CN115721967B - Coalescing material for oil-water separation and preparation method thereof, coalescing filter element, oil-water separator and oil-water separation method - Google Patents
Coalescing material for oil-water separation and preparation method thereof, coalescing filter element, oil-water separator and oil-water separation method Download PDFInfo
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- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 5
- 238000007654 immersion Methods 0.000 claims description 5
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Abstract
The present disclosure relates to coalescing materials for oil-water separation and methods of making the same, coalescing filter cartridges, oil-water separators, and methods of oil-water separation. The preparation method comprises the following steps: under the first impregnation condition, carrying out first impregnation treatment on the stainless steel mesh in an acidic copper salt solution to obtain a copper-deposited stainless steel mesh; under the second impregnation condition, carrying out second impregnation treatment on the stainless steel mesh deposited by copper in a silicon-containing polymer solution to obtain a stainless steel mesh attached by a silicon-containing polymer; and under the curing condition, the stainless steel net attached with the silicon-containing polymer is subjected to curing treatment. The surface of the coalescing material provided by the disclosure has excellent oleophilic and hydrophobic properties, and oil drops can be quickly wetted and spread on the surface of the coalescing material; when the oil remover is used for removing oil from waste water, coalescence and buoyancy of dispersed phase oil drops can be forcefully promoted, so that the oil removal efficiency is improved.
Description
Technical Field
The present disclosure relates to the field of oil-water separation, and in particular, to a coalescing material for oil-water separation and a preparation method thereof, a coalescing filter element, an oil-water separator, and an oil-water separation method.
Background
The process of crude oil exploitation, transportation, storage and refining all produce a large amount of oily wastewater. The oily wastewater has complex components and high treatment difficulty, and seriously threatens the water environment and human health. Petroleum substances in oily wastewater can be generally classified into floating oil, dispersed oil, emulsified oil and dissolved oil according to physical state. Because the solubility of water to petroleum substances is low, the wastewater oil removal mainly aims at floating oil, dispersed oil and emulsified oil, wherein the technical difficulty of separating and removing the emulsified oil is high.
At present, the oil removal method for wastewater can be categorized into four main categories: physical, chemical, physicochemical, and biochemical methods. The physical method is a separation method using differences in physical properties such as density of oil-water two phases, wettability and spreadability on the surface of a solid material, and existence of morphology, and mainly includes gravity sedimentation, cyclone, coalescence (also called "coarse granulation"), filtration separation, membrane separation, and the like. The chemical method mainly comprises coagulation/flocculation sedimentation, namely adding a proper amount of chemical agent (coagulant or flocculant) into the wastewater to destroy the stability of an oil-water interface, so that small-particle-size oil drops and the coagulant/flocculant are promoted to form floccules which are easy to settle. The physical and chemical method combines physical separation and chemical separation, thereby achieving the purpose of oil-water separation. For example, air flotation processes typically require the addition of flocculants or demulsifiers to the wastewater in order to increase the efficiency of oil removal. The biological method is to degrade and consume petroleum hydrocarbon in the wastewater by utilizing microorganisms, and mainly comprises an activated sludge method, a biological filter method, an aeration biological filter method and the like.
Among the above oil removal methods, the coalescing method realizes oil-water separation by means of wettability difference of coalescing materials on oil-water two phases, belongs to the oil-water separation technology of a physical method, has the advantages of small equipment, simple operation, low cost and the like, is regarded as an excellent oil removal method with wide prospects, and is widely studied and applied. However, the conventional coalescing materials generally have the problems of poor selective separation capability or poor pollution resistance, short service life and the like, and the separation effect on the high-oil-content wastewater is irrational, so that reports on successful industrial application are seen. For example, conventional coalescing materials such as polypropylene, polyvinyl chloride, glass fibers, etc. have low separation accuracy and particularly have poor coalescing effect on emulsified oil droplets. Development of novel coalescing materials with high selective separation capacity and oil-water separation devices based on such materials has become a research hotspot.
Disclosure of Invention
The purpose of the present disclosure is to provide a coalescing material for oil-water separation, a preparation method thereof, a coalescing filter element, an oil-water separator and an oil-water separation method, which have high selective separation capability for oily wastewater, and improve the oily wastewater treatment effect.
To achieve the above object, a first aspect of the present disclosure provides a method of preparing a coalescing material for oil-water separation, comprising the steps of: under the first impregnation condition, carrying out first impregnation treatment on the stainless steel mesh in an acidic copper salt solution, and then washing and drying to obtain a copper-deposited stainless steel mesh; under the second impregnation condition, carrying out second impregnation treatment on the stainless steel mesh deposited by copper in a silicon-containing polymer solution to obtain a stainless steel mesh attached by a silicon-containing polymer; and under the curing condition, the stainless steel net attached with the silicon-containing polymer is subjected to curing treatment.
Optionally, the first impregnation condition includes: the temperature is 5-45 ℃ and the time is 1-3600s; preferably, the temperature is 10-35 ℃ and the time is 100-2400s.
Optionally, the acidic copper salt solution is an aqueous solution comprising a copper salt and a mineral acid; wherein the copper salt is one or more of copper chloride, copper sulfate and copper nitrate; the inorganic acid is selected from one or more of hydrochloric acid, sulfuric acid and nitric acid;
Preferably, in the acidic copper salt solution: the concentration of copper ions is 0.1-2mol/L, and the pH value is not more than 4; preferably, the concentration of copper ions is 0.1-1.5mol/L and the pH is below 2;
optionally, the stainless steel mesh is 201 stainless steel mesh and 304 stainless steel mesh, and the pore diameter of the stainless steel mesh is 3-90 μm.
Optionally, the second impregnation condition includes: the temperature is 5-45 ℃ and the time is 300-1800s.
Optionally, the silicon-containing polymer solution comprises a silicon-containing polymer, a curing agent, and a solvent; the silicon-containing polymer comprises the following components in percentage by mass: curing agent: solvent = 1:0.1, (50-200);
optionally, the solvent is selected from one of tetrahydrofuran, n-hexane, cyclohexane, n-heptane and petroleum ether; preferably, the solvent is selected from n-hexane or cyclohexane;
Optionally, the curing agent is selected from at least one of aniline methyltriethoxysilane, ethyl orthosilicate or aminopropyl triethoxysilane.
Alternatively, the silicon-containing polymer is aminopropyl double-ended polydimethylsiloxane or hydroxyl-terminated polydimethylsiloxane; preferably, the silicon-containing polymer has a structure as shown in formula I and/or formula II below:
Wherein n is a positive integer;
Wherein m is a positive integer;
Preferably, the number average molecular weight of the silicon-containing polymer is 10 4～105 g/mol.
Optionally, the curing conditions include: the temperature is 80-130 ℃ and the time is 0.5-6h.
Optionally, the method further comprises the step of washing and drying the copper deposited stainless steel mesh prior to performing the second impregnation treatment.
A second aspect of the present disclosure provides a coalescing material prepared by the method of the first aspect of the present disclosure.
A third aspect of the present disclosure provides a coalescing filter cartridge for oil-water separation, comprising a porous center tube and a coalescing material layer coated on an outer wall of the porous center tube; the layer of coalescing material comprises the coalescing material of the second aspect of the present disclosure.
Optionally, the coalescing filter element comprises a plurality of stacked coalescing material layers, wherein the pore diameters of stainless steel meshes of the coalescing material layers are sequentially increased from inside to outside; preferably, among the plurality of coalescing material layers, the pore size of the innermost coalescing material layer is 3 to 10 μm and the pore size of the outermost coalescing material layer is 20 to 90 μm.
A fourth aspect of the present disclosure provides an oil-water separator comprising a cylinder, a water inlet, a tube sheet, an oil collection chamber, a water outlet, a drain outlet, and a coalescing filter element according to the third aspect of the present disclosure; wherein, the cylinder body is internally and sequentially provided with a water inlet distribution area, a coalescence area and a buoyancy lift separation area along the axial direction; the tube plate is arranged in the cylinder body along the radial direction of the cylinder body, and the opening edge of the tube plate is in circumferential sealing connection with the side wall of the cylinder body so as to separate the water inlet distribution area and the coalescence area; the water inlet is positioned at the upper part of the cylinder body of the water inlet distribution area; the sewage outlet is positioned at the lower part of the cylinder body of the water inlet distribution area; the coalescing filter element is disposed within the coalescing zone, and a first end opening of a porous center tube of the coalescing filter element is in communication with an outlet of the water inlet distribution zone such that the water inlet distribution zone is in fluid communication with the coalescing filter element interior only through an opening of the tube sheet; the second end of the porous center tube is closed so that the inner side and the outer side of the coalescing filter element are communicated only through the side wall openings of the coalescing filter element; the oil collecting chamber and the water outlet are respectively arranged at the upper part and the lower part of the cylinder body of the buoyancy separation zone.
Optionally, the oil-water separator comprises a plurality of said coalescing filter elements; the number and the size of the open holes on the tube plate are corresponding to the first end openings of the coalescing filter elements; the coalescing filter elements are respectively and axially parallel to the cylinder body and are uniformly arranged at intervals; preferably, the cylinder is of a horizontal cylinder structure; optionally, the oil-water separator further comprises a fluid distributor, wherein the fluid distributor is radially arranged in the water inlet distribution area along the cylinder body and is close to the tube plate; the edge of the fluid distributor is in circumferential sealing connection with the side wall of the cylinder.
A fifth aspect of the present disclosure provides a method for separating oil from water, which adopts the oil-water separator of the fourth aspect of the present disclosure, and makes the oily wastewater enter the oil-water separator through the water inlet of the cylinder; after passing through the water inlet distribution area, the water flows into the coalescing filter element, and flows through the porous central tube of the coalescing filter element and the coalescing material layer from inside to outside in sequence to perform oil-water separation treatment, so as to obtain gathered floating oil and purified water; collecting the gathered floating oil from the oil collecting chamber and collecting purified water from the water outlet.
Optionally, the method further comprises: the flow pattern of the oily wastewater maintains a laminar flow state as the oily wastewater flows through the apertures of the porous center tube of the coalescing filter element and the coalescing material layer by controlling the amount of the oily wastewater that enters.
Through the technical scheme, the disclosure provides the coalescing material for oil-water separation and the preparation method thereof. The method comprises the steps of carrying out first dipping treatment on the stainless steel mesh in acidic copper salt solution, washing with water after the dipping is finished, and then drying to obtain the stainless steel mesh with copper particles deposited, so that the surface roughness of the stainless steel mesh is increased, a rough structure is constructed, the subsequent silicon-containing polymer is favorably attached, and the coalescing performance of materials on oily wastewater is enhanced; and (3) carrying out second dipping treatment on the stainless steel mesh deposited with copper in a silicon-containing polymer solution to obtain a stainless steel mesh attached with the silicon-containing polymer, and then, after solidification, coating the surface of the stainless steel mesh deposited with copper particles by the silicon-containing polymer, so that the surface energy of the stainless steel mesh can be reduced, the surface of the modified stainless steel mesh presents hydrophobic and oleophylic characteristics, has high selective separation capability on oily wastewater, and can improve the treatment effect of the oily wastewater. The coalescing material provided by the disclosure has the advantages of simple preparation process, low cost, suitability for large-scale production, stable performance and long-period use.
The surface of the coalescing material provided by the disclosure has excellent oleophylic and hydrophobic characteristics, the static contact angle of a water drop on the surface of the coalescing material is larger than 120 degrees, the static contact angle of an oil drop on the surface of the coalescing material is close to 0 degree, and the oil drop can be quickly wetted and spread on the surface of the coalescing material; when the oil remover is used for removing oil from waste water, coalescence and buoyancy of dispersed phase oil drops can be forcefully promoted, so that the oil removal efficiency is improved.
The coalescing filter element and the oil-water separator based on the coalescing material have the characteristics of wide application range of water quality of oily wastewater and high oil removal efficiency.
Additional features and advantages of the present disclosure will be set forth in the detailed description which follows.
Drawings
The accompanying drawings are included to provide a further understanding of the disclosure, and are incorporated in and constitute a part of this specification, illustrate the disclosure and together with the description serve to explain, but do not limit the disclosure. In the drawings:
fig. 1 is a schematic structural diagram of an oil-water separator provided by the present disclosure;
FIG. 2 is a cross-sectional view of a coalescing filter cartridge provided by the present disclosure;
FIG. 3 is a photograph of the appearance of the agglomerate material produced in example 2;
FIG. 4 is a scanning electron microscope image of the coalescing material prepared in example 2;
FIG. 5 is an EDS spectrum of the agglomerate material produced in example 2;
FIG. 6 is a static contact angle of a water droplet on the surface of the coalescing material prepared in example 2;
fig. 7 is a static contact angle of oil droplets on the surface of the coalescing material prepared in example 2.
Description of the reference numerals
1-Cylinder, 2-water inlet, 3-fluid distributor, 4-coalescing filter element, 5-oil collecting chamber, 6-water outlet, 7-drain outlet, 8-porous central tube, 9-small Kong Jujie material layers, 10-medium Kong Jujie material layers and 11-large Kong Jujie material layers.
I-water distribution zone, II-coalescence zone, III-buoyancy separation zone.
Detailed Description
Specific embodiments of the present disclosure are described in detail below with reference to the accompanying drawings. It should be understood that the detailed description and specific examples, while indicating and illustrating the disclosure, are not intended to limit the disclosure.
In the present disclosure, unless otherwise indicated, the terms "first," "second," and the like are used merely to distinguish between different components and do not have the actual meaning of a tandem connection sequence. In this disclosure, terms such as "upper" and "lower" are used to refer to the upper and lower portions of the device in normal use, and "inner" and "outer" are used with respect to the device profile.
A first aspect of the present disclosure provides a method of preparing a coalescing material for oil-water separation, comprising the steps of:
Under the first impregnation condition, carrying out first impregnation treatment on the stainless steel mesh in an acidic copper salt solution, and then washing and drying to obtain a copper-deposited stainless steel mesh;
under the second impregnation condition, carrying out second impregnation treatment on the stainless steel mesh deposited by copper in a silicon-containing polymer solution to obtain a stainless steel mesh attached by a silicon-containing polymer;
and under the curing condition, the stainless steel net attached with the silicon-containing polymer is subjected to curing treatment.
The method comprises the steps of carrying out first dipping treatment on a stainless steel mesh in an acidic copper salt solution, washing with water after the dipping is finished, and then drying to obtain a copper-deposited stainless steel mesh, so that the surface roughness of the stainless steel mesh is increased, a coarse structure is constructed, the adhesion of a subsequent silicon-containing polymer is facilitated, and the coalescing performance of the material on oily wastewater is enhanced; and (3) carrying out second impregnation treatment on the stainless steel mesh deposited with copper in a silicon-containing polymer solution to obtain a stainless steel mesh attached with a silicon-containing polymer, and then, after solidification, coating the surface of the stainless steel mesh deposited with copper particles by the silicon-containing polymer, so that the surface energy of the stainless steel mesh can be reduced, the surface of the modified stainless steel mesh presents excellent hydrophobic and oleophylic characteristics, the contact angle of water drops is larger than 120 degrees, the contact angle of oil drops is 0 degree, the high-selectivity separation capability is realized on oily wastewater, and the treatment effect of the oily wastewater can be improved.
In the method, copper obtained through the first dipping treatment is deposited on a stainless steel mesh on the surface, the deposited copper exists in a form of tiny particles, and copper particles are obtained through substitution reaction of iron element in the stainless steel mesh and copper ions in an acidic copper salt solution. In the present disclosure, the impregnation process is based on the stainless steel mesh being completely immersed.
In one embodiment, the acidic copper salt solution is an aqueous solution comprising a copper salt and a mineral acid; wherein the copper salt is one or more of copper chloride, copper sulfate and copper nitrate; the inorganic acid is selected from one or more of hydrochloric acid, sulfuric acid and nitric acid.
In a preferred embodiment, the acidic copper salt solution is: the concentration of copper ions is 0.1-2mol/L, and the pH value is below 4; in a further preferred embodiment, the copper ion concentration is 0.1 to 1.5mol/L and the pH is 2 or less.
In one embodiment, the stainless steel mesh is 201 stainless steel mesh and 304 stainless steel mesh, and the pore size of the stainless steel mesh is 3-90 μm.
In one embodiment, the first impregnation condition includes: the temperature is 5-45 ℃ and the time is 1-3600s; preferably, the temperature is 10-35 ℃ and the time is 100-2400s.
In one embodiment, the silicon-containing polymer solution comprises a silicon-containing polymer, a curing agent, and a solvent; the silicon-containing polymer comprises the following components in percentage by mass: curing agent: solvent=1:0.1 (50-200).
In a preferred embodiment, the silicon-containing polymer is an aminopropyl bis-terminated polydimethylsiloxane or a hydroxyl-terminated polydimethylsiloxane; preferably, the silicon-containing polymer has a structure as shown in formula I and/or formula II below:
Wherein n is a positive integer;
Wherein m is a positive integer.
In one embodiment, the silicon-containing polymer has a number average molecular weight of 10 4～105 g/mol; for example, n in formula I can be any of 140 to 1500 and m in formula II can be any of 140 to 1500, such that the number average molecular weight of the silicon-containing polymer is within the stated range.
The silicon-containing polymer raw materials provided by the embodiment are easy to obtain, and are beneficial to further improving the oleophilic and hydrophobic properties of the coalesced material.
In one embodiment, the solvent is selected from one of tetrahydrofuran, n-hexane, cyclohexane, n-heptane, petroleum ether, and the solvent employed in the present disclosure is easily removed by evaporation.
In one embodiment, the curing agent is selected from at least one of aniline methyltriethoxysilane, ethyl orthosilicate, or aminopropyl triethoxysilane.
In a specific embodiment, the method further comprises the step of washing and drying the copper deposited stainless steel mesh prior to performing the second impregnation treatment.
In one embodiment, the second impregnation condition includes: the temperature is 5-45 ℃ and the time is 300-1800s.
In one embodiment, the curing conditions include: the temperature is 80-130 ℃ and the time is 0.5-6h; the curing treatment is preferably performed under vacuum.
A second aspect of the present disclosure provides a coalescing material prepared by the method of the first aspect of the present disclosure.
The surface of the coalescing material provided by the disclosure has excellent oleophylic and hydrophobic characteristics, the static contact angle of a water drop on the surface of the coalescing material is larger than 120 degrees, the static contact angle of an oil drop on the surface of the coalescing material is close to 0 degrees, and the oil drop can be quickly wetted and spread on the surface of the coalescing material; when the oil remover is used for removing oil from waste water, coalescence and buoyancy of dispersed phase oil drops can be forcefully promoted, so that the oil removal efficiency is improved.
A third aspect of the present disclosure provides a coalescing filter cartridge for oil-water separation, see fig. 2, comprising a porous central tube 8 and a layer of coalescing material coating the outer wall of the porous central tube; the layer of coalescing material comprises the coalescing material of the second aspect of the present disclosure.
In one embodiment, referring to fig. 2, the coalescing filter element comprises a plurality of layers of coalescing material stacked, the pore size of the stainless steel mesh of the plurality of layers of coalescing material increases sequentially from inside to outside. In the embodiment, a plurality of coalescing material layers are coated on the outer wall of the porous central tube in a mode that the pore diameters are sequentially increased from inside to outside, so that coalescence and buoyancy of separated dispersed phase oil drops are facilitated in treatment of oily wastewater.
In one embodiment, as shown in FIG. 2, the coalescing filter element comprises 3 layers of stacked coalescing material, including a small Kong Jujie layer of material 9, a medium Kong Jujie layer of material 10, and a large Kong Jujie layer of material 11; wherein the pore size of the stainless steel mesh of the small Kong Jujie material layer 9, the medium Kong Jujie material layer 10 and the large Kong Jujie material layer 11 increases in sequence.
In a preferred embodiment, the pore size of the innermost layer of the plurality of layers of coalescing material is in the range of 3 to 10 μm and the pore size of the outermost layer of coalescing material is in the range of 20 to 90 μm. The pore diameter of the pore opening of the pipe wall of the porous central pipe 8 is 5-20mm.
A fourth aspect of the present disclosure provides an oil-water separator, referring to fig. 1, which includes a cylinder 1, a water inlet 2, a tube sheet, a collection chamber 5, a water outlet 6, a drain 7, and a coalescing filter element 4 according to the third aspect of the present disclosure;
Wherein, a water inlet distribution area I, a coalescence area II and a buoyancy lift separation area III are sequentially arranged in the cylinder body 1 along the axial direction; the tube plate is arranged in the cylinder 1 along the radial direction of the cylinder 1, and the opening edge of the tube plate is in circumferential sealing connection with the side wall of the cylinder 1 so as to separate a water inlet distribution area I and a coalescence area II; the water inlet 2 is positioned at the upper part of the cylinder 1 in the water inlet distribution area I; the sewage outlet 7 is positioned at the lower part of the cylinder body 1 in the water inlet distribution area I;
The coalescing filter element 4 is arranged in the coalescing zone II, and the first end opening of the porous central tube 8 of the coalescing filter element 4 is communicated with the outlet of the water inlet distribution zone I, so that the water inlet distribution zone I is in fluid communication with the interior of the coalescing filter element 4 only through the opening of the tube plate; the second end of the porous central tube 8 is closed so that the inside and outside fluids of the coalescing filter element 4 communicate only through the sidewall openings of the coalescing filter element 4;
the oil collecting chamber 5 and the water outlet 6 are respectively arranged at the upper part and the lower part of the cylinder body 1 of the buoyancy separation zone III.
The oil-water separator based on the coalescing material has the characteristics of wide application range and high oil removal efficiency on the water quality of oily wastewater; according to the water inlet distribution area, the drain outlet is arranged in the water inlet distribution area and can be used for discharging particulate matters which are brought into and deposited in the water inlet distribution area by the water flow at an irregular period, so that the operation stability of the oil-water separator is improved.
In the present disclosure, the porous central tube may be made of materials conventionally selected in the art, such as 304 steel and 316 steel, and the wall of the porous central tube is provided with uniformly distributed openings for uniformly contacting the oily wastewater inside the porous central tube with the coalescing material and performing separation treatment through the coalescing material.
Devices not limited in this disclosure may employ devices conventionally selected in the art.
In one embodiment, referring to fig. 1, the oil-water separator comprises a plurality of coalescing filter cartridges 4; the number and the size of the open pores on the tube plate are corresponding to the first end openings of the coalescing filter elements 4; the plurality of coalescing cartridges 4 are disposed in parallel with each other in the axial direction and at uniform intervals with respect to the cylinder 1. Preferably, the cylinder 1 is of a horizontal cylinder structure;
in one embodiment, referring to fig. 1, the oil-water separator further comprises a fluid distributor 3, wherein the fluid distributor 3 is radially arranged in the water inlet distribution area I along the cylinder 1 and is close to the tube plate; the edge of the fluid distributor 3 is in circumferential sealing connection with the side wall of the cartridge 1.
In a specific embodiment, referring to fig. 1, a first side wall and a second side wall which are correspondingly arranged are axially included in a barrel 1, a water flow distributor 3 is arranged in the barrel 1 and is close to the first side wall, and a water inlet distribution area I is formed by the interval between the water flow distributor 3 and the first side wall; the coalescing filter element 4 is axially and horizontally arranged in the cylinder 1, and the central axis of the coalescing filter element 4 is parallel to the central axis of the cylinder 1; the first end opening of the coalescing filter element is adjacent the water flow distributor 3; the tube plate is arranged between the water flow distributor 3 and the coalescing filter element 4 and is spaced from the water flow distributor 3; the tube plate is connected with the inner wall of the cylinder body 1 along the edge of the opening, an opening is arranged on the tube plate, and the opening is matched with the opening at the first end of the porous central tube 8 of the coalescing filter element 4; in particular, this embodiment may comprise two or more coalescing filter cartridges 4, wherein the first end opening of each coalescing filter cartridge 4 is sealingly connected to the aperture of the tube sheet along the edge of the opening, such that water entering the compartment via the water flow distributor 3 only passes through the aperture of the tube sheet into the perforated central tube 8 of the coalescing filter cartridge 4; the second end of the porous central tube 8 of the coalescing filter element 4 is closed so that the inside and outside fluid of the coalescing filter element 4 are in communication only through the sidewall openings of the coalescing filter element 4; the oil collecting chamber 5 is arranged at the upper part of the cylinder body 1 of the buoyancy lift separation zone and is close to the second side wall, and the oil collecting chamber 5 comprises a buoyancy oil inlet and an oil discharge outlet; the floating oil inlet is communicated with the inside of the cylinder body 1; the water outlet 6 is arranged at the lower part of the cylinder body 1 and is close to the second side wall. Further, the number of the coalescing filter elements 4 can be adjusted according to the treatment amount of the oily wastewater, and the larger the treatment amount of the oily wastewater is, the larger the number of the coalescing filter elements 4 is.
The specific working principle of the oil-water separator shown in fig. 1 provided by the disclosure includes: the oily wastewater to be treated enters a water inlet distribution area I in a barrel body 1 of the oil-water separator through a water inlet 2; the oily wastewater is then uniformly distributed and enters the space between the fluid distributor 3 and the tube plate through the openings in the fluid distributor 3, and then enters the inside of the porous central tube 8 of each coalescing filter element 4 through the openings in the tube plate; in each coalescing filter element, the oily wastewater flows out through the openings on the wall of the porous central tube 8 and then sequentially flows through a plurality of coalescing material layers stacked in the coalescing filter element 4 from inside to outside, and in the process, oil drops can be quickly wetted and spread on the surface of the coalescing material due to the wettability difference of oil water on the surface of the coalescing material, so that the wetting and coalescing of the oil drops are realized; the coalescing materials are sequentially wrapped from inside to outside according to the sequence of the pore diameters of the stainless steel mesh from the small to the large, so that the oil-containing wastewater can promote collision coalescence of oil drops and reduce the possibility that the oil drops are torn into small oil drops again in the flowing process from the inside to the outside; after passing through the coalescence material of the outermost layer, the oil drops which are carried by the water flow and are coalesced in the coalescence material layer continue to coalesce, and the oil drops float to the water surface under the action of the oil-water density difference and are collected and discharged by the oil collecting chamber 5 at the upper part of the cylinder body 1; purified water obtained by separation is discharged through a water outlet 6 at the lower part of the cylinder body 1. In addition, particulate matter that is entrained and deposited in the intake distribution area I may be periodically discharged from the drain 7.
A fifth aspect of the present disclosure provides a method for separating oil from water, using the oil-water separator of the fourth aspect of the present disclosure, including the steps of:
Enabling the oily wastewater to enter an oil-water separator through a water inlet of the cylinder body 1; after passing through the water inlet distribution area I, the water flows into the coalescing filter element 4, and flows through the porous central tube 8 and the coalescing material layer of the coalescing filter element 4 from inside to outside in sequence to carry out oil-water separation treatment, so as to obtain gathered floating oil and purified water;
The collected oil slick is collected from the oil collecting chamber 5, and purified water is discharged from the water outlet 6.
In a further embodiment, the method further comprises: the flow pattern of the oily wastewater is maintained in a laminar flow state by controlling the amount of the oily wastewater entering so that the oily wastewater flows through the apertures of the porous central tube 8 of the coalescing filter element 4 and the coalescing material layer.
In particular, the oily wastewater in the present disclosure may be coker fractionator overhead condensate, electrical desalted drainage, oilfield produced water, and the like.
The present disclosure will be further illustrated by the following examples.
In the following examples, the test conditions for scanning electron microscopy of the coalescing material included: a Hitachi S-4800 scanning electron microscope (SEM; shimadzu corporation) is adopted to sample the surface microscopic morphology of the material sample under the condition of 5kV working voltage and a certain magnification; and the surface elements of the material sample are tested by adopting SEM-EDS.
The test conditions for conducting the static contact angle test of water drops and oil drops on the surface of the coalescence material comprise: contact angle data were determined using the Kjeldahl drop analysis system (DSA 100), and a 5. Mu.L sessile drop method.
The measurement of the oil content before and after the treatment of the oily wastewater is carried out by the method described in HJ 637-2018 (infrared spectrophotometry for measuring the oil quality of petroleum and animal and vegetable oils).
Hydroxy-terminated polydimethylsiloxane (number average molecular weight 10 4～105 g/mol, viscosity 5500 cps at 25 ℃), aminopropyl-terminated polydimethylsiloxane (number average molecular weight 10 4～105 g/mol, viscosity 5500 cps at 25): the molecular weight and viscosity of the polydimethylsiloxanes of the present disclosure are based on the specifications of the purchased product, as purchased from beijing enoKai technologies.
Example 1
Stainless steel mesh: a 201 stainless steel mesh with pore diameters of 6 μm, 22 μm and 87 μm respectively.
The following operations are respectively carried out on each stainless steel net:
acidic copper salt solution: the concentration of the copper chloride solution is 0.1mol/L, and inorganic acid (hydrochloric acid) is added to adjust the pH to 1. Immersing the stainless steel mesh in acid copper salt for 5s at 13 ℃ to obtain the stainless steel mesh deposited with copper particles.
Taking out the stainless steel mesh deposited by copper particles, washing with water and drying; the rinsed stainless steel mesh is then immersed in a solution of a silicon-containing polymer, wherein the silicon-containing polymer solution comprises: the mass ratio of the aminopropyl-terminated polydimethylsiloxane to the curing agent (aminopropyl triethoxysilane) to the tetrahydrofuran is 1:0.1:123.9, the dipping time is 480s, the dipping temperature is 21 ℃, and the stainless steel net attached with the silicon-containing polymer is obtained.
The stainless steel mesh with the silicon-containing polymer attached was taken out and placed in a vacuum oven at 100 ℃ for drying and curing for 4 hours, to obtain a stainless steel mesh (coalescent material) with the surface coated with the silicon-containing polymer.
Three kinds of coalescing materials obtained by stainless steel meshes with three kinds of apertures are sequentially coated on the outer wall of a porous central tube according to the sequence arrangement of gradually increasing apertures, wherein the diameter of the porous central tube is 100mm, the aperture on the tube wall is 5mm, and the coalescing filter element is obtained, as shown in figure 2.
The construction of the separator is shown in figure 1, with two coalescing cartridges installed. The oil-water separation process comprises the following steps: enabling the oily wastewater to enter an oil-water separator through a water inlet of the cylinder body 1; after passing through the water inlet distribution area I, the water flows into the coalescing filter element 4, and flows through the porous central tube 8 and the coalescing material layer of the coalescing filter element 4 from inside to outside in sequence to carry out oil-water separation treatment, so as to obtain gathered floating oil and purified water; the collected oil slick is collected from the oil collecting chamber 5, and the purified water is collected from the water outlet 6.
The oil removal effect on the condensate water at the top of the coking fractionation column was evaluated, and the evaluation results are shown in table 1.
Comparative example 1
The same three pore size stainless steel mesh as in example 1 was used without surface treatment.
The untreated stainless steel meshes with three pore diameters are sequentially coated on the outer wall of a porous central tube according to the sequence of gradually increasing pore diameters, wherein the pipe diameter of the porous central tube is 100mm, the pore diameter on the pipe wall is 5mm, and the coalescing filter element is obtained, as shown in figure 2.
The structure of the oil-water separator is shown in fig. 1, and two coalescing filter elements 4 are arranged in the oil-water separator. The oil-water separation process was the same as in example 1. The oil removal effect on the condensate water at the top of the coking fractionation column was evaluated, and the evaluation results are shown in table 1.
Comparative example 2
A coalescing material was prepared using the same reagents and methods as example 1, except that example 1: the impregnation treatment is not carried out by adopting an acidic copper solution, and the impregnation treatment is carried out on the stainless steel mesh with three pore diameters by adopting a polymer solution containing silicon, and then the solidification treatment is carried out. A stainless steel mesh (coalescing material) surface coated with a silicon-containing polymer was obtained.
Three kinds of coalescing materials obtained by stainless steel meshes with three kinds of apertures are sequentially coated on the outer wall of a porous central tube according to the sequence arrangement of gradually increasing apertures, wherein the diameter of the porous central tube is 100mm, the aperture on the tube wall is 5mm, and the coalescing filter element is obtained, as shown in figure 2.
The construction of the separator is shown in figure 1, with two coalescing cartridges installed. The oil removal effect on the condensate water at the top of the coking fractionation column was evaluated, and the evaluation results are shown in table 1.
Example 2
Stainless steel mesh: the holes were 304 stainless steel mesh with diameters of 6 μm, 20 μm, 62 μm, respectively.
Three types of coalescing materials were obtained as in example 1, with the difference from example 1:
Acidic copper salt solution: the concentration of the copper sulfate solution is 0.11mol/L, and the pH is adjusted to 2 by adding inorganic acid (sulfuric acid).
Immersion time of stainless steel mesh in acidic copper salt: 20min.
Silicon-containing polymer solution: the mass ratio of the hydroxyl-terminated polydimethylsiloxane, the curing agent (ethyl orthosilicate) and the n-hexane is 1:0.1:98.9.
Three kinds of coalescing materials obtained by stainless steel meshes with three kinds of apertures are sequentially coated on the outer wall of a porous central tube according to the sequence arrangement of gradually increasing apertures, wherein the diameter of the porous central tube is 100mm, the aperture on the tube wall is 10mm, and the coalescing filter element is obtained, as shown in figure 2.
The structure of the oil-water separator is shown in figure 1, and two coalescing filter elements are arranged in the oil-water separator. The oil-water separation process was the same as in example 1. The oil removal effect on the electric desalting drain water was evaluated, and the evaluation results are shown in Table 1.
Example 3
Stainless steel mesh: 304 stainless steel mesh with pore diameters of 6 μm, 24 μm and 44 μm respectively.
Three types of coalescing materials were obtained as in example 1, with the difference from example 1:
acidic copper salt solution: the concentration of the copper nitrate solution is 0.11mol/L, and inorganic acid (nitric acid) is added to adjust the pH to 2.
Immersion time of stainless steel mesh in acidic copper salt: 30min.
Silicon-containing polymer solution: the mass ratio of the hydroxyl-terminated polydimethylsiloxane, the curing agent (aniline methyltriethoxysilane) and the cyclohexane is 1:0.1:98.9.
Three kinds of coalescing materials obtained by stainless steel meshes with three kinds of apertures are sequentially coated on the outer wall of a porous central tube according to the sequence arrangement of gradually increasing apertures, wherein the diameter of the porous central tube is 125mm, and the aperture on the tube wall is 8mm, so that a coalescing filter element is obtained, and the coalescing filter element is shown in figure 2.
The structure of the oil-water separator is shown in figure 1, and two coalescing filter elements are arranged in the oil-water separator. The oil-water separation process was the same as in example 1. The oil removal effect on the electric desalting drain water was evaluated, and the evaluation results are shown in Table 1.
Example 4
Stainless steel mesh: 304 stainless steel with pore diameters of 6 μm, 13 μm and 44 μm respectively. ;
Three types of coalescing materials were obtained as in example 1, with the difference from example 1:
Acidic copper salt solution: the concentration of the copper sulfate solution is 0.12mol/L, and the pH is adjusted to 3 by adding inorganic acid (sulfuric acid).
Immersion time of stainless steel mesh in acidic copper salt: and 40min.
Silicon-containing polymer solution: the mass ratio of the hydroxyl-terminated polydimethylsiloxane, the curing agent (ethyl orthosilicate) and the n-hexane is 1:0.1:65.
Three kinds of coalescing materials obtained by stainless steel meshes with three kinds of apertures are sequentially coated on the outer wall of a porous central tube according to the sequence arrangement of gradually increasing apertures, wherein the diameter of the porous central tube is 125mm, and the aperture on the tube wall is 12mm, so that a coalescing filter element is obtained, and the coalescing filter element is shown in figure 2.
The structure of the oil-water separator is shown in figure 1, and two coalescing filter elements are arranged in the oil-water separator. The oil-water separation process was the same as in example 1. The oil removal effect on the electric desalting drain water was evaluated, and the evaluation results are shown in Table 1.
Example 5
Stainless steel mesh: 304 stainless steel mesh with pore diameters of 6 μm, 13 μm and 24 μm respectively.
Three types of coalescing materials were obtained as in example 1, with the difference from example 1:
acidic copper salt solution: the concentration of the copper chloride solution is 0.12mol/L, and inorganic acid (hydrochloric acid) is added to adjust the pH to 1.
Immersion time of stainless steel mesh in acidic copper salt: 20min.
Silicon-containing polymer solution: the mass ratio of the hydroxyl-terminated polydimethylsiloxane, the curing agent (ethyl orthosilicate) and the n-hexane is 1:0.1:98.9.
Three coalescing materials obtained by three stainless steel meshes with the aperture are sequentially coated on the outer wall of a porous central tube 8 according to the sequence arrangement of gradually increasing aperture, wherein the diameter of the porous central tube is 125mm, the aperture on the tube wall is 12mm, and the coalescing filter element 4 is obtained, as shown in figure 2.
The structure of the oil-water separator is shown in fig. 1, and the difference is that: three coalescing filter elements are arranged in the oil-water separator. The oil-water separation process was the same as in example 1. The oil removal effect on the produced water of the oil field was evaluated, and the evaluation results are shown in Table 1.
TABLE 1
According to table 1 above, compared with comparative examples 1 and 2, the coalescing materials, coalescing filter element and oil-water separator provided in the embodiments of the present disclosure can effectively reduce the oil content in the oily wastewater from different sources, and have high oil removal rate and good water-oil separation effect.
In fig. 3, the surface of the coalescing material is copper colored (color not shown), indicating copper particle deposition on the surface of the stainless steel mesh. As can be seen in conjunction with fig. 4 and 5, the present disclosure provides a coalescing material surface having copper particle deposition and coated with a silicon-containing polymer.
As can be seen from fig. 6 and 7, the contact angle of the surface of the coalescing material prepared according to the present disclosure with water drops is 147.3 °; the contact angle with oil drops is 0 degrees, and the oil drops can be spread on the surface of the coalescence material, so that the coalescence material provided by the disclosure has good oleophilic and hydrophobic properties.
The preferred embodiments of the present disclosure have been described in detail above with reference to the accompanying drawings, but the present disclosure is not limited to the specific details of the embodiments described above, and various simple modifications may be made to the technical solutions of the present disclosure within the scope of the technical concept of the present disclosure, and all the simple modifications belong to the protection scope of the present disclosure.
In addition, the specific features described in the above embodiments may be combined in any suitable manner without contradiction. The various possible combinations are not described further in this disclosure in order to avoid unnecessary repetition.
Moreover, any combination between the various embodiments of the present disclosure is possible as long as it does not depart from the spirit of the present disclosure, which should also be construed as the disclosure of the present disclosure.
Claims (22)
1. A method of preparing a coalescing material for oil-water separation comprising the steps of:
Under the first impregnation condition, carrying out first impregnation treatment on the stainless steel mesh in an acidic copper salt solution, and then washing and drying to obtain a copper-deposited stainless steel mesh;
under the second impregnation condition, carrying out second impregnation treatment on the stainless steel mesh deposited by copper in a silicon-containing polymer solution to obtain a stainless steel mesh attached by a silicon-containing polymer;
Under the curing condition, curing the stainless steel net attached with the silicon-containing polymer;
wherein the acidic copper salt solution is an aqueous solution comprising a copper salt and a mineral acid; wherein the copper salt is one or more of copper chloride, copper sulfate and copper nitrate; the inorganic acid is selected from one or more of hydrochloric acid, sulfuric acid and nitric acid;
The silicon-containing polymer is aminopropyl double-end-capped polydimethylsiloxane or hydroxyl-end-hydroxyl polydimethylsiloxane; wherein the silicon-containing polymer has a structure represented by formula I and/or formula II:
(formula I),
Wherein n is a positive integer;
(formula II),
Wherein m is a positive integer.
2. The method of claim 1, wherein the first impregnation condition comprises: the temperature is 5-45 ℃ and the time is 1-3600s.
3. The method of claim 2, wherein the first impregnation condition comprises: the temperature is 10-35 ℃ and the time is 100-2400s.
4. The method according to claim 1 or 2, characterized in that in the acidic copper salt solution: the concentration of copper ions is 0.1-2mol/L, and the pH value is below 4;
The stainless steel mesh is 201 stainless steel mesh and 304 stainless steel mesh, and the aperture of the stainless steel mesh is 3-90 mu m.
5. The method according to claim 4, wherein in the acidic copper salt solution: the concentration of copper ions is 0.1-1.5mol/L, and the pH value is below 2.
6. The method of claim 1, wherein the second impregnation condition comprises: the temperature is 5-45 ℃ and the time is 300-1800s.
7. The method of claim 1, wherein the silicon-containing polymer solution comprises a silicon-containing polymer, a curing agent, a solvent; the silicon-containing polymer comprises the following components in percentage by mass: curing agent: solvent=1:0.1 (50-200).
8. The method according to claim 7, wherein the solvent is one selected from tetrahydrofuran, n-hexane, cyclohexane, n-heptane, petroleum ether;
The curing agent is at least one selected from aniline methyl triethoxysilane, tetraethoxysilane or aminopropyl triethoxysilane.
9. The method of claim 8, wherein the solvent is selected from n-hexane or cyclohexane.
10. The method of claim 1, wherein the silicon-containing polymer has a number average molecular weight of 10 4~105 g/mol.
11. The method of claim 1, wherein the curing conditions comprise: the temperature is 80-130 ℃ and the time is 0.5-6h.
12. The method of claim 1, further comprising the step of washing and drying the copper deposited stainless steel mesh prior to performing the second immersion treatment.
13. A coalesced material prepared by the method of any one of claims 1 to 12.
14. A coalescing filter element for oil-water separation, characterized by comprising a porous central tube (8) and a coalescing material layer coated on the outer wall of the porous central tube (8); the layer of coalescing material comprising the coalescing material of claim 13.
15. The coalescing filter element of claim 14, comprising a plurality of the coalescing material layers stacked, wherein the pore size of the stainless steel mesh of the plurality of coalescing material layers increases sequentially from inside to outside.
16. The coalescing filter element of claim 15, wherein the pore size of the innermost coalescing material of the plurality of coalescing material layers is 3-10 μm and the pore size of the outermost coalescing material is 20-90 μm.
17. An oil-water separator, characterized in that it comprises a cylinder (1), a water inlet (2), a tube sheet, a collection chamber (5), a water outlet (6), a drain outlet (7) and a coalescing filter element (4) according to any of claims 14-16;
Wherein, a water inlet distribution area (I), a coalescence area (II) and a buoyancy lift separation area (III) are sequentially arranged in the cylinder (1) along the axial direction; the tube plate is arranged inside the cylinder (1) along the radial direction of the cylinder (1), and the opening edge of the tube plate is in circumferential sealing connection with the side wall of the cylinder (1) so as to separate the water inlet distribution area (I) and the coalescence area (II); the water inlet (2) is positioned at the upper part of the cylinder (1) of the water inlet distribution area (I); the sewage outlet (7) is positioned at the lower part of the cylinder (1) of the water inlet distribution area (I);
The coalescing filter element (4) is arranged in the coalescing zone (II), and a first end opening of a porous central tube (8) of the coalescing filter element (4) is communicated with an outlet of the water inlet distribution zone (I) so that the water inlet distribution zone (I) is in fluid communication with the interior of the coalescing filter element (4) only through an opening of the tube sheet; the second end of the porous central tube (8) is closed so that the inside and outside fluids of the coalescing filter element (4) are communicated only through the side wall openings of the coalescing filter element (4);
the oil collecting chamber (5) and the water outlet (6) are respectively arranged at the upper part and the lower part of the cylinder body (1) of the buoyancy separation zone (III).
18. -Oil-water separator according to claim 17, characterized in that it comprises a plurality of said coalescing filter elements (4); the number and the size of the holes on the tube plate are corresponding to the first end openings of the coalescing filter elements (4); the coalescing filter elements (4) are respectively arranged in parallel with the cylinder (1) in the axial direction at uniform intervals.
19. The oil-water separator according to claim 18, characterized in that the cylinder (1) is of a horizontal cylinder structure.
20. -Oil-water separator according to claim 18, characterized in that it further comprises a fluid distributor (3), said fluid distributor (3) being radially arranged along said cylinder (1) inside said water intake distribution zone (I) and close to said tube sheet; the edge of the fluid distributor (3) is in circumferential sealing connection with the side wall of the cylinder (1).
21. A method of oil-water separation employing the oil-water separator according to any one of claims 17 to 20, comprising the steps of:
Enabling oily wastewater to enter the oil-water separator through a water inlet of the cylinder (1); after passing through the water inlet distribution area (I), the water flows into the coalescing filter element (4) and sequentially flows through the porous central tube (8) of the coalescing filter element (4) and the coalescing material layer from inside to outside for oil-water separation treatment to obtain gathered floating oil and purified water;
collecting the collected floating oil from the oil collecting chamber (5) and collecting purified water from the water outlet (6).
22. The method of claim 21, further comprising: the flow pattern of the oily wastewater is maintained in a laminar flow state by controlling the amount of the oily wastewater entering so that the oily wastewater flows through the orifice of the porous central tube (8) of the coalescing filter element (4) and the coalescing material layer.
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| CN112221201B (en) * | 2020-09-11 | 2022-04-19 | 中国科学院理化技术研究所 | Oil-water separation pipe with hydrophobic and oleophylic surface and preparation method and application thereof |
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| CN106519753A (en) * | 2016-10-26 | 2017-03-22 | 华南理工大学 | Superhydrophobic coating based on metallic iron product and preparation method thereof |
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