CN110339722B - Inorganic ceramic membrane self-cleaning filtering technology for shale gas fracturing flowback fluid - Google Patents

Inorganic ceramic membrane self-cleaning filtering technology for shale gas fracturing flowback fluid Download PDF

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CN110339722B
CN110339722B CN201910709813.0A CN201910709813A CN110339722B CN 110339722 B CN110339722 B CN 110339722B CN 201910709813 A CN201910709813 A CN 201910709813A CN 110339722 B CN110339722 B CN 110339722B
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ceramic membrane
cleaning
solid cleaning
filtering
cleaning particles
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CN110339722A (en
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任宏洋
汪佳敏
施斌
张欢
熊明洋
雷杰霞
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Southwest Petroleum University
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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D65/00Accessories or auxiliary operations, in general, for separation processes or apparatus using semi-permeable membranes
    • B01D65/02Membrane cleaning or sterilisation ; Membrane regeneration
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D65/00Accessories or auxiliary operations, in general, for separation processes or apparatus using semi-permeable membranes
    • B01D65/02Membrane cleaning or sterilisation ; Membrane regeneration
    • B01D65/04Membrane cleaning or sterilisation ; Membrane regeneration with movable bodies, e.g. foam balls

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Abstract

The invention relates to an inorganic ceramic membrane self-cleaning filtering technology for shale gas fracturing flowback fluid, which is characterized in that solid cleaning particles are added into feed liquid, so that the collision and the collision of pollutants on the surface of a ceramic membrane are realized during the filtering,The material has the functions of crushing, adsorbing and carrying, realizes self-cleaning, and preferably selects solid cleaning particles prepared from the pecan shell material, wherein the particle size of the solid cleaning particles is 1-2 mm, and the density of the solid cleaning particles is 1.2-1.6 g/cm3The porosity is 27-50%, the molar hardness is 3-4, the adding amount is 5-10 g/L, the ratio of the circulation flow of the feed liquid to the water inflow of the shale gas fracturing flow-back fluid is 30: 1-50: 1, the filtering pressure is 0.15-0.25 MPa, and the flow velocity of the liquid on the surface of the ceramic membrane is 10-20L/s.m2. The method has the advantages of synchronous ceramic membrane cleaning and filtering processes, high equipment operation efficiency, simplicity, convenience, easiness in operation, high cleaning efficiency, no secondary pollution, good economy and the like.

Description

Inorganic ceramic membrane self-cleaning filtering technology for shale gas fracturing flowback fluid
Technical Field
The invention belongs to the field of environment-friendly water treatment, and relates to a self-cleaning filtering technology in a filtering process of an inorganic ceramic membrane of shale gas fracturing flowback fluid.
Background
In recent years, the shale gas industry develops rapidly, and China has proved that the reserves reach the first world and the yield reaches the first three world. The hydraulic fracturing method is a technology widely applied to shale gas exploitation, and is characterized in that a well is drilled through hydraulic pressurization, a small gap is opened to allow shale gas to flow to a drilling hole, and fracturing flowback fluid is mixed liquor which is flowback from the well at the initial stage of completion of hydraulic fracturing. The water quality characteristics of the oil-gas separator vary due to different geological conditions, generally, the oil-gas separator has the advantages of complex components, high COD (chemical oxygen demand), high TSS (total suspended solids) and high TDS (total dissolved solids), and great treatment difficulty, and becomes a great technical problem in the oil-gas industry.
Ceramic membrane separation technology has been widely used in petrochemical, food, biotechnology and pharmaceutical industries, as well as a range of environmental applications, and compared with other separation methods (such as adsorption or distillation), the simplicity and low cost and high efficiency of the process technology make it widely used in water treatment engineering. Low energy consumption, easy expansion, capacity of being used in combination with other processes, high strength and continuous automatic operation, are the main advantages of ceramic membrane filtration processes, but have the limitation of the problem of membrane pollution.
In the case of inorganic ceramic membranes, fouling of the membrane leads to a decrease in flux and the membrane must be cleaned. Generally, membrane cleaning methods are generally classified into physical methods, which remove contaminants by washing with high-flow water, mechanical cleaning with sponge balls, and the like, and chemical methods, which clean membranes with chemical agents that do not destroy membrane materials themselves and have a dissolving or displacing effect on contaminants.
Organic pollutants in the shale gas fracturing flowback fluid mainly comprise macromolecular hydrocarbons, polyacrylamide and byproducts generated after gel breaking and oxidation in the fracturing process of the polyacrylamide, inorganic pollutants mainly comprise metal ions, rock debris and clay, wherein the metal ions mainly comprise: sodium, potassium, calcium, magnesium, barium and the like, the total mineralization degree of the shale gas fracturing flowback fluid can reach 30000 mg/L-120000 mg/L, the content of suspended solids can reach 80-400 mg/L, and the COD is about 100-2000 mgL. Organic matters in the shale gas fracturing flowback fluid have large molecular weight and strong adhesive capacity, are easy to adsorb on the surface of the membrane, and are main factors influencing the performance of the ceramic membrane. Over time during filtration, adsorption or accumulation of contaminants within the pores of the membrane can lead to a decrease in pore size and an increase in membrane resistance, which is difficult to recover, especially for large organic species, even at lower concentrations, which can greatly affect the membrane over clay or other inorganic colloidal particles.
At present, there are reports on the related art regarding the cleaning method for inorganic ceramic membranes. Chinese patent application No. 201610845396.9 discloses a cleaning agent for inorganic ceramic membrane, which is prepared by adopting tetrapropenyl sodium benzenesulfonate, magnesium sulfate, corrosion inhibitor, sodium carbonate, sodium chloride, sodium oxychloride, fatty alcohol-polyoxyethylene ether, deionized water, zeolite and ethylene glycol monobutyl ether as raw materials to chemically clean the ceramic membrane. Chinese patent (application number: 201811165720.8) discloses a method for cleaning a flat ceramic membrane, which comprises the following steps: (1) physical cleaning: ultra-pure water spray washing, and back washing with ultra-pure water at a preset flow rate and preset time; (2) chemical cleaning: the cleaning and static soaking are cyclically carried out with the compound medicament at a preset flow rate and preset time. The technologies promote the popularization of the ceramic membrane cleaning technology, but the cleaning technology has the defects of complex cleaning process, more used medicaments and the like, and the cleaning process needs to stop the ceramic membrane filtering operation and then starts an independent cleaning process, so that the filtering process cannot be continuously carried out, and the operating efficiency of inorganic ceramic membrane filtering equipment is reduced.
Disclosure of Invention
The invention aims to solve the problem of membrane pollution caused by adsorption of macromolecular organic matters and suspended matters in shale gas fracturing flow-back fluid on the surface of a membrane in the filtering process of an inorganic ceramic membrane, simultaneously improve the defects of complicated technical process, more used medicaments, independent increase of a cleaning process after the filtering is stopped and the like of the ceramic membrane, and realize self-cleaning effect synchronously performed in the filtering process and the cleaning process of the ceramic membrane by adding preferred solid cleaning particles into liquid to be filtered and optimizing the process conditions of the filtering process.
The invention relates to an inorganic ceramic membrane self-cleaning filtering technology of shale gas fracturing flowback fluid, which adopts the technical scheme that: preferably and preparing solid cleaning particles with specific density, particle size, porosity and hardness according to the pollution characteristics of macromolecular organic matters and suspended matters on the ceramic membrane in the filtering process of the shale gas fracturing flow-back fluid ceramic membrane; solid cleaning particles are added into shale gas fracturing flowback fluid according to the optimal concentration and pumped into a ceramic membrane filter to start filtering, the adsorption or accumulation of macromolecular organic matters and suspended matters on the surface of the membrane is reduced by utilizing the collision, crushing, adsorption and carrying effects of the solid cleaning particles on pollutants adsorbed on the surface of an inorganic ceramic membrane in the flowing process, the self-cleaning effect is realized, the process parameters such as pressure, flow rate and the like in the filtering process are optimized, the collision, crushing, adsorption and carrying amounts of the solid cleaning particles on the pollutants are maximized, and the self-cleaning efficiency is improved; the solid cleaning particles are regenerated and recycled by physical cyclone separation and chemical cleaning.
The further concrete technical scheme of the invention comprises the following steps:
(1) selecting solid cleaning particles, preferably a pecan shell material, crushing and screening the pecan shell, modifying, soaking the pecan shell in a mixed acid of sulfuric acid with the concentration of 1-2% (v/v) and nitric acid with the concentration of 0.5-1% (v/v) for 1-2 h, filtering and cleaning; heating at a rate of 10-15 deg.C/minHeating to 300-400 ℃ at a speed rate for 3-4 h, controlling the oxygen concentration to be 1-5% (v/v) in the heating process, cooling and taking out to obtain particles with a multi-prismatic shape, a particle diameter of 1-2 mm and a particle density of 1.2-1.6 g/cm3Solid cleaning particles with the particle porosity of 27% -50% and the molar hardness of 3-4;
(2) mixing the prepared solid cleaning particles and shale gas fracturing flow-back fluid in a buffer tank, controlling the circular flow of feed liquid between a ceramic membrane filter and the buffer tank in the filtering process, wherein the ratio of the circulation flow of the feed liquid to the water inflow is 30: 1-50: 1, the filtering pressure is 0.15 MPa-0.25 MPa, and the flow velocity of the liquid on the surface of the ceramic membrane is 10-20L/s.m2The concentration of the solid cleaning particles in the feed liquid is 5 g/L-10 g/L;
(3) the solid cleaning particles are cleaned and regenerated by acid liquor and alkali liquor respectively after inorganic pollutants are separated by a cyclone separator, and then are recycled, wherein the acid liquor is 1-2% (v/v) hydrochloric acid, and the alkali liquor is 1-2% (v/v) sodium hydroxide.
Technical characteristics
For the problem of membrane pollution cleaning in the ceramic membrane filtration process, a rapid, simple and easy-to-operate cleaning technology is the key influencing the operation efficiency and the economical efficiency. The difficulty of the invention lies in that:
(1) the shale gas fracturing flowback fluid is relatively complex in pollutant composition, wherein the pollution characteristics of inorganic scale formed by the adhesion of macromolecular organic matters represented by polyacrylamide and the hydrolysis of metal ions such as calcium and magnesium on a ceramic membrane are greatly different, and a self-cleaning process needs to be designed according to different pollution characteristics;
(2) the damage to the ceramic membrane in the cleaning process is as small as possible;
(3) the cleaning process and the filtering process are synchronously carried out, so that the operating efficiency of the filtering process is improved;
(4) the method is simple to operate, fast and efficient, and has no secondary pollution.
In order to solve the technical problems, the innovation of the cleaning mode, the optimization of the cleaning material, the optimization of the parameters of the cleaning process, and the regeneration and recycling of the cleaning material are significant innovations in the invention.
According to the invention, the step (1) is preferably carried out on a cleaning material polluted by the ceramic membrane, and different from the traditional method of adopting acid liquor, alkali liquor and an organic solvent as the cleaning material, aiming at the pollution characteristic of the ceramic membrane in the filtering process of the shale gas fracturing flow-back fluid, namely the agglomeration and adhesion of organic macromolecules represented by polyacrylamide and inorganic scale formed by the hydrolysis of metal ions such as calcium, magnesium and the like, solid cleaning particles with special functions are creatively invented, organic pollutants and inorganic pollutants on the surface of the ceramic membrane are efficiently removed, and the ceramic membrane is ensured not to be damaged.
In the step (1), the main organic pollutant in the shale gas fracturing flowback fluid is polyacrylamide which is stable in chemical property and not easy to be chemically oxidized or dissolved, meanwhile, the polyacrylamide has a large molecular weight, and molecules on the surface of the ceramic membrane are mutually wound and agglomerated during filtering to form a supermolecular cluster structure3~1.5g/cm3Has strong carrying capacity and can efficiently remove organic pollutants on the surface of the ceramic membrane. Too low particle size and particle density carrying capacity are weak, cleaning performance on the surface of the ceramic membrane is poor, too high particle size and particle density easily cause uneven distribution of cleaning particles in a liquid phase, and cleaning performance on the surface of the ceramic membrane is poor.
Inorganic pollutants generated in the filtering process of the shale gas fracturing flowback fluid ceramic membrane are mainly inorganic scale accumulated on the surface of the ceramic membrane, and the hardness of mixed scale formed on the surface of the ceramic membrane according to metal ion hydrolysis products such as calcium, magnesium and barium and clay, rock debris powder and the like in the flowback fluidAnd analyzing the bonding strength of the scale and the ceramic membrane, wherein in the step (1), the molar hardness of the prepared solid cleaning particles is preferably 3-4, the particles are polygonal, and inorganic pollutants on the surface of the ceramic membrane can be efficiently removed through collision and crushing. Analyzing the accumulation rate and distribution condition of inorganic scale on the surface of the combined ceramic membrane, preferably selecting the particle size of 1-2 mm and the particle density of 1.2g/cm3~1.5g/cm3The solid cleaning particles can efficiently remove inorganic pollutants on the surface of the ceramic membrane.
The hardness of the ceramic membrane is 6.0-7.0, the preferable solid cleaning particles with the molar hardness of 3-4 cannot damage the membrane structure of the ceramic membrane in the cleaning process, and the integrity of the particles in the operation process can be guaranteed. The aperture specification of the ceramic membrane is generally 1 nm-5 mu m, the particle size of the preferred solid cleaning particles is larger than the aperture of the ceramic membrane, and the blockage and damage of the solid cleaning particles to the ceramic membrane in the operation process can be avoided.
In the filtering process of the shale gas fracturing flowback fluid, the main organic pollutant causing the ceramic membrane pollutant is polyacrylamide, the molecular chain of the polyacrylamide contains amide groups and other ionic groups, and the shale gas fracturing flowback fluid has the characteristic of high hydrophilicity, the pecan shell material is modified in the step (1), solid cleaning particles are prepared, the hydrophilicity of the surface of the solid cleaning particles is improved, the solid cleaning particles are soaked in mixed acid of 1-2% (v/v) sulfuric acid and 0.5-1% (v/v) nitric acid for 1-2 hours, and then the shale gas fracturing flowback fluid is heated for 3-4 hours under the conditions that the oxygen concentration is 1-5% (v/v) and the temperature is 300-400 ℃. Under the heating condition, oxygen-containing functional groups such as-COO-, -OH and the like are formed on the surfaces of the solid cleaning particles made of the hickory shell material, so that the hydrophilicity of the surfaces of the solid cleaning particles is enhanced, and the adsorption and carrying capacity of the solid cleaning particles on organic pollutants on the surface of the ceramic membrane is improved. The method optimizes the type and concentration of the treating agent, preferably selects the heat treatment temperature of 300-400 ℃, has too low heating temperature, is not beneficial to the surface thermochemical reaction to form oxygen-containing functional groups, and has the advantages of damaging polar functional groups on the surfaces of the solid cleaning particles due to too high temperature, reducing the surface hydrophilicity of the solid cleaning particles, weakening the carrying capacity of the solid cleaning particles on organic pollutants and reducing the cleaning capacity of ceramic membrane pollution.
In conclusion, the membrane pollution removal material in the shale gas fracturing flow-back fluid ceramic membrane filtration technology is innovatively prepared, and the preferable and prepared solid cleaning particles have the following characteristics: the composite material has proper density, particle shape and particle size, enhances the capability of carrying organic and inorganic pollutants, and has strong pollutant interception capability and high pollutant removal rate; secondly, the ceramic membrane has proper surface polarity and porosity, and has higher adsorption and removal efficiency on organic pollutants on the surface of the ceramic membrane; the ceramic membrane has proper hardness, has higher removal efficiency on inorganic scale on the surface of the ceramic membrane, is not easy to break, and has higher utilization rate; and fourthly, the prepared solid particles do not cause damage to the ceramic membrane structure.
In the step (2), a process technology for synchronously performing the filtering process and the cleaning process is creatively invented according to the operation characteristics of the ceramic membrane filter, the operation of the ceramic membrane filter is characterized in that cross-flow filtration is adopted, blanking liquid is pushed by a pump to flow parallel to a membrane surface, clear water after filtration vertically penetrates through the ceramic membrane along the flowing direction of the material liquid, and meanwhile solid cleaning particles in the material liquid flow through the membrane surface and take away pollutants remained on the membrane surface through collision, crushing, adsorption and carrying effects, so that the self-cleaning effect is realized. By optimizing the process condition of the filtering pressure, the carrying capacity of macromolecular organic matters and suspended matters is maximized while the water outlet efficiency is ensured. The adding amount of the solid cleaning particles is preferably 5 g/L-10 g/L, so that the solid cleaning particles can fully perform collision, crushing, adsorption and carrying effects on the polluted surface of the membrane, the adsorption or accumulation of macromolecular organic matters and suspended matters in the fracturing flow-back fluid on the surface of the membrane is reduced, and a self-cleaning effect is realized; the ratio of the circulation flow of the feed liquid to the water inflow of the shale gas fracturing flow-back fluid in the filtering process is preferably 30: 1-50: 1, the lateral shearing force of the shale gas fracturing flow-back fluid is increased due to the increase of the circulation flow of the feed liquid, and the action frequency of solid cleaning particles and pollutants in the feed liquid is increased, so that the scouring action on organic pollutants attached to the surface of a ceramic membrane is enhanced, the organic pollutants are not easy to deposit on the surface of the membrane, and the membrane is not easy to block; the filtering pressure has great influence on the filtering and self-cleaning processes of the ceramic membrane, the filtering efficiency of the ceramic membrane is low due to the smaller filtering pressure, and the organic components can be separated due to the larger filtering pressureThe filtering pressure is preferably 0.15MPa to 0.25MPa, so that the water outlet efficiency is ensured, the deposition of organic matters on the surface of the membrane is reduced, and the self-cleaning effect of pollutants is maximized; preferably, the flow velocity of the liquid on the surface of the ceramic membrane is 10-20L/s.m2Under the action of the flow velocity, the feed liquid flows parallel to the membrane surface under the driving of the pump to generate a large scouring action on the membrane surface, and meanwhile, the solid cleaning particles remove pollutants remained on the membrane surface through collision, crushing, adsorption and carrying actions generated when flowing through the membrane surface.
In the step (3), the cleaning principle of solid cleaning particles on organic pollutants and inorganic pollutants on the surface of the ceramic membrane in the filtering process of the ceramic membrane is combined, and a physical and chemical combined solid cleaning particle regeneration and circulation technology is creatively developed in the invention. Aiming at inorganic scale debris collided and crushed by solid cleaning particles, a cyclone separation process is optimized by analyzing the density difference between the inorganic scale debris and the solid cleaning particles, the solid cleaning particles with larger particle size and density enter a subsequent cleaning process from the bottom through a cyclone separator, the inorganic scale debris is separated by a filter press, and the separated liquid is circulated back to a buffer tank for recycling; aiming at organic pollutants and inorganic pollutants adsorbed and carried by the solid cleaning particles, the step (3) designs a recycling process after cleaning and regenerating the acid solution and the alkali solution, wherein the acid solution selects 1-2% (v/v) hydrochloric acid to clean and regenerate the inorganic pollutants adsorbed and carried by the solid cleaning particles; and (3) selecting 1-2% (v/v) sodium hydroxide as the alkali liquor, and cleaning and regenerating the organic pollutants adsorbed and carried by the solid cleaning particles.
The invention develops a self-cleaning process technology by combining the ceramic membrane filtration process principle aiming at the pollution characteristic of the shale gas fracturing flowback fluid, and has the advantages of synchronous cleaning and filtration processes, high operation efficiency of equipment, simplicity, convenience, easiness in operation, high cleaning efficiency, no secondary pollution, good economy and the like.
Drawings
The invention will be described in further detail with reference to the following drawings and detailed description:
FIG. 1 is a schematic view of the apparatus of the present invention;
the specific labels in the figure are:
1. the device comprises a buffer tank, 2. a water inlet pump, 3. a water inlet control valve, 4. a ceramic membrane filter, 5. a pressure gauge, 6. a pressure regulating valve, 7. a flow meter, 8. a discharge control valve, 9. a cyclone, 10. a pressure filter, 11. an acid liquor tank, 12. a centrifuge, 13. an alkali liquor tank, 14. a centrifuge and 15. a screw conveyer.
Detailed Description
The invention will be better understood from the following examples. However, those skilled in the art will readily appreciate that the description of the embodiments is only for illustrating the present invention and should not be taken as limiting the invention as detailed in the claims.
Example 1
In the embodiment, inorganic ceramic membrane filtration operation is performed on the fracturing flow-back fluid of a certain well in the Sichuan shale gas development area, the COD of the fracturing flow-back fluid is 186mg/L, and the technology is compared with a method without adopting two ceramic membrane devices for filtration treatment. Homogenizing and buffering the flowback liquid, keeping the pH value of a water sample unchanged, then respectively adding 10L of fracturing flowback liquid into a ceramic membrane feed liquid tank, adding 5g/L of solid cleaning particles into one ceramic membrane feed liquid tank in the circulating and filtering operation process of the fracturing flowback liquid, not adding the other ceramic membrane feed liquid, adjusting the filtering pressure to be 0.15MPa for operation when a ceramic membrane starts to operate, controlling the ratio of the circulating flow to the water inflow of the shale gas fracturing flowback liquid to be 50:1, and controlling the surface liquid flow rate of the ceramic membrane to be 10L/s.m.2. The flux of the inorganic ceramic membrane added with the solid cleaning particles in the same 3-hour filtration time is 605L/(m)2H) down to 492L/(m)2H) the water outlet rate of the inorganic ceramic membrane without adding solid cleaning particles is 605L/(m)2H) down to 348L/(m)2H). The filter working time of the filter without solid cleaning particles is about 8-10 hours and the filter with solid cleaning particles is about 116-1 hours on the basis of 70% reduction of the filter water flux of the ceramic membraneFor 22 hours.
Example 2
In the embodiment, inorganic ceramic membrane filtration operation is performed on the fracturing flow-back fluid of a certain well in the Sichuan shale gas development area, the COD of the fracturing flow-back fluid is 656mg/L, and the technology is compared with a method which does not adopt two ceramic membrane devices for filtration treatment. Homogenizing and buffering the flowback liquid, keeping the pH value of a water sample unchanged, then respectively adding 10L of fracturing flowback liquid into a ceramic membrane feed liquid tank, adding 8g/L of solid cleaning particles into one ceramic membrane feed liquid tank in the circulating and filtering operation process of the fracturing flowback liquid, not adding the other ceramic membrane feed liquid, adjusting the filtering pressure to be 0.20MPa for operation when a ceramic membrane starts to operate, controlling the ratio of the circulating flow to the water inflow of the shale gas fracturing flowback liquid to be 40:1, and controlling the surface liquid flow rate of the ceramic membrane to be 15L/s.m.2. The flux of the inorganic ceramic membrane added with the solid cleaning particles in the same 3-hour filtration time is 560L/(m)2H) to 469L/(m)2H), the water outlet rate of the inorganic ceramic membrane without adding solid cleaning particles is 560L/(m)2H) down to 357L/(m)2H). The filter working time of the filter without the solid body for cleaning particles is about 4-5 hours, and the filter with the solid body for cleaning particles is about 72-76 hours.
Example 3
In the embodiment, inorganic ceramic membrane filtration operation is performed on the fracturing flow-back fluid of a certain well in the Sichuan shale gas development area, the COD of the fracturing flow-back fluid is 1228mg/L, and the technology is compared with a method which does not adopt two ceramic membrane devices for filtration treatment. Homogenizing and buffering the flowback liquid, keeping the pH value of a water sample unchanged, then respectively adding 10L of fracturing flowback liquid into a ceramic membrane feed liquid tank, adding 10g/L of solid cleaning particles into one ceramic membrane feed liquid tank in the circulating and filtering operation process of the fracturing flowback liquid, not adding the other ceramic membrane feed liquid, adjusting the filtering pressure to be 0.25MPa for operation when a ceramic membrane starts to operate, controlling the ratio of the circulating flow to the water inflow of the shale gas fracturing flowback liquid to be 30:1, and controlling the surface liquid flow rate of the ceramic membrane to be 20L/s.m.2. During the same filtration time of 3 hours,the membrane flux of the inorganic ceramic membrane added with the solid cleaning particles is 525L/(m)2H) down to 437L/(m)2H) the water outlet rate of the inorganic ceramic membrane without adding solid cleaning particles is 525L/(m)2H) down to 261L/(m)2H). The filter working time of cleaning particles without fixing bodies is about 3-4 hours, and the filter working time of cleaning particles with fixing bodies is about 66-68 hours.

Claims (4)

1. An inorganic ceramic membrane self-cleaning filtering method for shale gas fracturing flowback fluid is characterized in that aiming at the problem of pollution on the membrane surface when the inorganic ceramic membrane filters the shale gas fracturing flowback fluid, solid cleaning particles are added into the shale gas fracturing flowback fluid to be filtered, and in the filtering process, the solid cleaning particles perform collision, crushing, adsorption and carrying effects on pollutants adsorbed on the surface of the inorganic ceramic membrane along with the flow of feed liquid, so that organic pollutants and inorganic pollutants on the surface of the ceramic membrane are removed, and self-cleaning of the surface of the ceramic membrane in the filtering process is realized; the solid cleaning particles are made of hickory shells; preparing solid cleaning particles by using hickory shells, crushing and screening the hickory shells, putting the hickory shells into mixed acid of sulfuric acid with the volume ratio concentration of 1-2% and nitric acid with the volume ratio of 0.5-1%, soaking for 1-2 hours, filtering and cleaning; heating to 300-400 ℃ at a heating rate of 10-15 ℃/min for 3-4 h, controlling the volume concentration of oxygen to be 1-5% in the heating process, and taking out after cooling; the prepared solid cleaning particles are polygonal, the particle size is 1-2 mm, and the particle density is 1.2-1.6 g/cm3The porosity of the particles is 27% -50%, and the molar hardness is 3-4.
2. The self-cleaning filtration process of claim 1 wherein the solid cleaning particles are mixed with the shale gas fracking flowback fluid in a surge tank, the concentration of the solid cleaning particles in the feed liquid being controlled to be in the range of 5g/L to 10 g/L.
3. The self-cleaning filtration process of claim 1, wherein the inorganic is controlledIn the process of circulating flow of the feed liquid in the ceramic membrane filter, the ratio of the circulation flow of the feed liquid in the inorganic ceramic membrane filter to the water inflow is 30: 1-50: 1, the filtering pressure is 0.15 MPa-0.25 MPa, and the flow velocity of the liquid on the surface of the inorganic ceramic membrane is 10-20L/s.m2
4. The self-cleaning filtration method of claim 1, wherein the solid cleaning particles are recycled after being cleaned and regenerated by an acid solution and an alkali solution respectively after being separated from inorganic contaminants by the cyclone separator, wherein the acid solution is hydrochloric acid with a volume concentration of 1-2%, and the alkali solution is sodium hydroxide solution with a volume concentration of 1-2%.
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1616140A (en) * 2004-09-29 2005-05-18 高邮市铸锋机械制造有限公司 Film filter
US20110186513A1 (en) * 2010-02-04 2011-08-04 Dxv Water Technologies, Llc Water treatment systems and methods

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1616140A (en) * 2004-09-29 2005-05-18 高邮市铸锋机械制造有限公司 Film filter
US20110186513A1 (en) * 2010-02-04 2011-08-04 Dxv Water Technologies, Llc Water treatment systems and methods

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