CN107055888B - Shale gas flowback liquid multidimensional electrode treatment process - Google Patents

Shale gas flowback liquid multidimensional electrode treatment process Download PDF

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CN107055888B
CN107055888B CN201710521020.7A CN201710521020A CN107055888B CN 107055888 B CN107055888 B CN 107055888B CN 201710521020 A CN201710521020 A CN 201710521020A CN 107055888 B CN107055888 B CN 107055888B
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electrode
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shale gas
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pyrolusite
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CN107055888A (en
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梁宏
邱阳
任阳民
王兵
李永涛
任宏洋
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Southwest Petroleum University
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    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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    • C02F9/00—Multistage treatment of water, waste water or sewage
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/46104—Devices therefor; Their operating or servicing
    • C02F1/46109—Electrodes
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F11/00—Treatment of sludge; Devices therefor
    • C02F11/12—Treatment of sludge; Devices therefor by de-watering, drying or thickening
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/46104—Devices therefor; Their operating or servicing
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/463—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrocoagulation
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
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    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
    • C02F1/56—Macromolecular compounds
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    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F2001/007—Processes including a sedimentation step
    • C—CHEMISTRY; METALLURGY
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    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/46104—Devices therefor; Their operating or servicing
    • C02F1/46109—Electrodes
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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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    • C02F2301/00—General aspects of water treatment
    • C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00—Use of specific compounds during water treatment
    • C02F2305/02—Specific form of oxidant
    • C02F2305/023—Reactive oxygen species, singlet oxygen, OH radical

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Abstract

The invention belongs to the field of oil and gas field wastewater treatment, and particularly relates to a treatment process of shale gas flowback fluid in a shale gas development process, which comprises the steps of sand setting, chemical coagulation, electric flocculation treatment, multi-dimensional electrode treatment, desalination and the like. The method effectively removes various pollutants such as suspended matters, heavy metal ions, organic matters, a large amount of salts and the like in the return liquid through chemical coagulation, electric flocculation, multi-dimensional electrode method treatment and desalination treatment, has high treatment efficiency, is green and environment-friendly, obtains good economic and social benefits, and is worthy of popularization and application.

Description

Shale gas flowback liquid multidimensional electrode treatment process
Technical Field
The invention belongs to the field of oil and gas field wastewater treatment, and particularly relates to a treatment process of shale gas flowback fluid in a shale gas development process.
Background
Shale gas is an important unconventional natural gas resource that is produced from shale formations. The formation and enrichment of shale gas has its own unique characteristics that tend to be distributed in relatively thick, widely distributed shale and source rock formations within the basin. Compared with the conventional natural gas, shale gas development generally has the characteristics of long mining life and long production period, and most of gas-producing shale has wide distribution range and large thickness and generally contains gas, so that the shale gas well can produce gas at a stable rate for a long time.
The resource amount of the Chinese shale gas is about 15 trillion to 30 trillion cubic meters, which is approximately equivalent to the reserve amount of 28.3 trillion cubic meters in the United states, and the economic value is huge. On the other hand, the production cycle of shale gas is long, and the mining life of the shale gas can generally reach 30-50 years or more. The latest data of the federal geological survey bureau in the U.S. shows that the service life of the Barnett shale gas field in the basin of Watsburg in the U.S. is as long as 80-100 years. The long life of mining means that the value of exploitable exploitation is great, which also determines its strong development potential.
The core technology of shale gas exploitation at present is horizontal well drilling and a hydraulic fracturing method, but fracturing exploitation needs to consume a large amount of water resources, even if high flowback utilization rate is realized, the water consumption is more than 10 times of that of conventional natural gas, which can cause great influence on sustainable utilization of local water resources, so that the great consumption of the water resources also becomes a bottleneck restricting development of shale gas in China. Moreover, shale gas flowback fluid contains refractory organics, heavy metals and water-soluble salts, and if the shale gas flowback fluid is not properly treated, the shale gas flowback fluid is easy to pollute the surrounding environment
At present, most of domestic treatment of shale gas flowback liquid aims at reinjection, and the main process is to reinject the flowback liquid to the underground after centralized simple treatment (dosing, filtering and the like). This approach may result in soil and groundwater contamination, which is not a fundamental solution to the problem, but also a secondary pollution problem. With the increasing requirement for environmental protection, the improvement of the shale gas flowback liquid treatment process to achieve the standard emission is urgently needed at present.
CN106315903A discloses a treatment process of shale gas flowback fluid, which comprises the steps of pumping the shale gas flowback fluid into a coagulation reaction tank for chemical coagulation to remove suspended matters and colloidal particles in water. And (3) allowing the treated wastewater to enter an ozone tower for advanced oxidation treatment, adjusting the pH value of the oxidized effluent to 7-9, pumping the effluent into a reverse osmosis desalination device for desalination treatment, and allowing the treated water to reach the standard and be discharged and used for farm irrigation.
CN105621809A discloses a shale gas flowback liquid treatment process, which comprises the steps of firstly adding an inorganic coagulant for stirring, then adding a first organic coagulant and a second organic coagulant for continuous stirring, standing for precipitation, and realizing solid-liquid separation; and then carrying out gradient ozone catalytic oxidation treatment on the supernatant, treating the generated oxidation waste liquid by adopting an aeration biological filter technology, then discharging the oxidation waste liquid after UV sterilization, carrying out solid-liquid separation treatment on the generated coagulating sedimentation, returning the filtrate to the treatment process for cyclic treatment, backfilling or paving the mud cake after treatment, basically losing the pollution of the shale gas flowback liquid after treatment, and realizing the recycling of the waste, wherein the shale gas flowback liquid can be reinjected and can also be discharged after further treatment and reaching the standard.
How to safely and efficiently treat a large amount of fracturing flowback fluid and formation water with high salt content, and then recycle the fracturing flowback fluid, relieve the condition of water resource shortage in a shale gas development area, and avoid environmental pollution becomes a difficult problem which must be solved at present.
Disclosure of Invention
In order to solve the technical problems, the invention provides a shale gas flowback liquid multidimensional electrode treatment process, which treats suspended particles, heavy metal ions, organic matters, salt substances and the like in water through various levels of treatment devices and technologies, adopts a series of physical, chemical and electrochemical treatment steps, has good treatment effect, strong economy, simple process, high treatment efficiency and strong economical practicability, and realizes the standard treatment of shale gas flowback liquid.
The invention discloses a shale gas flowback fluid multidimensional electrode treatment process for solving the technical problems, which is characterized by comprising the following steps of: the method comprises the following steps:
(1) sand setting: removing large granular substances and rock debris in the shale gas flowback fluid; and removing larger suspended particles and rock debris in the shale gas flowback liquid through natural sedimentation.
(2) Chemical coagulation: adding a coagulating agent into the flowback liquid after sand settling in the step (1), adjusting the pH value to 6-8 in the coagulating process, and precipitating; firstly, adding a certain amount of polyaluminium chloride (PAC), stirring for a period of time, adding Polyacrylamide (PAM) with a certain concentration, and precipitating and removing colloidal suspended substances after the colloidal suspended substances are mutually flocculated to form large granular substances;
the concentration of the polyaluminium chloride is 30-40%, the concentration of the PAM is 0.1-0.5%, and the concentration and the addition are determined according to the change of water quality. Polyacrylamide (PAM) with a molecular weight of 800-2500 ten thousand.
(3) Electric flocculation treatment: carrying out electric flocculation treatment on the shale gas flowback liquid precipitated in the step (2), adjusting the pH to 7-9, removing heavy metal ions and oxidizing and degrading organic pollutants;
(4) and (3) multi-dimensional electrode treatment: carrying out multi-dimensional electrode treatment in a multi-dimensional electrode treatment device, wherein the electrolysis reaction is carried out under the conditions of aeration rate of 600mL/min, current intensity of 0.9A and electrolysis time of 60min, and organic pollutants difficult to degrade are removed;
(5) desalting: adjusting the pH value of the shale gas flowback liquid treated by the multidimensional electrode in the step (4) to 6-8, desalting by using a desalting device, wherein the operating pressure is 60kg/m2-70kg/m2And removing inorganic salt in the shale gas flowback liquid.
And (4) arranging particle electrodes which are pyrolusite fillers or ceramic pyrolusite fillers.
The particle electrode is made of pyrolusite filler and is a solid section formed by mixing, pressing and firing pyrolusite powder and graphite powder; wherein, the balance of 60 percent of pyrolusite powder by mass is graphite powder, the ignition temperature is 330 ℃, and the ignition time is 2 hours.
The ceramic pyrolusite filler is a solid section formed by mixing, pressing and firing pyrolusite powder, activated carbon powder, a sodium silicate adhesive and clay; wherein the mass ratio of the pyrolusite powder to the clay is 6-3:4-7, and the optimized ratio is 6: 4; adding 12 percent of activated carbon powder and 15 percent of sodium silicate adhesive by the total weight of the pyrolusite and the clay, wherein the firing temperature is 600 ℃, and the firing time is 2 hours.
The novel ceramic pyrolusite filler has the following effects: A. the activated carbon powder is added, so that the activated carbon powder has stronger adsorption capacity and can effectively improve the treatment effect; B. the selected adhesive is an inorganic adhesive, has stable chemical performance and better performance under high temperature and extreme electrolysis conditions; C. the ceramic particle electrode has better stability, and can still keep higher removal rate after being electrolyzed for multiple times, which shows that the service life of the particle electrode is obviously prolonged compared with other particle electrodes.
The particle electrode used in the present invention is formed by adding a ceramic material and calcining the material under anaerobic and high-temperature conditions.
The process also comprises a sludge concentration step, wherein sludge generated in the sand setting step, the chemical coagulation step and the electric flocculation treatment step is collected and concentrated. The sludge concentration step is used for collecting the sludge generated in the process, and the sludge is processed to be made into building bricks or solidified to be paved, so that the pollution is reduced, the waste utilization rate is increased, and meanwhile, the economic benefit and the social benefit are brought.
The treatment system used in the treatment process comprises a grit chamber device, a chemical coagulation device, an electric flocculation treatment device, a multidimensional electrode treatment device, a desalination treatment device and a sludge concentration device, wherein the grit chamber device is connected with the chemical coagulation device, the chemical coagulation device is connected with the electric flocculation treatment device, the electric flocculation treatment device is connected with the multidimensional electrode treatment device, the multidimensional electrode treatment device is connected with the desalination treatment device, the sludge concentration device is respectively connected with the chemical coagulation device and the electric flocculation treatment device, and the devices are connected through pipelines.
The device comprises a grit chamber device, a chemical coagulation device, a sludge concentration device, a multidimensional electrode treatment device, a sedimentation tank, a chemical flocculation device, a reaction tank, an electrocoagulation device and a chemical flocculation device, wherein the grit chamber device is provided with a grit chamber, the chemical coagulation device is provided with a coagulation tank and a sedimentation tank, the sludge concentration device is provided with a concentration tank, the multidimensional electrode treatment device is provided with a reaction tank, the grit chamber is connected with the coagulation tank, the coagulation tank is connected with the sedimentation tank, the sedimentation tank is connected with the electrocoagulation device, the electrocoagulation device is; be equipped with plate electrode, particle electrode, delivery port and water inlet in the reaction tank, plate electrode one end sets up on the reactor inside wall, in the other end stretches into the reactor, or plate electrode and the laminating of reaction tank inside wall, and the particle electrode distributes in the reaction tank, and delivery port and water inlet are established respectively at the reaction tank both ends.
The multidimensional electrode treatment device adopts a baffling type flow mode, N electrode plates are arranged in the reaction tank and are mutually staggered, the distance between the electrode plates is 40mm, and the electrode plates are graphite electrode plates.
The multidimensional electrode treatment device adopts the design of a plurality of electrode plates to ensure that the electrolysis sewage forms a baffling type flow mode in the electrolysis reactor, the flow mode of the wastewater in the reactor can realize the uniform distribution of the sewage in the reactor, the concentration polarization in the solution is avoided, and meanwhile, the sewage flows through different anode plates and cathode plates in the electrolysis process, which is equivalent to multiple times of electrolysis in the same electrolysis reactor, thereby greatly enhancing the treatment effect. The number of the polar plates and the distance between the polar plates can be flexibly adjusted according to the water quality condition, and the polar plates have strong adaptability to the high-chlorine-content shale gas flowback liquid with large change of substance concentration.
The N particle electrodes are irregularly distributed in the reaction tank.
The particle electrode is 5.5mm in particle size, 8mm in length and cylindrical, can effectively promote the generation of active chlorine and enhance the removal effect of organic matters.
The electric flocculation treatment device takes an iron sheet as an electrode plate, removes heavy metal ions in the wastewater through oxidation reduction and flocculation precipitation, and simultaneously can oxidize and degrade organic pollutants by hydroxyl free radical strong oxidizing substances generated in the electrolytic process. Namely, the catalyst has good effect of removing heavy metals and can oxidize and decompose organic pollutants.
The water inlet in the reaction tank is arranged at the lower part of the reaction tank, the water outlet is arranged at the upper part of the reaction tank, so that shale gas flowback liquid treated in the previous steps enters from the lower part of the reaction tank and flows out from the upper part after treatment, and the flowing mode of water inlet and water outlet can prevent organic pollutants from being adsorbed on a polar plate to influence the treatment effect, can also avoid concentration polarization in the solution and enhance the treatment effect of the multidimensional electrode treatment device.
According to the invention, the self-made particle electrodes are filled in the reaction tank, countless micro-electrolysis tanks are formed in the electrolysis process, so that the effective electrode area is increased, the mass transfer distance is reduced, the mass transfer of materials is enhanced, the electrochemical reaction of oxidation and reduction is generated, the current efficiency is improved, and the treatment effect is greatly enhanced; in addition, the electrolytic reaction in the reaction tank mainly comprises direct electrolysis and indirect electrolysis, wherein the direct electrolysis is mainly divided into anode oxidation and cathode reduction according to the electron transfer direction, and the organic matter degradation is realized through the oxidation-reduction reaction; the indirect oxidation is mainly related to the strongly oxidative intermediates generated in the electrolytic process, such as hydroxyl radical (. OH), hydrogen peroxide (H)2O2) Ozone (O)3) Etc. while containing Cl in the solution-When the process is carried out (the content of chloride ions in shale gas flowback liquid is generally as high as 10000-30000 mg/L), active chlorine (such as Cl) with strong oxidizing property can be generated in the electrolytic process2、OCl-And HClO, etc.), the pyrolusite filler or the ceramic pyrolusite filler can effectively promote the generation of active chlorine when being used for treating high-chlorine wastewater, and further enhance the treatment effect of organic pollutants.
The high-chlorine-content shale gas flowback liquid contains a large amount of soluble inorganic salts, has high conductivity, does not need to be additionally provided with electrolyte when adopting a multidimensional electrode treatment technology, simultaneously can obtain larger current intensity by adopting lower voltage when the waste water is electrolyzed due to the high conductivity of the waste water, greatly reduces the electrolysis energy consumption, and is favorable for strengthening the degradation effect of organic matters due to the active chlorine generated by a large amount of chlorine ions in the high-chlorine-content waste water in the electrolysis process.
The process and the system are simple in arrangement and convenient to operate, the treated shale gas flowback fluid can be recycled and can also be discharged after reaching the standard after being further treated, and the produced sludge can be prepared into building bricks or paves after being treated, so that the resource maximum utilization of the shale gas fracturing flowback fluid is realized.
Drawings
The invention will be described in further detail with reference to the following drawings and detailed description:
fig. 1 is a schematic diagram of the overall structure of a multidimensional electrode treatment process for shale gas flowback fluid.
Fig. 2 is a front view of a multidimensional electrode processing device of the shale gas flow-back fluid multidimensional electrode processing technology.
Fig. 3 is a top view of a multidimensional electrode processing device of the shale gas flowback fluid treatment process.
Wherein the labels in the figure are as follows:
1. a grit chamber, 2 a chemical coagulation tank, 3a sedimentation tank, 4 an electric flocculation device, 5 a multi-dimensional electrode treatment device, 6 a desalination treatment device, 7 a concentration tank, 8 a pipeline, 9a particle electrode, 10 an electrode plate, 11 a water outlet, 12 a water inlet
Detailed Description
The process scheme in the embodiment of the invention will be fully and clearly described below with reference to the accompanying drawings in the embodiment of the invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments obtained by a person of ordinary skill in the art based on the embodiments of the present invention without any creative effort belong to the protection scope of the present invention.
Example 1
The shale gas flowback fluid multidimensional electrode treatment process comprises the following steps:
(1) sand setting: removing large granular substances and rock debris in the shale gas flowback fluid; and removing larger suspended particles and rock debris in the shale gas flowback liquid through natural sedimentation.
(2) Chemical coagulation: adding a coagulating agent into the flowback liquid after sand settling in the step (1), adjusting the pH value to 6 in the coagulation process, and precipitating; firstly, adding a certain amount of polyaluminium chloride (PAC), stirring for a period of time, adding Polyacrylamide (PAM) with a certain concentration, and precipitating and removing colloidal suspended substances after the colloidal suspended substances are mutually flocculated to form large granular substances;
the concentration of the polyaluminium chloride is 30-40 percent, the concentration of the PAM is 0.1-0.5 percent, and the concentration and the addition are determined according to the change of water quality. The molecular weight of Polyacrylamide (PAM) is about 800 ten thousand.
(3) Electric flocculation treatment: carrying out electric flocculation treatment on the shale gas flowback liquid precipitated in the step (2), adjusting the pH to 7, removing heavy metal ions and oxidizing and degrading organic pollutants; the electric flocculation treatment device takes an iron sheet as an electrode plate.
(4) And (3) multi-dimensional electrode treatment: carrying out multi-dimensional electrode treatment in a multi-dimensional electrode treatment device, wherein the aeration rate of an electrolytic reaction is 600mL/min, the current intensity is 0.9A, and the electrolytic time is 60min, so as to remove organic pollutants difficult to degrade;
the particle electrode is a novel pyrolusite filler and is a solid section formed by mixing, pressing and firing pyrolusite powder and graphite powder; wherein the pyrolusite powder accounts for 60 percent by mass, the balance is graphite powder, the ignition temperature is 330 ℃, and the ignition time is 2 hours.
(5) Desalting: adjusting the pH value of the shale gas flowback liquid treated by the multidimensional electrode in the step (4) to 6, desalting by using a desalting device, wherein the operating pressure is 60kg/m2And removing inorganic salt in the shale gas flowback liquid.
The shale gas flowback liquid treatment system based on the multidimensional electrode technology comprises a grit chamber device, a chemical coagulation device, an electric flocculation treatment device, a multidimensional electrode treatment device, a desalination treatment device and a sludge concentration device, wherein the grit chamber device is connected with the chemical coagulation device, the chemical coagulation device is connected with the electric flocculation treatment device, the electric flocculation treatment device is connected with the multidimensional electrode treatment device, the multidimensional electrode treatment device is connected with the desalination treatment device, the sludge concentration device is respectively connected with the chemical coagulation device and the electric flocculation treatment device, and the devices are connected through pipelines.
The device comprises a grit chamber device, a chemical coagulation device, a sludge concentration device, a multidimensional electrode treatment device, a sedimentation tank, a chemical flocculation device, a reactor and an electric flocculation treatment device, wherein the grit chamber device is provided with a grit chamber, the chemical coagulation device is provided with a coagulation tank and a sedimentation tank, the sludge concentration device is provided with a concentration tank, the multidimensional electrode treatment device is provided with a reactor, the grit chamber is connected with the coagulation tank, the coagulation tank is connected with the sedimentation tank, the sedimentation tank is connected with the electric flocculation treatment device, the electric flocculation treatment device is connected with; be equipped with plate electrode, particle electrode, delivery port and water inlet in the reaction tank, plate electrode one end sets up on the lateral wall in the reaction tank, in the other end stretches into the reaction tank, or plate electrode and the laminating of lateral wall in the reaction tank, particle electrode distributes in the reaction tank, and delivery port and water inlet are established respectively at the reaction tank both ends.
Firstly, a grit chamber is used for treating large granular substances in shale gas flowback fluid, then the shale gas flowback fluid enters a chemical coagulation device to treat colloidal suspended particles (the pH value is adjusted to 6-7) in the shale gas flowback fluid, and the colloidal suspended particles are precipitated and removed after forming the large granular substances by adding a coagulation agent; then the shale gas flowback liquid enters an electric flocculation device to treat heavy metal ions in the water; after the shale gas returns from the electric flocculation treatment device, the shale gas returns the flowing liquid and directly enters the multidimensional electrode treatment device, and a novel pyrolusite filler is added into the multidimensional electrode treatment device to be used as a particle electrode for treating organic pollutants in the shale gas returns the flowing liquid; a desalting treatment device is arranged behind the multidimensional electrode treatment device and is used for treating a large amount of inorganic salts in the shale gas flowback liquid; the sludge generated by the grit chamber, the sedimentation tank and the electric flocculation device is collected and treated by the sludge concentration tank. The process can effectively remove various pollutants such as suspended matters, heavy metal ions, organic matters, a large amount of salts and the like in the flowback fluid through chemical coagulation, electric flocculation, multi-dimensional electrode method advanced oxidation treatment and desalination treatment. The process has high treatment efficiency, is green and environment-friendly, has great economic benefit and social benefit, and is worthy of popularization and wide application.
Example 2
The shale gas flowback fluid multidimensional electrode treatment process is characterized in that: the method comprises the following steps:
(1) sand setting: removing large granular substances and rock debris in the shale gas flowback fluid; and removing larger suspended particles and rock debris in the shale gas flowback liquid through natural sedimentation.
(2) Chemical coagulation: adding a coagulating agent into the flowback liquid after sand settling in the step (1), adjusting the pH value to 8 in the coagulating process, and precipitating; firstly, adding a certain amount of polyaluminium chloride (PAC), stirring for a period of time, adding Polyacrylamide (PAM) with a certain concentration, and precipitating and removing colloidal suspended substances after the colloidal suspended substances are mutually flocculated to form large granular substances;
the concentration of polyaluminum chloride is 40%, the concentration of PAM is generally 0.2%, and the concentration and the addition amount are determined according to the change of water quality.
(3) Electric flocculation treatment: carrying out electric flocculation treatment on the shale gas flowback liquid precipitated in the step (2), adjusting the pH to 9, removing heavy metal ions and oxidizing and degrading organic pollutants; the electric flocculation treatment device takes an iron sheet as an electrode plate.
(4) And (3) multi-dimensional electrode treatment: carrying out multi-dimensional electrode treatment in a multi-dimensional electrode treatment device, wherein the aeration rate of an electrolytic reaction is 600mL/min, the current intensity is 0.9A, and the electrolytic time is 60min, so as to remove organic pollutants difficult to degrade;
(5) desalting: adjusting the pH value of the shale gas flowback liquid treated by the multidimensional electrode in the step (4) to 8, desalting by using a desalting device, wherein the operating pressure is 70kg/m2Removing inorganic salt in the shale gas flowback liquid;
(6) sludge concentration step: collecting and concentrating sludge generated in the sand setting step, the chemical coagulation step and the electric flocculation treatment step. The sludge concentration step is used for collecting the sludge generated in the process, and the sludge is processed to be made into building bricks or paves, so that the pollution is reduced, the waste utilization rate is increased, and meanwhile, economic benefits and social benefits are brought.
The particle electrode is a novel pyrolusite filler and is a solid section formed by mixing, pressing and firing pyrolusite powder and graphite powder; wherein the pyrolusite powder accounts for 60 percent by mass, the balance is graphite powder, the ignition temperature is 330 ℃, and the ignition time is 2 hours.
Shale gas flowback liquid processing system based on multidimension electrode technique, including grit chamber device, chemistry thoughtlessly congeals the device, the electric flocculation treatment device, multidimension electrode processing apparatus, desalination device and sludge thickening device, grit chamber device and chemistry thoughtlessly congeal the device to be connected, chemistry thoughtlessly congeals the device and is connected with the electric flocculation treatment device, electric flocculation treatment device and multidimension electrode processing apparatus are connected, multidimension electrode processing apparatus and desalination device are connected, sludge thickening device thoughtlessly congeals the device with chemistry respectively, the electric flocculation treatment device is connected, above each device passes through the pipe connection.
The device comprises a grit chamber device, a chemical coagulation device, a sludge concentration device, a multidimensional electrode treatment device, a sedimentation tank, a chemical flocculation device, a reactor and an electric flocculation treatment device, wherein the grit chamber device is provided with a grit chamber, the chemical coagulation device is provided with a coagulation tank and a sedimentation tank, the sludge concentration device is provided with a concentration tank, the multidimensional electrode treatment device is provided with a reactor, the grit chamber is connected with the coagulation tank, the coagulation tank is connected with the sedimentation tank, the sedimentation tank is connected with the electric flocculation treatment device, the electric flocculation treatment device is connected with; be equipped with plate electrode, particle electrode, delivery port and water inlet in the reaction tank, plate electrode one end sets up on the lateral wall in the reaction tank, in the other end stretches into the reaction tank, or plate electrode and the laminating of lateral wall in the reaction tank, particle electrode distributes in the reaction tank, and delivery port and water inlet are established respectively at the reaction tank both ends.
The multidimensional electrode treatment device adopts a baffling type flow mode, N electrode plates are arranged in the reaction tank and are mutually staggered, and the distance between the electrode plates is 40 mm.
The multidimensional electrode treatment device adopts the design of a plurality of graphite electrode plates to ensure that the electrolysis sewage forms a baffling type flow mode in the electrolysis reactor, the flow mode can realize the uniform distribution of the sewage in the electrolysis reactor, the concentration polarization appearing in the solution is avoided, meanwhile, the sewage flows through different anode plates and cathode plates in the electrolysis process, the electrolysis is carried out for a plurality of times in the same electrolysis reactor, and the treatment effect is greatly enhanced. The number of the polar plates and the distance between the polar plates can be flexibly adjusted according to the water quality condition, and the polar plates have strong adaptability to the high-chlorine-content shale gas flowback liquid with large change of substance concentration.
N particle electrodes are irregularly distributed in the reactor. The particle electrode has the particle size of 5.5mm and the length of 8mm, is cylindrical, can effectively promote the generation of active chlorine, and enhances the removal effect of organic matters.
When the treatment system is used for treating the shale gas flowback liquid, the treatment process is as follows: the shale gas flowback liquid firstly removes large particulate matters and rock debris in water through a grit chamber 1, the generated sludge enters a sludge concentration tank 7 through a backflow pipeline 8, then the shale gas flowback liquid enters a chemical coagulation tank 2 through a pipeline, a coagulation agent is added into the water to remove suspended particles and colloidal impurities in the water (the pH value is adjusted to 6-7 to be optimal), and finally the sludge is precipitated in a sedimentation tank 3, the precipitate generated in the process also enters the sludge concentration tank 7 through the pipeline 8, then the shale gas flowback liquid enters an electric flocculation device 4 through the pipeline, heavy metal ions and partial organic pollutants in the water are removed through the electric flocculation effect, the treated shale gas flowback liquid enters a multi-dimensional electrode treatment device 5 through the pipeline to remove a large amount of organic pollutants in the water, and a self-made novel pyrolusite filler is added in the multi-dimensional electrode treatment device to serve as a particle electrode. And then the wastewater enters a desalting treatment device through a pipeline to remove a large amount of inorganic salts in the water, and salts generated after further treatment of concentrated solution generated by desalting treatment can be sold as industrial salts. The wastewater after the series of treatments can reach the standard of reinjection and discharge.
Multidimensional electrode processing apparatus adopts baffling formula's mobile mode, has set up the polylith polar plate in the reaction tank, and shale gas flowback liquid gets into by the reaction tank lower part, flows by upper portion after the processing, and this mobile mode can prevent to adsorb organic pollutant on the polar plate and influence the treatment effect, can also avoid appearing concentration polarization in the solution.
Example 3
The shale gas flowback fluid treatment process based on the multidimensional electrode technology comprises the following steps:
(1) firstly, removing large granular substances from shale gas flowback liquid through a grit chamber;
(2) and then entering a coagulation tank for coagulation treatment, firstly adding polyaluminium chloride (PAC) with the concentration controlled between 35%, stirring for 30 seconds, then adding Polyacrylamide (PAM) with the molecular weight of 800 ten thousand and the concentration controlled at 0.3%, stirring for 30 seconds until a large amount of floccules appear in water, then entering a sedimentation tank for standing and sedimentation, and concentrating and collecting the generated sediment in a sludge concentration tank.
(3) The shale gas flow-back liquid after the treatment enters an electric flocculation device which takes an iron sheet as an electrode plate, removes heavy metal ions in the wastewater through oxidation reduction and flocculation precipitation, and takes care to ensure that the pH value of the device is maintained at 8 so as to ensure that the reaction is normally and effectively carried out.
(4) Shale gas flowback liquid after the electrocoagulation treatment enters a multidimensional electrode treatment device, the device is provided with a plurality of polar plates (graphite polar plates), the distance between the polar plates is 40mm, self-made pyrolusite filler is added between the polar plates to serve as particle electrodes, the particle electrodes are columnar particles, the particle diameter is 5.5mm, the length is 8mm, the device adopts a baffled flow mode, the flowback liquid enters from a water inlet at the lower part of a reaction tank and is discharged from a water outlet at the upper part of the other side after treatment.
The novel pyrolusite filler is a solid section formed by mixing, pressing and firing pyrolusite powder and graphite powder; wherein the pyrolusite powder accounts for 60 percent by mass, the balance is graphite powder, the ignition temperature is 330 ℃, and the ignition time is 2 hours.
(5) The flowback liquid treated by the multidimensional electrode device enters a desalination treatment device through a pipeline, the device adopts reverse osmosis membrane treatment, firstly, the pH of the flowback liquid treated by the multidimensional electrode device is adjusted to 6, then the flowback liquid enters the reverse osmosis desalination treatment device through the pipeline to remove inorganic salts in the shale gas flowback liquid, and the operation pressure is 65kg/m2。
(5) And (4) further treating the concentrated solution generated by the desalting treatment device to generate salts or selling the salts as industrial salts.
In-process electroflocculationThe method for removing heavy metal ions is to generate a large amount of cations (Fe) under the action of external voltage by using a soluble anode (generally iron or aluminum)2+、Al3+) A series of multi-core hydrolysis products are generated through hydrolysis, polymerization and the like, and flocculation and precipitation effects are performed on heavy metal ions, so that the heavy metal ions in the wastewater are removed, partial heavy metals can be directly reduced into metal simple substances through the redox reaction of the anode/cathode, oxygen and hydrogen generated by electrolysis can form small bubbles to achieve an air floatation-like effect, and strong oxidizing substances such as oxygen, hydroxyl free radicals and the like can be oxidized and decomposed into organic pollutants. Thus, the electroflocculation process actually has redox, flocculation, and flotation simultaneously, as a result of the synergistic effect of the various processes.
Example 4
Otherwise, as in example 1, the particulate electrode was a ceramic pyrolusite filler. The ceramic pyrolusite filler is a solid section formed by mixing, pressing and firing pyrolusite powder, activated carbon powder, a sodium silicate adhesive and clay; wherein the mass ratio of the pyrolusite powder to the clay is 7: 3; adding 12 percent of activated carbon powder and 15 percent of sodium silicate adhesive by the total weight of the pyrolusite and the clay, wherein the firing temperature is 600 ℃, and the firing time is 2 hours.
Example 5
Otherwise, as in example 1, the particulate electrode was a ceramic pyrolusite filler. The novel ceramic pyrolusite filler is a solid section formed by mixing, pressing and firing pyrolusite powder, activated carbon powder, a sodium silicate adhesive and clay; the optimal mass ratio of the pyrolusite powder to the clay is 6: 4; the content of the activated carbon powder is 12 percent, and the content of the sodium silicate is 15 percent; the optimal ignition temperature of the particle electrode is 600 ℃, and the ignition time is 2 h.
Example 6
Otherwise, as in example 1, the particulate electrode was a ceramic pyrolusite filler. The ceramic pyrolusite filler is a solid section formed by mixing, pressing and firing pyrolusite powder, activated carbon powder, a sodium silicate adhesive and clay; wherein the mass ratio of the pyrolusite powder to the clay is 5: 5; adding 12 percent of activated carbon powder and 15 percent of sodium silicate adhesive by the total weight of the pyrolusite and the clay, wherein the firing temperature is 600 ℃, and the firing time is 2 hours.
Example 7
Otherwise, as in example 1, the particulate electrode was a ceramic pyrolusite filler. The ceramic pyrolusite filler is a solid section formed by mixing, pressing and firing pyrolusite powder, activated carbon powder, a sodium silicate adhesive and clay; wherein the mass ratio of the pyrolusite powder to the clay is 4: 6; adding 12 percent of activated carbon powder and 15 percent of sodium silicate adhesive by the total weight of the pyrolusite and the clay, wherein the firing temperature is 600 ℃, and the firing time is 2 hours.
Example 8
Otherwise, as in example 1, the particulate electrode was a ceramic pyrolusite filler. The ceramic pyrolusite filler is a solid section formed by mixing, pressing and firing pyrolusite powder, activated carbon powder, a sodium silicate adhesive and clay; wherein the mass ratio of the pyrolusite powder to the clay is 3: 7; adding 12 percent of activated carbon powder and 15 percent of sodium silicate adhesive by the total weight of the pyrolusite and the clay, wherein the firing temperature is 600 ℃, and the firing time is 2 hours.
Example 9
On the basis of embodiment 3, this embodiment provides an example of an on-site application of the method for treating shale gas flowback fluid:
the pH value of shale gas flowback liquid at a certain well site in Sichuan is 7.60, the shale gas flowback liquid is yellow in color and has no pungent smell, and the specific parameters are shown in Table 1:
TABLE 1 shale gas flowback water quality at certain well site of Sichuan
Figure BDA0001337592540000101
Figure BDA0001337592540000111
Removing large granular substances in water through a grit chamber, then entering a chemical coagulation tank, adjusting the pH value to 6-7, adding a 34% polyaluminum chloride (PAC) solution, stirring for a certain time, then adding a Polyacrylamide (PAM) solution with the molecular weight of 1200 ten thousand and the concentration of 0.2%, stirring until flocs appear in the water, standing for a period of time, then entering a sedimentation tank, allowing an upper clear liquid to enter an electrocoagulation device through a water outlet pipeline, allowing a lower sediment to enter a sludge concentration tank through a sludge pipeline, concentrating and collecting, and waiting for subsequent treatment. Heavy metal ions in water are removed from the shale gas flowback liquid entering the electrocoagulation device through the electrocoagulation action, the treated shale gas flowback liquid enters the multidimensional electrode treatment device through a sewage pipeline, a large amount of organic pollutants which are difficult to treat in the shale gas flowback liquid are subjected to electrolytic treatment, then the shale gas flowback liquid is subjected to desalination treatment through the desalination treatment device to remove a large amount of inorganic salts in the water, and concentrated liquid generated by the desalination treatment is further treated and then is sold as industrial salt. The water quality of the shale gas flowback liquid after treatment is colorless and uniform, and reaches the treatment standard of reinjection or discharge.
The water quality after the series of treatments is shown in the table 2:
Figure BDA0001337592540000112
(Note: only the major remaining criteria are listed here, and nothing is recorded if none of the required or minor compliance with the criteria is present)
From the above, it can be seen that the treatment process of the present invention and the system apparatus used therein bring about excellent effects.
The fracturing fluid used for shale gas is a water-based fracturing fluid, also called slickwater, and mainly comprises a resistance reducing agent, a discharge aiding agent and an anti-swelling agent.
The largest occupied amount of the inhibitor is polyacrylamide inhibitor (one thousandth of the fracturing fluid). The polyacrylamide has the advantages of high resistance reduction performance, low use concentration, economy and the like, and is widely applied to shale gas fracturing. During the fracturing process, polyacrylamide is changed into small molecular compounds through high-shear chain cutting, and the small molecular compounds and the flowback liquid are flowback to the ground together.
Therefore, PAM is taken as a target pollutant in the invention, and the PAM is treated by adopting a multidimensional electrolysis unit.
The shale gas also has high chlorine content, the organic matter is difficult to treat under the high chlorine condition, and the content is greatly reduced after the treatment by the method of the invention.
Wherein, the electric flocculation is mainly used for removing heavy metals, such as mercury exceeding parts, and after the treatment is finished, the subsequent desalination treatment is mainly used for removing chloride ions, so that the discharged water reaches the standard.
While the foregoing shows and describes the fundamental principles and principal features of the invention, together with the advantages thereof, the foregoing embodiments and description are illustrative only of the principles of the invention, and various changes and modifications can be made therein without departing from the spirit and scope of the invention, which will fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (5)

1. A shale gas flowback fluid multidimensional electrode treatment process is characterized in that: the method comprises the following steps:
(1) sand setting: removing large granular substances and rock debris in the shale gas flowback fluid;
(2) chemical coagulation: adding a coagulating agent into the flowback liquid after sand settling in the step (1), adjusting the pH value to 6-8, and precipitating;
(3) electric flocculation treatment: carrying out electric flocculation treatment on the shale gas flowback liquid precipitated in the step (2), adjusting the pH to 7-9, removing heavy metal ions and oxidizing and degrading organic pollutants; the electric flocculation treatment device takes an iron sheet as an electrode plate, removes heavy metal ions in the wastewater through oxidation reduction and flocculation precipitation, and simultaneously can oxidize and degrade organic pollutants by hydroxyl radical strong oxidizing substances generated in the electrolytic process;
(4) and (3) multi-dimensional electrode treatment: carrying out multi-dimensional electrode treatment in a multi-dimensional electrode treatment device, wherein the aeration rate of the electrolysis reaction is 600mL/min, the current intensity is 0.9A, and the electrolysis time is 60min, so as to remove organic pollutants difficult to degrade; the multi-dimensional electrode processing device is provided with N particle electrodes, wherein the N particle electrodes are made of ceramic pyrolusite filler, N electrode plates in the multi-dimensional electrode processing device are arranged in a mutually staggered mode, the distance between the electrode plates is 40mm, and the electrode plates are graphite electrode plates; the ceramic pyrolusite filler is a solid section formed by mixing, pressing and firing pyrolusite powder, activated carbon powder, a sodium silicate adhesive and clay; wherein the mass ratio of the pyrolusite powder to the clay is 6-3: 4-7; adding 12 percent of activated carbon powder and 15 percent of sodium silicate adhesive by the total weight of the pyrolusite and the clay, wherein the firing temperature is 600 ℃, and the firing time is 2 hours;
(5) desalting: and (5) adjusting the pH value of the shale gas flowback liquid treated by the multidimensional electrode in the step (4) to 6-8, desalting by using a desalting device under the operation pressure of 60kg/m & lt 2 & gt-70 kg/m & lt 2 & gt, and removing inorganic salts in the shale gas flowback liquid.
2. The shale gas flowback fluid multidimensional electrode treatment process of claim 1, wherein: the mass ratio of pyrolusite powder to clay in the ceramic pyrolusite filler is 6: 4.
3. the shale gas flowback fluid multidimensional electrode treatment process of claim 1, wherein: the process also comprises a sludge concentration step, wherein sludge generated in the sand setting step, the chemical coagulation step and the electric flocculation treatment step is collected and concentrated.
4. The shale gas flowback fluid multidimensional electrode treatment process of claim 1, wherein: the treatment system used in the treatment process comprises a grit chamber device, a chemical coagulation device, an electric flocculation treatment device, a multidimensional electrode treatment device, a desalination treatment device and a sludge concentration device, wherein the grit chamber device is connected with the chemical coagulation device; n electrode plates in the multidimensional electrode processing device are arranged in a staggered mode, the distance between the electrode plates is 40mm, and the electrode plates are graphite electrode plates.
5. The shale gas flowback fluid multidimensional electrode treatment process according to claim 4, characterized in that: the device comprises a grit chamber device, a chemical coagulation device, a sludge concentration device, a multidimensional electrode treatment device, a sedimentation tank, a chemical flocculation device, a reaction tank, an electrocoagulation device and a chemical flocculation device, wherein the grit chamber device is provided with a grit chamber, the chemical coagulation device is provided with a coagulation tank and a sedimentation tank, the sludge concentration device is provided with a concentration tank, the multidimensional electrode treatment device is provided with a reaction tank, the grit chamber is connected with the coagulation tank, the coagulation tank is connected with the sedimentation tank, the sedimentation tank is connected with the electrocoagulation device, the electrocoagulation device is; the reactor is internally provided with a plate electrode, a particle electrode, a water outlet and a water inlet, wherein one end of the plate electrode is arranged on the inner side wall of the reactor, the other end of the plate electrode extends into the reactor and is attached to the plate electrode and the inner side wall of the reactor, the particle electrode is distributed in the reactor, and the water outlet and the water inlet are respectively arranged at two ends of the reactor; the electric flocculation treatment device takes an iron sheet as an electrode plate, removes heavy metal ions in the wastewater through oxidation reduction and flocculation precipitation, and simultaneously can oxidize and degrade organic pollutants by hydroxyl radical strong oxidizing substances generated in the electrolytic process; n particle electrodes are irregularly distributed in the reactor; the particle electrode has a particle diameter of 5.5mm and a length of 8mm, and is cylindrical.
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