CN105565449A - Pretreatment method of flown back fracturing fluid - Google Patents

Pretreatment method of flown back fracturing fluid Download PDF

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CN105565449A
CN105565449A CN201410534357.8A CN201410534357A CN105565449A CN 105565449 A CN105565449 A CN 105565449A CN 201410534357 A CN201410534357 A CN 201410534357A CN 105565449 A CN105565449 A CN 105565449A
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outlet liquid
viscosity
fracturing outlet
agent
fracturing
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CN105565449B (en
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高峰
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Sinopec Research Institute of Petroleum Processing
China Petroleum and Chemical Corp
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Sinopec Research Institute of Petroleum Processing
China Petroleum and Chemical Corp
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Abstract

The invention discloses a pretreatment method of a flown back fracturing fluid. The method comprises the following steps: 1, dividing flown back fracturing fluids to be treated into a flown back fracturing fluid with the viscosity being smaller than 1.5mpa.s, a flown back fracturing fluid with the viscosity of 1.5-3mpa.s and a flown back fracturing fluid with the viscosity being greater than 3mpa.s according to the viscosity size; 2, adding a flocculating agent to the flown back fracturing fluid with the viscosity being smaller than 1.5mpa.s to carry out flocculation precipitation treatment; 3, adding a floating agent to the flown back fracturing fluid with the viscosity of 1.5-3mpa.s to carry out air floatation treatment; and 4, adding a viscosity reducer to the flown back fracturing fluid with the viscosity being greater than 3mpa.s to carry out viscosity reduction treatment, and carrying out flocculation precipitation treatment or air floatation treatment according to the viscosity size when the viscosity of the flown back fracturing fluid for viscosity reduction treatment is not greater than 3mpa.s. The method has the advantages of low consumption of a medicine, low treatment cost, strong pertinence, and excellent oil and turbidity removal effect.

Description

A kind of pretreatment process of fracturing outlet liquid
Technical field
The present invention relates to field of waste water treatment, particularly, relate to a kind of pretreatment process of fracturing outlet liquid.
Background technology
Along with countries in the world are for the continuous increase of energy demand and the day by day exhausted of conventional gas and oil resource, the exploitation of the unconventional petroleum resourceses such as tight sand oil gas, shale oil gas, coal-seam gas is more and more paid attention to.The exploitation of unconventional petroleum resources adopts horizontal well multistage subsection fracturing technique usually, thus needs to adopt a large amount of fracturing liquids.The fracturing liquid adopted in existing fracturing technique is mainly divided into aqueous fracturing fluid, oil base fracturing fluid and foamed fracturing fluid etc.And aqueous fracturing fluid is use fracturing liquid the most general at present because effective, cost is low.According to the difference of geologic condition, water-based fracturing liquid system is divided into again slippery water (riverfrac treatment) system, linear colloid system and jelly system.In the recovery process of conventional oil reservoir and unconventional tight sandstone reservoir, being particularly that the frozen glue pressure break system of thickening material has the features such as treatment effect is good with modifyed guar gum due to jelly system, is current the most widely used fracturing liquid.
The performance history of the nontraditional reservoir such as tight sand have fluid volume large, return the large feature of lifting rate, consequent a large amount of fracturing waste liquor, complicated component, suspended substance and oil-contg high, variation water quality is large, difficult treatment, environmental pollution is serious, has become in the exploitation of current unconventional (oil) gas without one of avoidable technical bottleneck.
At present, research both at home and abroad about fracturing outlet liquid process mainly concentrates on oxidation, flocculate and multiple technologies coupling in, as: patent application CN102701486A proposes a kind of combination treatment method for shale gas fracturing waste water, the method adopts the suites of measure process waste water such as coagulation, electrolytic oxidation, second coagulation, catalytic ozonation, and water outlet can reach the water quality requirement of outer row and re-injection.
Owing to containing a large amount of oil and suspended substance in fracturing outlet liquid, to be no matter fracturing outlet liquid after process carry out reuse or re-injection bottom or outer row for pressure break dosing water all needs oil in removal fracturing outlet liquid and suspended substance, and in existing method, oil removing is carried out to fracturing outlet liquid, when going turbid process, especially oil removing is carried out to the fracturing outlet liquid of the larger jelly system of viscosity fluctuation, when going turbid process, no matter be adopt broken glue, flocculation, the treatment process of air supporting or several technique coupling, gel breaker, the consumption of the medicaments such as flocculation agent is all higher, especially the dosage of flocculation agent usually can reach several thousand ppm, not only with high costs, but also the sediment that flocculates in a large number can be produced, cause secondary pollution and oil removing and go turbid effect to have much room for improvement.Therefore, research and develop that a kind of reagent consumption amount is few, processing cost is low, there is excellent oil removing for different quality strong adaptability and remove the pretreatment process of fracturing outlet liquid of turbid effect, have important practical significance.
Summary of the invention
When the method that the object of the invention is to overcome prior art is carried out oil removing to fracturing outlet liquid and goes turbid process, reagent consumption amount is high, processing cost is high, oil removing poor to different quality specific aim and the defect of going turbid effect to have much room for improvement, a kind of pretreatment process of fracturing outlet liquid is provided, the method reagent consumption amount is low, processing cost is low, with strong points to different quality, and there is excellent oil removing and go turbid effect.
The present inventor surprisingly finds under study for action, when carrying out pre-treatment to fracturing outlet liquid, by being divided into viscosity to be less than 1.5mpa.s according to the pending fracturing outlet liquid of the large young pathbreaker of viscosity, viscosity is the fracturing outlet liquid that 1.5-3mpa.s and viscosity are greater than 3mpa.s, then be less than in the fracturing outlet liquid of 1.5mpa.s in viscosity respectively and add flocculation agent and carry out flocculation sediment process, be add flotation agent in the fracturing outlet liquid of 1.5-3mpa.s to carry out air-flotation process in viscosity, be greater than in viscosity in the fracturing outlet liquid of 3mpa.s and add viscosity-depression agent and carry out viscosity reduction process, when the viscosity of the fracturing outlet liquid after viscosity reduction process is not more than 3mpa.s, the method of flocculation sediment process or air-flotation process is carried out again according to viscosity size, obviously can reduce the consumption of medicament, reduce processing cost, with strong points to different quality, and there is excellent oil removing and go turbid effect.
Therefore, to achieve these goals, the invention provides a kind of pretreatment process of fracturing outlet liquid, said method comprising the steps of:
(1) be divided into according to the fracturing outlet liquid that the large young pathbreaker of viscosity is pending that viscosity is less than 1.5mpa.s, viscosity is the fracturing outlet liquid that 1.5-3mpa.s and viscosity are greater than 3mpa.s;
(2) be less than in viscosity and add flocculation agent in the fracturing outlet liquid of 1.5mpa.s and carry out flocculation sediment process;
(3) in viscosity be 1.5-3mpa.s fracturing outlet liquid in add flotation agent and carry out air-flotation process;
(4) be greater than in viscosity and add viscosity-depression agent in the fracturing outlet liquid of 3mpa.s and carry out viscosity reduction process, when the viscosity of the fracturing outlet liquid after viscosity reduction process is not more than 3mpa.s, then carry out flocculation sediment process or air-flotation process according to viscosity size.
Compared with prior art, treatment process technique of the present invention is simple, easy enforcement, obviously can reduce the consumption of medicament needed for process fracturing outlet liquid, reduce processing cost, with strong points to different quality, and there is excellent oil removing and go turbid effect, significantly can reduce the suspension content in fracturing outlet liquid and oil-contg.
Other features and advantages of the present invention are described in detail in embodiment part subsequently.
Embodiment
Below the specific embodiment of the present invention is described in detail.Should be understood that, embodiment described herein, only for instruction and explanation of the present invention, is not limited to the present invention.
The invention provides a kind of pretreatment process of fracturing outlet liquid, the method comprises the following steps:
(1) be divided into according to the fracturing outlet liquid that the large young pathbreaker of viscosity is pending that viscosity is less than 1.5mpa.s, viscosity is the fracturing outlet liquid that 1.5-3mpa.s and viscosity are greater than 3mpa.s;
(2) be less than in viscosity and add flocculation agent in the fracturing outlet liquid of 1.5mpa.s and carry out flocculation sediment process;
(3) in viscosity be 1.5-3mpa.s fracturing outlet liquid in add flotation agent and carry out air-flotation process;
(4) be greater than in viscosity and add viscosity-depression agent in the fracturing outlet liquid of 3mpa.s and carry out viscosity reduction process, when the viscosity of the fracturing outlet liquid after viscosity reduction process is not more than 3mpa.s, then carry out flocculation sediment process or air-flotation process according to viscosity size.
In the inventive method, for the method for the viscosity detecting pending fracturing outlet liquid, there is no particular limitation, and the various methods can commonly used for this area can be such as brookfield viscosity assay method.
In the inventive method, be divided into by pending fracturing outlet liquid the method for the fracturing outlet liquid of different viscosity size to be conventionally known to one of skill in the art, do not repeat them here.
In the inventive method, for flocculation agent, there is no particular limitation, the various flocculation agents can commonly used for this area, in order to can reduce further medicament consumption, reduce processing cost and improve the oil removing of fracturing outlet liquid and go turbid effect, under preferable case, flocculation agent comprises inorganic flocculating agent and organic floculant, further preferably, inorganic flocculating agent is the mixture of polyaluminium sulfate and bodied ferric sulfate, and organic floculant is anionic polyacrylamide.For anionic polyacrylamide, there is no particular limitation, and the various anionic polyacrylamides can commonly used for this area, under preferable case, the molecular weight of anionic polyacrylamide is 8,000,000-1,200 ten thousand.
In the inventive method, in order to can improve the oil removing of fracturing outlet liquid further and go turbid effect, under preferable case, relative to often liter of fracturing outlet liquid, the dosage of flocculation agent is 10-2000mg, more preferably 20-1000mg, more more preferably 100-500mg; More preferably, the weight ratio of polyaluminium sulfate, bodied ferric sulfate and anionic polyacrylamide is 1:0.1-1:0.005-0.05.
In the inventive method, in order to can improve the oil removing of fracturing outlet liquid further and go turbid effect, under preferable case, the condition of flocculation sediment process comprises: the time of flocculating settling is 5-300 minute, more preferably 10-180 minute, is more preferably 30-120 minute; The pH value of fracturing outlet liquid is 6-9.
In the inventive method, for flotation agent, there is no particular limitation, the various flotation agent can commonly used for this area, in order to can reduce further medicament consumption, reduce processing cost and improve the oil removing of fracturing outlet liquid and go turbid effect, under preferable case, flotation agent comprises Inorganic floatation agent and organic flotation agent, further preferably, Inorganic floatation agent is the mixture of Tai-Ace S 150 and polymerize aluminum chloride, and organic flotation agent is anionic polyacrylamide.For anionic polyacrylamide, there is no particular limitation, and the various anionic polyacrylamides can commonly used for this area, under preferable case, the molecular weight of anionic polyacrylamide is 8,000,000-1,200 ten thousand.
In the present invention, molecular weight all refers to viscosity-average molecular weight.
In the inventive method, in order to can improve the oil removing of fracturing outlet liquid further and go turbid effect, under preferable case, relative to often liter of fracturing outlet liquid, the dosage of flotation agent is 10-1000mg, more preferably 20-500mg, more more preferably 50-300mg; More preferably, the weight ratio of polymerize aluminum chloride, Tai-Ace S 150 and anionic polyacrylamide is 1:0.05-0.8:0.01-0.1.
In the inventive method, in order to can improve the oil removing of fracturing outlet liquid further and go turbid effect, under preferable case, the condition of air-flotation process comprises: the residence time of fracturing outlet liquid in air supporting reactor is 3-180 minute, more preferably 5-120 minute, is more preferably 10-90 minute; The pH value of fracturing outlet liquid is 6-9.
In the inventive method, when carrying out flocculation sediment process and air-flotation process, for regulating the method for pH value of fracturing outlet liquid, there is no particular limitation, as long as the pH value of fracturing outlet liquid can be adjusted to 6-9.Such as, can by adding acid or alkali regulates, acid can be one or more in sulfuric acid, hydrochloric acid, nitric acid and acetic acid, and alkali can be one or more in sodium hydroxide, potassium hydroxide and ammoniacal liquor.
In the inventive method, for viscosity-depression agent, there is no particular limitation, the various viscosity-depression agents can commonly used for this area, in order to consumption, the reduction processing cost also viscosity reduction treatment effect of raising to fracturing outlet liquid of medicament can be reduced further, under preferable case, viscosity-depression agent comprises oxygenant, catalyzer and acid, further preferably, oxygenant is one or more in hydrogen peroxide, hypochlorite, ozone and persulphate, is more preferably persulphate; Catalyzer is one or more in soluble metallic salt, is more preferably ferrous salt; Acid is one or more in sulfuric acid, hydrochloric acid, nitric acid and acetic acid, is more preferably hydrochloric acid and acetic acid.For hypochlorite, persulphate and ferrous salt, there is no particular limitation, various hypochlorites, persulphate and ferrous salt that this area is conventional can be respectively, such as, hypochlorite can be one or more in potassium hypochlorite, clorox and Losantin, persulphate can be one or more in Potassium Persulphate, Sodium Persulfate and ammonium persulphate, and ferrous salt can be one or more in iron protochloride, ferrous sulfate and Iron nitrate.
In the inventive method, in order to strengthen the effect of viscosity reduction process further, under preferable case, viscosity-depression agent also comprises activator.For promoting agent, there is no particular limitation, can be the conventional various activators in this area, and under preferable case, activator is one or more in organic reducing agent, more preferably trolamine.
In the inventive method, in order to the viscosity reduction treatment effect to fracturing outlet liquid can be improved further, under preferable case, relative to often liter of fracturing outlet liquid, the total amount that adds of oxygenant, catalyzer and activator is 30-3000mg, more preferably 50-2000mg, is more preferably 100-1000mg; The weight ratio of oxygenant, catalyzer and activator is 1:0.1-10:0.005-0.1, more preferably 1:0.3-3:0.01-0.05; The amount of the acid added in fracturing outlet liquid makes the pH value of fracturing outlet liquid be preferably 0.5-6, more preferably 1-4, then a step is preferably 2-3, still more preferably, the hydrochloric acid added in fracturing outlet liquid and the weight ratio of acetic acid are 1:0.3-2, are more preferably 1:0.5-1.
In the inventive method, under preferable case, the time of viscosity reduction process is 5-360 minute, more preferably 10-180 minute, is more preferably 15-120 minute.
In the inventive method, the process of one or many viscosity reduction can be carried out, until by the viscosity drop of fracturing outlet liquid to being not more than 3mpa.s to the fracturing outlet liquid that viscosity is greater than 3mpa.s.
In the inventive method, under preferable case, the fracturing outlet liquid that pending fracturing outlet liquid produces for adopting the fracturing liquid of jelly system.Further preferably, the viscosity of pending fracturing outlet liquid is 1-20mpa.s; Oil-contg is 0-3000mg/L, is further preferably 10-1000mg/L; Suspension content is 0-2000mg/L, is further preferably 30-1500mg/L.
Embodiment
The present invention is further illustrated for following embodiment, but therefore do not limit the present invention.
In following examples and comparative example:
The mensuration of suspended substance adopts weighting method (GB11901-89), and the mensuration of oil-contg adopts " in oil field extracted water determination method for oil content (SY/T0530-2011) ".
The detection method of the viscosity of fracturing outlet liquid is brookfield viscosity assay method.
Flocculation agent used and flotation agent are all purchased from Beijing Lin Hua water quality stabilizer factory, and wherein, the molecular weight of anionic polyacrylamide is 9,000,000.
Embodiment 1
The present embodiment is for illustration of the pretreatment process of fracturing outlet liquid of the present invention.
(1) fracturing outlet liquid (fracturing outlet liquid for adopting the fracturing liquid of jelly system to produce) that pending fracturing outlet liquid produces for Gu Dong oil recovery factory tight sand oil well, detect the viscosity of pending fracturing outlet liquid, viscosity is greater than the fracturing outlet liquid that fracturing outlet liquid between 1.5-3mpa.s of the fracturing outlet liquid of 3mpa.s, viscosity and viscosity is less than 1.5mpa.s to deposit respectively to tank 1, tank 2 and tank 3, the water-quality guideline in each tank is in table 1.
Table 1
Tank is numbered 1 2 3
Account for the weight ratio of total fracturing outlet liquid 39 26 35
Viscosity (mpa.s) 8.08 2.38 1.13
Suspension content/mg/L 630 940 580
Oil-contg/mg/L 28 73 229
PH value 7.88 8.12 8.93
(2) flocculating settling process is carried out to the fracturing outlet liquid in tank 3: the pH value of the fracturing outlet liquid in tank 3 is adjusted to 7 by the hydrochloric acid soln with 36.5 % by weight, relative to often liter of fracturing outlet liquid in tank 3,150mg polyaluminium sulfate, 50mg bodied ferric sulfate and 5mg anion-polyacrylamide is added, flocculating settling 60 minutes in fracturing outlet liquid.Suspension content in fracturing outlet liquid after flocculating settling process is 20mg/L, and oil-contg is 2mg/L.
(3) air-flotation process is carried out to the fracturing outlet liquid in tank 2: the pH value of the fracturing outlet liquid in tank 2 is adjusted to 7 by the hydrochloric acid soln with 36.5 % by weight, relative to often liter of fracturing outlet liquid in tank 2, in fracturing outlet liquid, add 200mg polymerize aluminum chloride, 30mg Tai-Ace S 150 and 13mg anion-polyacrylamide, and the residence time of fracturing outlet liquid in air supporting reactor is controlled to be 15 minutes.Suspension content in fracturing outlet liquid after air-flotation process is 30mg/L, and oil-contg is 7mg/L.
(4) viscosity reduction process is carried out to the fracturing outlet liquid in tank 1: with the mixed acid solution (weight ratio of hydrochloric acid and acetic acid is 1:0.8) of hydrochloric acid and acetic acid, the pH value of the fracturing outlet liquid in tank 1 is adjusted to 2.5, relative to often liter of fracturing outlet liquid in tank 1, in fracturing outlet liquid, add 300mg Potassium Persulphate, 200mg ferrous sulfate and 5mg trolamine, react 45 minutes.The viscosity of the detection fracturing outlet liquid after viscosity reduction process is 2.73mpa.s, and pH value is 2.3.
Air-flotation process is carried out to the fracturing outlet liquid that viscosity reduction process obtains: the pH regulator of the fracturing outlet liquid that viscosity reduction process obtains by the sodium hydroxide solution with 30 % by weight is 7, relative to being often elevated the fracturing outlet liquid gluing and process and obtain, in fracturing outlet liquid, add 200mg polymerize aluminum chloride, 40mg Tai-Ace S 150 and 15mg anion-polyacrylamide, and the residence time of fracturing outlet liquid in air supporting reactor is controlled to be 20 minutes.Suspension content in fracturing outlet liquid after air-flotation process is 18mg/L, and oil-contg is 12mg/L.
Embodiment 2
The present embodiment is for illustration of the pretreatment process of fracturing outlet liquid of the present invention.
According to the method for embodiment 1, unlike, step (2)-(4) are as follows respectively:
(2) flocculating settling process is carried out to the fracturing outlet liquid in tank 3: the pH value of the fracturing outlet liquid in tank 3 is adjusted to 6 by the hydrochloric acid soln with 36.5 % by weight, relative to often liter of fracturing outlet liquid in tank 3,452.5mg polyaluminium sulfate, 45.25mg bodied ferric sulfate and 2.25mg anion-polyacrylamide is added, flocculating settling 30 minutes in fracturing outlet liquid.Suspension content in fracturing outlet liquid after flocculating settling process is 15mg/L, and oil-contg is 1.2mg/L.
(3) air-flotation process is carried out to the fracturing outlet liquid in tank 2: the pH value of the fracturing outlet liquid in tank 2 is adjusted to 9 by the sodium hydroxide solution with 30 % by weight, relative to often liter of fracturing outlet liquid in tank 2, in fracturing outlet liquid, add 283mg polymerize aluminum chloride, 14.15mg Tai-Ace S 150 and 2.85mg anion-polyacrylamide, and the residence time of fracturing outlet liquid in air supporting reactor is controlled to be 10 minutes.Suspension content in fracturing outlet liquid after air-flotation process is 26mg/L, and oil-contg is 5mg/L.
(4) viscosity reduction process is carried out to the fracturing outlet liquid in tank 1: with the mixed acid solution (weight ratio of hydrochloric acid and acetic acid is 1:0.5) of hydrochloric acid and acetic acid, the pH value of the fracturing outlet liquid in tank 1 is adjusted to 2, relative to often liter of fracturing outlet liquid in tank 1, in fracturing outlet liquid, add 763.3mg Sodium Persulfate, 229mg iron protochloride and 7.7mg trolamine, react 15 minutes.The viscosity detecting fracturing outlet liquid after viscosity reduction process is 2.1mpa.s, and pH value is 1.9.
Air-flotation process is carried out to the fracturing outlet liquid that viscosity reduction process obtains: the pH regulator of the fracturing outlet liquid that viscosity reduction process obtains by the sodium hydroxide solution with 30 % by weight is 9, relative to being often elevated the fracturing outlet liquid gluing and process and obtain, in fracturing outlet liquid, add 100mg polymerize aluminum chloride, 50mg Tai-Ace S 150 and 50mg anion-polyacrylamide, and the residence time of fracturing outlet liquid in air supporting reactor is controlled to be 40 minutes.Suspension content in fracturing outlet liquid after air-flotation process is 26mg/L, and oil-contg is 19mg/L.
Embodiment 3
The present embodiment is for illustration of the pretreatment process of fracturing outlet liquid of the present invention.
According to the method for embodiment 1, unlike, step (2)-(4) are as follows respectively:
(2) flocculating settling process is carried out to the fracturing outlet liquid in tank 3: the pH value of the fracturing outlet liquid in tank 3 is adjusted to 9 by the sodium hydroxide solution with 30 % by weight, relative to often liter of fracturing outlet liquid in tank 3,48.8mg polyaluminium sulfate, 48.8mg bodied ferric sulfate and 2.4mg anion-polyacrylamide is added, flocculating settling 120 minutes in fracturing outlet liquid.Suspension content in fracturing outlet liquid after flocculating settling process is 35mg/L, and oil-contg is 16mg/L.
(3) air-flotation process is carried out to the fracturing outlet liquid in tank 2: the pH value of the fracturing outlet liquid in tank 2 is adjusted to 6 by the acetum with 36.5 % by weight, relative to often liter of fracturing outlet liquid in tank 2, in fracturing outlet liquid, add 26.3mg polymerize aluminum chloride, 21.05mg Tai-Ace S 150 and 2.65mg anion-polyacrylamide, and the residence time of fracturing outlet liquid in air supporting reactor is controlled to be 90 minutes.Suspension content in fracturing outlet liquid after air-flotation process is 36mg/L, and oil-contg is 21mg/L.
(4) viscosity reduction process is carried out to the fracturing outlet liquid in tank 1: with the mixed acid solution (weight ratio of hydrochloric acid and acetic acid is 1:1) of hydrochloric acid and acetic acid, the pH value of the fracturing outlet liquid in tank 1 is adjusted to 3, relative to often liter of fracturing outlet liquid in tank 1, in fracturing outlet liquid, add 24.7mg ammonium persulphate, 74.1mg Iron nitrate and 1.2mg trolamine, react 120 minutes.The viscosity detecting fracturing outlet liquid after viscosity reduction process is 2.6mpa.s, and pH value is 2.7.
Air-flotation process is carried out to the fracturing outlet liquid that viscosity reduction process obtains: the pH regulator of the fracturing outlet liquid that viscosity reduction process obtains by the sodium hydroxide solution with 30 % by weight is 6, relative to being often elevated the fracturing outlet liquid gluing and process and obtain, in fracturing outlet liquid, add 200mg polymerize aluminum chloride, 80mg Tai-Ace S 150 and 120mg anion-polyacrylamide, and the residence time of fracturing outlet liquid in air supporting reactor is controlled to be 7 minutes.Suspension content in fracturing outlet liquid after air-flotation process is 35mg/L, and oil-contg is 26mg/L.
Embodiment 4
The present embodiment is for illustration of the pretreatment process of fracturing outlet liquid of the present invention.
According to the method for embodiment 1, unlike, step (2)-(4) are as follows respectively:
(2) flocculating settling process is carried out to the fracturing outlet liquid in tank 3: the pH value of the fracturing outlet liquid in tank 3 is adjusted to 7 by the hydrochloric acid soln with 36.5 % by weight, relative to often liter of fracturing outlet liquid in tank 3,657.9mg polyaluminium sulfate molecular weight, 328.9mg bodied ferric sulfate and 13.2mg anion-polyacrylamide is added, flocculating settling 15 minutes in fracturing outlet liquid.Suspension content in fracturing outlet liquid after flocculating settling process is 21mg/L, and oil-contg is 10mg/L.
(3) air-flotation process is carried out to the fracturing outlet liquid in tank 2: the pH value of the fracturing outlet liquid in tank 2 is adjusted to 6 by the hydrochloric acid soln with 36.5 % by weight, relative to often liter of fracturing outlet liquid in tank 2, in fracturing outlet liquid, add 400mg polymerize aluminum chloride, 80mg Tai-Ace S 150 and 20mg anion-polyacrylamide, and the residence time of fracturing outlet liquid in air supporting reactor is controlled to be 8 minutes.Suspension content in fracturing outlet liquid after air-flotation process is 34mg/L, and oil-contg is 16mg/L.
(4) viscosity reduction process is carried out to the fracturing outlet liquid in tank 1: with the mixed acid solution (weight ratio of hydrochloric acid and acetic acid is 1:1.5) of hydrochloric acid and acetic acid, the pH value of the fracturing outlet liquid in tank 1 is adjusted to 4, relative to often liter of fracturing outlet liquid in tank 1, in fracturing outlet liquid, add 246mg clorox, 1229.4mg ferrous sulfate and 24.6mg trolamine, react 10 minutes.The viscosity detecting fracturing outlet liquid after viscosity reduction process is 1.4mpa.s, and pH value is 3.5.
Flocculation sediment process is carried out to the fracturing outlet liquid that viscosity reduction process obtains: the pH regulator of the fracturing outlet liquid that viscosity reduction process obtains by the sodium hydroxide solution with 30 % by weight is 6, relative to being often elevated the fracturing outlet liquid gluing and process and obtain, 139mg polyaluminium sulfate, 55.5mg bodied ferric sulfate and 5.5mg anion-polyacrylamide is added, flocculating settling 40 minutes in fracturing outlet liquid.Suspension content in fracturing outlet liquid after flocculating settling process is 32mg/L, and oil-contg is 13mg/L.
Embodiment 5
According to the method for embodiment 1, unlike, in step (2), do not add bodied ferric sulfate, relative to often liter of fracturing outlet liquid in tank 3, the amount of the polyaluminium sulfate added is 200mg.Suspension content in fracturing outlet liquid after flocculating settling process is 60mg/L, and oil-contg is 8mg/L.
Embodiment 6
According to the method for embodiment 1, unlike, in step (3), do not add Tai-Ace S 150, relative to often liter of fracturing outlet liquid in tank 2, the amount of the polymerize aluminum chloride added is 230mg.Suspension content in fracturing outlet liquid after air-flotation process is 80mg/L, and oil-contg is 15mg/L.
Embodiment 7
According to the method for embodiment 1, unlike, in step (4), when carrying out viscosity reduction process, do not add trolamine.The viscosity detecting fracturing outlet liquid after viscosity reduction process is 4.38mpa.s, need proceed viscosity reduction process.
Embodiment 8
According to the method for embodiment 1, unlike, in step (4), when carrying out viscosity reduction process, the pH value of the fracturing outlet liquid in tank 1 is adjusted to 2.5 by the hydrochloric acid soln with 36.5 % by weight.The viscosity detecting fracturing outlet liquid after viscosity reduction process is 3.26mpa.s, need proceed viscosity reduction process.
Comparative example 1
According to the method for embodiment 1, unlike, during pending fracturing outlet liquid in Processing Example 1, dual treatment is not carried out according to viscosity size, but all fracturing outlet liquids are all collected in a homogeneous tank, in tank, the water-quality guideline of fracturing outlet liquid is as follows: viscosity is 4.23mpa.s, and suspension content is 715mg/L, oil-contg is 83mg/L, and pH value is 8.32.Then carry out viscosity reduction process according to embodiment 1 step (4), the viscosity detecting fracturing outlet liquid after viscosity reduction process is 2.65mpa.s.Carry out air-flotation process according to embodiment 1 step (3) to the fracturing outlet liquid after viscosity reduction process again, the suspension content in the fracturing outlet liquid after air-flotation process is 36mg/L, and oil-contg is 18mg/L.
Comparative example 2
According to the method for embodiment 1, unlike, in step (2), air-flotation process is carried out to the fracturing outlet liquid in tank 3: the pH value of the fracturing outlet liquid in tank 3 is adjusted to 7 by the hydrochloric acid soln with 36.5 % by weight, relative to often liter of fracturing outlet liquid in tank 3, in fracturing outlet liquid, add 200mg polymerize aluminum chloride, 30mg Tai-Ace S 150 and 13mg anion-polyacrylamide, and the residence time of fracturing outlet liquid in air supporting reactor is controlled to be 15 minutes.Suspension content in fracturing outlet liquid after air-flotation process is 120mg/L, and oil-contg is 6mg/L.
Comparative example 3
According to the method for embodiment 1, unlike, in step (3), flocculating settling process is carried out to the fracturing outlet liquid in tank 2: the pH value of the fracturing outlet liquid in tank 2 is adjusted to 7 by the hydrochloric acid soln with 36.5 % by weight, relative to often liter of fracturing outlet liquid in tank 2,150mg polyaluminium sulfate, 50mg bodied ferric sulfate and 5mg anion-polyacrylamide is added, flocculating settling 60 minutes in fracturing outlet liquid.Suspension content in fracturing outlet liquid after flocculating settling process is 350mg/L, and oil-contg is 32mg/L.
Embodiment 1 is more known with comparative example 1, the method of embodiment 1 carries out dual treatment to pending fracturing outlet liquid, the fracturing outlet liquid of 39% is only had to need to carry out viscosity reduction process, fracturing outlet liquid is being carried out in pretreated whole process, the consumption of medicament is significantly reduced, and has better oil removing and go turbid effect.
Embodiment 1 is more known with comparative example 2, and carry out compared with air-flotation process, fracturing outlet liquid viscosity being less than to 1.5mpa.s carries out flocculation sediment process, has obviously better oil removing and goes turbid effect.
Embodiment 1 is more known with comparative example 3, and carry out compared with flocculation sediment process, carrying out air-flotation process to the fracturing outlet liquid that viscosity is 1.5-3mpa.s, there is obviously better oil removing and go turbid effect.
Embodiment 1 is more known with embodiment 5, when the inorganic flocculating agent in flocculation agent is the mixture of polyaluminium sulfate and bodied ferric sulfate, there is obviously better oil removing and go turbid effect.
Embodiment 1 is more known with embodiment 6, when the Inorganic floatation agent in flotation agent is the mixture of Tai-Ace S 150 and polymerize aluminum chloride, there is obviously better oil removing and go turbid effect.
Embodiment 1 is more known with embodiment 7, when viscosity-depression agent comprises activator, there is obviously better viscosity reducing effect.
Embodiment 1 is more known with embodiment 8, the acid in viscosity-depression agent be hydrochloric acid and acetic acid time, there is obviously better viscosity reducing effect.
Treatment process technique of the present invention is simple, easy enforcement, obviously can reduce the consumption of medicament needed for process fracturing outlet liquid, reduce processing cost, with strong points to different quality, and there is excellent oil removing and go turbid effect, significantly can reduce the suspension content in fracturing outlet liquid and oil-contg.
More than describe the preferred embodiment of the present invention in detail; but the present invention is not limited to the detail in above-mentioned embodiment, within the scope of technical conceive of the present invention; can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.
It should be noted that in addition, each concrete technical characteristic described in above-mentioned embodiment, in reconcilable situation, can be combined by any suitable mode, in order to avoid unnecessary repetition, the present invention illustrates no longer separately to various possible array mode.
In addition, also can carry out arbitrary combination between various different embodiment of the present invention, as long as it is without prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.

Claims (12)

1. a pretreatment process for fracturing outlet liquid, is characterized in that, the method comprises the following steps:
(1) be divided into according to the fracturing outlet liquid that the large young pathbreaker of viscosity is pending that viscosity is less than 1.5mpa.s, viscosity is the fracturing outlet liquid that 1.5-3mpa.s and viscosity are greater than 3mpa.s;
(2) be less than in viscosity and add flocculation agent in the fracturing outlet liquid of 1.5mpa.s and carry out flocculation sediment process;
(3) in viscosity be 1.5-3mpa.s fracturing outlet liquid in add flotation agent and carry out air-flotation process;
(4) be greater than in viscosity and add viscosity-depression agent in the fracturing outlet liquid of 3mpa.s and carry out viscosity reduction process, when the viscosity of the fracturing outlet liquid after viscosity reduction process is not more than 3mpa.s, then carry out flocculation sediment process or air-flotation process according to viscosity size.
2. method according to claim 1, wherein, described flocculation agent comprises inorganic flocculating agent and organic floculant; Preferably, described inorganic flocculating agent is the mixture of polyaluminium sulfate and bodied ferric sulfate, and described organic floculant is anionic polyacrylamide.
3. method according to claim 2, wherein, relative to often liter of fracturing outlet liquid, the dosage of described flocculation agent is 10-2000mg, is preferably 20-1000mg, more preferably 100-500mg; More preferably, the weight ratio of polyaluminium sulfate, bodied ferric sulfate and anionic polyacrylamide is 1:0.1-1:0.005-0.05.
4. method according to claim 3, wherein, the condition of described flocculation sediment process comprises: the time of flocculating settling is 5-300 minute, is preferably 10-180 minute, is more preferably 30-120 minute; The pH value of described fracturing outlet liquid is 6-9.
5. method according to claim 1, wherein, described flotation agent comprises Inorganic floatation agent and organic flotation agent, and preferably, described Inorganic floatation agent is the mixture of Tai-Ace S 150 and polymerize aluminum chloride, and described organic flotation agent is anionic polyacrylamide.
6. method according to claim 5, wherein, relative to often liter of fracturing outlet liquid, the dosage of described flotation agent is 10-1000mg, is preferably 20-500mg, more preferably 50-300mg; More preferably, the weight ratio of polymerize aluminum chloride, Tai-Ace S 150 and anionic polyacrylamide is 1:0.05-0.8:0.01-0.1.
7. method according to claim 6, wherein, the condition of described air-flotation process comprises: the residence time of fracturing outlet liquid in air supporting reactor is 3-180 minute, is preferably 5-120 minute, is more preferably 10-90 minute; The pH value of described fracturing outlet liquid is 6-9.
8. method according to claim 1, wherein, described viscosity-depression agent comprises oxygenant, catalyzer and acid, and preferably, described oxygenant is one or more in hydrogen peroxide, hypochlorite, ozone and persulphate, is more preferably persulphate; Described catalyzer is one or more in soluble metallic salt, is more preferably ferrous salt; Described acid is one or more in sulfuric acid, hydrochloric acid, nitric acid and acetic acid, is more preferably hydrochloric acid and acetic acid.
9. method according to claim 8, wherein, described viscosity-depression agent also comprises activator, and described activator is one or more in organic reducing agent, is preferably trolamine.
10. method according to claim 9, wherein, relative to often liter of fracturing outlet liquid, the total amount that adds of described oxygenant, catalyzer and activator is 30-3000mg, is preferably 50-2000mg, is more preferably 100-1000mg; The weight ratio of oxygenant, catalyzer and activator is 1:0.1-10:0.005-0.1, is preferably 1:0.3-3:0.01-0.05; The amount of the acid added in fracturing outlet liquid makes the pH value of fracturing outlet liquid be 0.5-6, be preferably 1-4, more preferably 2-3, more further preferably, the hydrochloric acid added in fracturing outlet liquid and the weight ratio of acetic acid is 1:0.3-2, most preferably are 1:0.5-1.
11. methods according to claim 10, wherein, the time of described viscosity reduction process is 5-360 minute, is preferably 10-180 minute, is more preferably 15-120 minute.
12. according to the method in claim 1-11 described in any one, wherein, the fracturing outlet liquid that described pending fracturing outlet liquid produces for adopting the fracturing liquid of jelly system, preferably, the viscosity of described pending fracturing outlet liquid is 1-20mpa.s, oil-contg is 0-3000mg/L, and suspension content is 0-2000mg/L.
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CN105645650A (en) * 2015-12-30 2016-06-08 哈尔滨工业大学 Method for efficiently and rapidly reducing viscosity of polymers in oil field polymer-bearing wastewater and ternary composite flooding water
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CN106318363A (en) * 2016-08-23 2017-01-11 烟台智本知识产权运营管理有限公司 Fracturing recovery fluid gel breaker and preparation method thereof
CN106318364A (en) * 2016-08-23 2017-01-11 烟台智本知识产权运营管理有限公司 Compound gel breaker and preparing method thereof
CN106350054A (en) * 2016-08-23 2017-01-25 烟台智本知识产权运营管理有限公司 Oil field fracturing fluid flow back liquid composite gel breaker and preparation method thereof
CN107226552A (en) * 2017-07-04 2017-10-03 中国石油化工股份有限公司 A kind of low temperature rapid preprocessing method for being crosslinked guanidine glue fracturing outlet liquid
CN109550517A (en) * 2018-10-12 2019-04-02 中国石油天然气股份有限公司 The purposes of the catalysis oxidation composition, method and composition that are handled for fracturing outlet liquid
CN109550518A (en) * 2018-10-12 2019-04-02 中国石油天然气股份有限公司 The purposes of the catalysis oxidation composition, method and composition that are handled for fracturing outlet liquid
CN110902875A (en) * 2019-11-19 2020-03-24 西安威尔电子有限责任公司 Oil-gas field produced water treatment system and method based on ozone air floatation device
CN111499040A (en) * 2020-04-26 2020-08-07 克拉玛依翎昊科技有限责任公司 Oil field fracturing flowback fluid reinjection treatment method
CN112479468A (en) * 2020-11-18 2021-03-12 三桶油环保科技(宜兴)有限公司 Two-stage magnetic method rapid separation treatment method for fracturing flow-back fluid
CN112479469A (en) * 2020-11-18 2021-03-12 三桶油环保科技(宜兴)有限公司 Separation agent and magnetic separation method for oilfield fracturing flowback fluid
CN113150789A (en) * 2020-12-30 2021-07-23 陕西品物皆春生态科技有限公司 Guar gum-humic acid type oil and gas field fracturing fluid flowback fluid water retention and sand fixation agent and preparation method and application thereof

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