water quality reaches the high standard requirement to water quality of oil recovery re-injection water and configuration polymer oil-displacing agent water.Be mainly used in the processing and the recycle of oil production waste water in oil field.CN1429781A has disclosed a kind of treatment process and isolated plant thereof of oil extraction waste water.It is to adopt in reaction unit, feeds ozone, and oil extraction waste water is from bottom to top by reaction unit, makes that ozone concn reaches 5～20mg/L in the reaction unit; Meanwhile, add ultrasonic wave, its frequency is greater than 20kHz, smaller or equal to 25kHz, and sound intensity value is controlled between 0.5～1.0I0; Oil extraction waste water and ozone are stirred, it is fully contacted; The residence time of oil extraction waste water in reaction unit is 8～20 minutes.CN1358673A has disclosed the separation method and the device of calcium, magnesium ion in a kind of oil extraction waste water.It is to adopt the oily(waste)water that will contain calcium, magnesium ion, flow through the last one electrostatic field, the ion of positively charged in the waste water is assembled to the negative pole of electric field, and electronegative ion is assembled to the positive pole of electric field, again waste water is flow through a weak electrostatic field, ion is concentrated collection, and the waste water after the purification then can be used for the re-injection in oil field.CN1362373A discloses a kind of treatment process of oily(waste)water, adopts a kind of inorganic flocculating agent and two kinds of organic floculants, and wherein inorganic flocculating agent and a kind of organic floculant are compound, add in the oily(waste)water simultaneously respectively with another kind of organic floculant then.The component that this patent is used is more, and certain inconvenience is arranged during application.In addition, when using inorganic flocculating agent, the oil phase of recovery contains the part inorganic impurity, and utilization has adverse influence to oil recovery.USP4,818,410 and USP4,839,054 have proposed to utilize acidifying, mixing, are separated to remove the method for organic pollutant in the oil field extracted water.Not only accelerate the corrosion of equipment yet add strong acid, and in treating processes, additionally added other pollutent again.
Summary of the invention
At the deficiencies in the prior art, the present invention discloses the treatment process of the oily(waste)water that a kind of deoiling effect is good, method is easy, particularly at the treatment process of refinery oily(waste)water, oil production waste water in oil field.
The oily method of wastewater treatment that the present invention contains may further comprise the steps:
(1) emulsion splitter A is added in the oily(waste)water, add-on is 0.5～500mg/L, and preferred 1～200mg/L stirs.Emulsion splitter A is a kind of cationic polymers of quaternary ammonium type.
(2) flocculating agent B is added in the waste water that step (1) obtains, add-on is 0.5～500mg/L, and preferred 1～200mg/L stirs.Flocculating agent B be a kind of be the colloid aqueous solution of main component with the sulfonated methyl polyacrylamide.
(3) static separation.
The emulsion splitter A that the present invention uses is a kind of cationic polymers of quaternary ammonium type, not only have good demulsification performance, and the scum silica frost generation is few, can adopt conventional aqueous solution polymerization method to obtain.
It has following structure:
In the formula: R is H or CH
3
The scope of m is 10,000～200,000, and the scope of n is 10,000～100,000.
The cationic polymers colloid aqueous solution that the flocculating agent B that the present invention uses has following structure:
It has following structure:
In the formula: the scope of m is 10,000～200,000, and the scope of n is 10,000～280,000, and the weight concentration of polymkeric substance is 0.05%～3%, and polymeric colloid aqueous solution kinematic viscosity is 100～600mm
2/ s.
Advantage of the present invention is to adopt the emulsion splitter A and the flocculating agent B of different performance to be used.Emulsion splitter A is a kind of cationic polymers of quaternary ammonium type, when handling oily(waste)water, has good demulsification performance and deoiling effect.Flocculating agent B is that a kind of sulfonated methyl polyacrylamide is the colloid aqueous solution of main component, has outstanding cohesion bridging action.After flocculating agent B, it can condense the formed flco of adding emulsion splitter A, elaioleucite fast, forms big flco and elaioleucite, separate rapidly with water, and floating upward quickly is to the water surface.Be more significantly, emulsion splitter A and flocculating agent B are all organic polymer, and waste water is not after treatment brought other inorganic impurity into, helps improving the water quality of re-injection water, and formed scum silica frost oleaginousness height is easy to aftertreatment.Emulsion splitter A that the present invention relates to and flocculating agent B not only use properties are good, and have treatment effect preferably.
Embodiment
Oily wastewater treatment method of the present invention adopts emulsion splitter A and two kinds of polymkeric substance of flocculating agent B to be used, and earlier emulsion splitter A is dropped in the oily(waste)water, behind the breakdown of emulsion, flocculating agent B is dropped in the oily(waste)water again, and the oil removing process of oily(waste)water is finished in static then separation.The consumption of emulsion splitter and flocculation agent can be determined or determine by simple experiment according to the character of institute's treating water and the index request of processing back water outlet, in general oil-contg is high more in institute's treating water, the requirement of water outlet oil-contg is low more, needs the amount of emulsion splitter and flocculation agent just big more.Can determine by the design of this area general knowledge, be generally 5 minutes～5 hours rest time.
Emulsion splitter A of the present invention is a kind of cationic polymers of quaternary ammonium type, with acrylamide monomer and dimethylaminoethyl methacrylate monomer is main raw material, at first at 60 ℃～80 ℃, distillation purifying methyl acrylic dimethylaminoethyl monomer (overhead product is the dimethylaminoethyl methacrylate monomer after purifying) under negative pressure 0.092～0.097MPa condition, in the dimethylaminoethyl methacrylate monomer after the quaternizing agent adding purification, and obtain quaternized monomer, then with acrylamide, the quaternized monomer of dimethylaminoethyl methacrylate, after deionized water mixes by a certain percentage, nitrogen blowing is removed dissolved oxygen, adds initiator at last and carries out polyreaction.Negative pressure value refers to that absolute pressure is lower than the normal pressure numerical value of (normal pressure refers to a normal atmosphere 0.101325MPa), refers to that as negative pressure 0.092MPa the absolute pressure value of this moment is lower than normal pressure 0.092MPa, and promptly absolute pressure is 0.009325MPa (9.325KPa).In the raw material dimethylaminoethyl methacrylate of preparation polymeric flocculant, contain the stopper that prevents polyreaction, as phenol, hydroquinone monomethyl ether etc.Experiment shows, the existence of these stoppers can consume initiator, and the monomer free radical is lost activity, and influences the polyreaction of polymeric flocculant, generates low molecular polymkeric substance.When the dimethylaminoethyl methacrylate monomer after the purification carries out polyreaction, eliminated the influence of stopper, product property is good.
Other synthesis step of the emulsion splitter A that relates in the inventive method and condition can adopt existing conventional scheme in this area.As the reaction of dimethylaminoethyl methacrylate monomeric quaternary ammonium is to add quaternizing agent in the dimethylaminoethyl methacrylate monomer, regulating the pH value is 2～9, be preferably 4～8, reacting is that very exothermic is reacted, and should carry out or take other temperature measure of control in water-bath or ice-water bath.Quaternizing agent is hydrochloric acid or methyl chloride.The quaternized monomeric polymeric proportioning of acrylamide and dimethylaminoethyl methacrylate (mol ratio) is, acrylamide: dimethylaminoethyl methacrylate=10: 1～1: 10, best polymerization proportioning is: acrylamide: dimethylaminoethyl methacrylate=8: 1～1: 8, the total concn of monomer polymerization is: 0.5～1.5mol/L, best polymerization concentration is: 0.6～1.2mol/L, the polymeric temperature of reaction is: 20～90 ℃, optimum temps is: 30～80 ℃, polymerization reaction time is 1～10h, preferably 1～6h.Polymerization process can adopt different initiator systems to carry out Raolical polymerizable, adopt water-soluble azo initiator, as N, N-dihydroxy ethyl azo-bis-isobutyrate hydrochloride, the two amidine propane dihydrochlorides, 2 of azo, one or more in two (2-methyl 2-the amidine propane)-hydrochlorides of 2-azo.The add-on of initiator is 10
-5Mol/L～10
-2Mol/L; Adopting redox initiator is to be in Potassium Persulphate, ammonium persulphate and the Sodium Persulfate one or more; Sulphite is one or more in S-WAT, sodium bisulfite, potassium sulfite, Potassium hydrogen sulfite, ammonium sulphite and the ammonium bisulfite.One or both of persulphate and sulphite, wherein the proportioning of persulphate and sulphite is: 1: 0～1, the add-on of initiator is 10 of a monomer total amount
-3～10
-4Mol/L, optimal addn is: 5 * 10
-4～10
-4Mol/L.
The cationic polymers colloid aqueous solution that the flocculating agent B that the present invention uses has following structure:
It has following structure:
In the formula: the scope of m is 10,000～200,000, and the scope of n is 10,000～280,000, and the weight concentration of polymkeric substance is 0.05%～3%, and the kinematic viscosity of dewatering agent is 100～600mm
2/ s.
Its preparation process is as follows:
Fresh water is added in the reactor, under condition of stirring, equably negatively charged ion or non-ionic polyacrylamide are added in the reactor.After treating that it dissolves fully, add mineral alkali, adjust the pH value of solution.Add sequestrant, reaction promotor then, control reaction temperature adds formaldehyde, organic amine in the reactor, behind the reaction certain hour, adds the terminator stopped reaction, can obtain product.
Wherein, the best proportioning of each reaction raw materials is negatively charged ion or non-ionic polyacrylamide: formaldehyde: organic amine: fresh water: sequestrant: reaction promotor: terminator is=1: 0.5～2.5: 0.5～2.5: 100～5000: 0.005～0.05: 0.005～0.05: 10～500 (mol ratios) are preferably 1: 0.5～2.0: 0.5～2.0: 500～4000: 0.005～0.01: 0.005～0.01: 10～500 (mol ratios).The selection of negatively charged ion or non-ionic polyacrylamide does not require, and can be common commercial goods.Mineral alkali is a kind of of sodium hydroxide, potassium hydroxide; Organic amine is one or more of dimethylamine, diethylamine, Dyhard RU 100; Sequestrant is one or more in edta and its sodium salt, ethylene diaminetetraacetic acid and sodium salt thereof and diethylenediamine pentaacetic acid and the sodium salt thereof; Reaction promotor is one or more in persulphate and the water-soluble azo class material, wherein persulphate is one or more of Potassium Persulphate, ammonium persulphate, Sodium Persulfate, water-soluble azo class thing is N, N-dihydroxy ethyl azo-bis-isobutyrate hydrochloride, the two amidine propane dihydrochlorides, 2 of azo, one or more of two (2-methyl 2-the amidine propane)-hydrochlorides of 2-azo.Terminator be hydrochloric acid, vitriolic one or both.
Add mineral alkali, adjust the pH value of solution, be controlled between 7～14, preferably between 8～13; Temperature of reaction is controlled between 20 ℃～80 ℃, preferably between 20 ℃～70 ℃; The dissolution time of negatively charged ion or non-ionic polyacrylamide is controlled at 1h～6h, preferably is controlled at 2h～5h; Reaction times is controlled at 2h～10h, preferably is controlled at 2h～8h.
The scheme and the effect of the inventive method are described below by embodiment.
Embodiment 1 commercially available dimethylaminoethyl methacrylate monomer is purified
Quantitative commercially available dimethylaminoethyl methacrylate monomer is added in the matrass, vacuumize, under negative pressure 0.095MPa condition, be warming up to 75 ℃, distill, will collect the dimethylaminoethyl methacrylate monomer of purifying, it is stand-by to put into refrigerator.
Embodiment 2
In the four-hole boiling flask of the 500ml that agitator, thermometer, filling tube, import and export of nitrogen are housed, add the dimethylaminoethyl methacrylate 36.8g after purifying, the HCl 45ml that adds 1N, regulating pH value is 4.0, adds acrylamide 4.26g then, deionized water 430ml, after mixing, logical nitrogen removes dissolved oxygen, adds N, N-dihydroxy ethyl azo-bis-isobutyrate hydrochloride initiator 5 * 10
-4Mol/L adds ammonium persulphate (chemical pure) 5 * 10
-4Mol/L, sodium bisulfite (chemical pure) 2 * 10
-5Mol/L in 35 ℃ of water-baths, carries out copolymerization 6h, obtains emulsion splitter A-1.Limiting viscosity: 830cm
3/ g; Cationic degree: 4.5mmol/g.
Embodiment 3
In the four-hole boiling flask of the 500ml that agitator, thermometer, filling tube, import and export of nitrogen are housed, add the dimethylaminoethyl methacrylate 9.6g after purifying, the HCl 2ml that adds 1N, regulating pH value is 3.5, adds acrylamide 38.6g then, deionized water 460ml, after mixing, logical nitrogen removes dissolved oxygen, adds N, N-dihydroxy ethyl azo-bis-isobutyrate hydrochloride initiator 5 * 10
-4Mol/L, ammonium persulphate (chemical pure) 2 * 10
-4Mol/L, sodium bisulfite (chemical pure) 1 * 10
-5Mol/L in 35 ℃ of water-baths, reacted 3 hours, and in 60 ℃ of water-baths, reaction 1.5h obtains emulsion splitter A-2 again.Limiting viscosity: 1510cm
3/ g; Cationic degree: 1.5mmol/g.
Embodiment 4
In reactor, add the 499kg fresh water, start and stir, add non-ionic polyacrylamide 1.1kg.After treating that it dissolves fully, add 0.1kg sodium hydroxide (chemical pure), the pH value of adjusting solution is 11～12.Add 0.5g disodium ethylene diamine tetraacetate (chemical pure) then, control reaction temperature, adds in the reactor 1000mL formaldehyde (chemical pure) and sodium bisulfite (chemical pure) 1.5kg at 30 ℃, and the reaction times is 4h.Add 500mL hydrochloric acid (chemical pure) stopped reaction at last, obtain flocculating agent B-1.Kinematic viscosity: 406.9mm
2/ s.
Embodiment 5
In reactor, add the 986kg fresh water, start and stir, add anionic polyacrylamide 3.88kg.After treating that it dissolves fully, add 0.31kg sodium hydroxide (chemical pure), the pH value of adjusting solution is 9～10.Add 0.8g disodium ethylene diamine tetraacetate (chemical pure) then, control reaction temperature, adds in the reactor 3200mL formaldehyde (chemical pure) and sodium bisulfite (chemical pure) 6.5kg at 55 ℃, and the reaction times is 2h.Add 3200mL hydrochloric acid (chemical pure) stopped reaction at last, obtain flocculating agent B-2.Kinematic viscosity: 586.8mm
2/ s.
Embodiment 6
Get certain refinery oil trap water outlet and carry out the breakdown of emulsion test, add the flocculation agent of different varieties, stir, static then 30 minutes, get clear liquor and analyze oil-contg.When using emulsion splitter and flocculation agent, add emulsion splitter earlier and stir, add flocculation agent then and stir, last static 30 minutes, get clear liquor and analyze oil-contg.Its result sees Table 1.
Table 1 emulsion splitter is to the treatment effect of certain refinery oil trap water outlet
Embodiment 7
Get certain oil production waste water in oil field and do evaluation test.
Oil extraction waste water is added the flocculation agent of different varieties, stir, static then 30 minutes, get clear liquor and analyze oil-contg.When using emulsion splitter and flocculation agent, add emulsion splitter earlier and stir, add flocculation agent then and stir, last static 30 minutes, get clear liquor and analyze oil-contg.Treatment effect sees Table 2.
The flocculation agent of table 2 different varieties is to the treatment effect of oil-containing wastewater
Claims (8)
1, a kind of treatment process of oily(waste)water may further comprise the steps:
(1) emulsion splitter A is added in refinery oily(waste)water or the oil production waste water in oil field, add-on is 0.5～500mg/L, stirs, and emulsion splitter A is a kind of cationic polymers of quaternary ammonium type;
(2) flocculating agent B is added in the waste water that step (1) obtains, add-on is 0.5～500mg/L, stir, flocculating agent B be a kind of be the colloid aqueous solution of main component with the sulfonated methyl polyacrylamide;
(3) static separation;
Wherein the structure of the emulsion splitter A described in the step (1) is:
In the formula: R is H or CH
3
The scope of m is 10,000～200,000, and the scope of n is 10,000～100,000;
Flocculating agent B described in the step (2) is that a kind of sulfonated methyl polyacrylamide is the colloid aqueous solution of main component, has following structure:
In the formula: the scope of m is 10,000～200,000, and the scope of n is 10,000～280,000, and the weight concentration of polymkeric substance is 0.05%～3%, and the kinematic viscosity of colloid aqueous solution is 100～600mm
2/ s.
2, in accordance with the method for claim 1, the preparation process that it is characterized in that described emulsion splitter A is as follows: with acrylamide monomer and dimethylaminoethyl methacrylate monomer is main raw material, at first at 60 ℃～80 ℃, distillation purifying methyl acrylic dimethylaminoethyl monomer under negative pressure 0.092～0.097MPa condition, in the dimethylaminoethyl methacrylate monomer after the quaternizing agent adding purification, and obtain quaternized monomer, then with acrylamide, the quaternized monomer of dimethylaminoethyl methacrylate, after deionized water mixes by a certain percentage, nitrogen blowing is removed dissolved oxygen, adds initiator at last and carries out polyreaction.
3, in accordance with the method for claim 2, it is characterized in that the quaternized monomeric polymeric mol ratio of described acrylamide and dimethylaminoethyl methacrylate is, acrylamide: dimethylaminoethyl methacrylate=10: 1～1: 10, the total concn of monomer polymerization is: 0.5～1.5mol/L, the polymeric temperature of reaction is: 20～90 ℃, polymerization reaction time is 1～10h.
4, in accordance with the method for claim 1, it is characterized in that the preparation process of described flocculating agent B is as follows: fresh water is added in the reactor, under condition of stirring, equably negatively charged ion or non-ionic polyacrylamide are added in the reactor; After treating that it dissolves fully, add mineral alkali, adjust the pH value of solution; Add sequestrant then, control reaction temperature adds formaldehyde, sodium bisulfite in the reactor, behind the reaction certain hour, adds the terminator stopped reaction, can obtain flocculating agent B.
5, in accordance with the method for claim 4, the mole proportioning that it is characterized in that described each raw material is negatively charged ion or non-ionic polyacrylamide: formaldehyde: sodium bisulfite: fresh water: auxiliary agent: terminator=1: 0.5～2.5: 0.5～2.5: 100～5000: 0.005～0.05: 10～500.
6, in accordance with the method for claim 4, it is characterized in that described mineral alkali is a kind of of sodium hydroxide, potassium hydroxide; Auxiliary agent is edta and its sodium salt, ethylene diaminetetraacetic acid and sodium salt thereof or diethylenediamine pentaacetic acid and sodium salt thereof; Terminator is that hydrochloric acid, vitriolic are a kind of.
7, in accordance with the method for claim 4, the pH value that it is characterized in that described adding mineral alkali adjustment solution is controlled between 7～14, temperature of reaction is controlled between 20 ℃～80 ℃, the dissolution time of negatively charged ion or non-ionic polyacrylamide is controlled at 1h～6h, and the reaction times is controlled at 2h～10h.
8, in accordance with the method for claim 1, it is characterized in that described static disengaging time is 5 minutes～5 hours.
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| CN102887580B (en) * | 2011-07-21 | 2014-03-05 | 克拉玛依奥克化学有限公司 | Preparation method of high salinity heavy oil sewage deoiling water purifier |
| CN102689941B (en) * | 2012-05-29 | 2013-12-25 | 中国海洋石油总公司 | Method for treating sewage in polymer flooding oilfield |
| CN102951702A (en) * | 2012-11-13 | 2013-03-06 | 山东泰德新能源有限公司 | Crude-oil sewage treating agent |
| CN105271466B (en) * | 2014-07-11 | 2018-03-20 | 中国石油化工股份有限公司 | Oil-containing dross dehydration agent and preparation method thereof |
| CN104492400B (en) * | 2014-12-23 | 2017-12-29 | 马鞍山金泉工业介质科技有限公司 | A kind of water treatment absorbent and its preparation method and application |
| CN105347453A (en) * | 2015-11-12 | 2016-02-24 | 威海翔宇环保科技股份有限公司 | Processing technology of mixed liquid containing various plant oils and used for carpet industry |
| CN105417781B (en) * | 2015-12-09 | 2018-05-08 | 中国海洋石油集团有限公司 | A kind of processing method of high oil-containing polymer-bearing waste-water |
| CN105540919A (en) * | 2015-12-16 | 2016-05-04 | 杭州富阳伟文环保科技有限公司 | Tar-containing wastewater treatment method |
| CN107345950A (en) * | 2016-05-06 | 2017-11-14 | 中国石油化工股份有限公司 | Oil field extracted water flocculant evaluation method |
| CN107188334A (en) * | 2017-06-27 | 2017-09-22 | 山东新美达科技材料有限公司 | Waste emulsified mixture processing method and processing system |
| CN114308402A (en) * | 2022-01-14 | 2022-04-12 | 湖南新田岭钨业有限公司 | Flocculation sedimentation process for flotation tungsten ore tailings |
| CN115196733B (en) * | 2022-07-20 | 2023-10-31 | 克拉玛依新科澳石油天然气技术股份有限公司 | Oilfield sewage treatment medicament and preparation method thereof |
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