CN109761311B - Reverse osmosis system applied to industrial strong brine sewage - Google Patents
Reverse osmosis system applied to industrial strong brine sewage Download PDFInfo
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- CN109761311B CN109761311B CN201811246589.8A CN201811246589A CN109761311B CN 109761311 B CN109761311 B CN 109761311B CN 201811246589 A CN201811246589 A CN 201811246589A CN 109761311 B CN109761311 B CN 109761311B
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- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 5
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Abstract
The invention discloses a reverse osmosis system applied to industrial concentrated salt sewage, which comprises a tank body, wherein two horizontal partition plates are oppositely arranged in the tank body, the tank body is divided into a raw water chamber, a primary reverse osmosis chamber and a secondary reverse osmosis chamber by the two horizontal partition plates, the raw water chamber, the primary reverse osmosis chamber and the secondary reverse osmosis chamber are communicated through pipelines, and at least one reverse osmosis device is arranged in the primary reverse osmosis chamber. Compared with the prior art, the invention improves the production efficiency by simultaneously working a plurality of reverse osmosis devices, reduces intermediate water pools and supercharging equipment, and realizes the reduction of cost and energy consumption; the reverse osmosis device drives the liquid in the liquid containing area to clean the reverse osmosis membrane through the ultrasonic vibration device and the aeration device, so that the reverse osmosis device is prevented from being blocked, the water yield of purified water is improved, and the energy consumption required by operation is reduced; the reverse osmosis membrane can effectively prevent charged ions from passing through and allow neutral water molecules to freely pass through, greatly improves the flux of the composite membrane under the condition that the salt rejection rate is basically kept unchanged, and has long service life.
Description
Technical Field
The invention relates to the technical field of wastewater treatment, in particular to a reverse osmosis system applied to industrial strong brine sewage.
Background
A large amount of wastewater with high salt content is generated in the industrial production of chemical industry, printing and dyeing, medicine, food and the like, and the emission of the wastewater can cause serious pollution to the environment. Therefore, how to treat high-salinity wastewater has become a hot point of research. Reverse osmosis, also known as reverse osmosis, is a membrane separation operation that uses a pressure differential as a driving force to separate a solvent from a solution. Reverse osmosis is known because it is in the opposite direction to natural osmosis. According to different osmotic pressures of various materials, a reverse osmosis pressure which is larger than the osmotic pressure, namely a reverse osmosis method, can be used for achieving the purposes of separation, extraction, purification and concentration. The most central component in the reverse osmosis technology is the reverse osmosis membrane, which is an artificial semipermeable membrane with certain characteristics and is made by simulating a biological semipermeable membrane and is the core component of the reverse osmosis technology. The principle of reverse osmosis is that under the action of the osmotic pressure higher than that of the solution, other substances are separated from water based on the fact that the substances cannot permeate a semipermeable membrane. The reverse osmosis membrane has a very small membrane pore size, and thus can effectively remove dissolved salts, colloids, microorganisms, organic substances, and the like in water.
The defects of the prior art are as follows: at present, in order to improve the recovery rate of wastewater of a system, the prior treatment method is to discharge concentrated water subjected to primary reverse osmosis treatment into a middle water tank or a middle water tank, pressurize the concentrated water by a high-pressure pump, perform secondary reverse osmosis treatment, and discharge the concentrated water and primary reverse osmosis produced water into a production water tank or a production water tank, so that the recovery rate of the disc-tube reverse osmosis system is improved, but the problems of high investment cost, high energy consumption and large occupied area exist; the reverse osmosis device can cause blockage when being used for a long time, the water yield of purified water is reduced, the greatly reduced working efficiency and energy consumption are high, meanwhile, salt ions in the wastewater can easily cause equipment corrosion and scaling, the treatment efficiency of the equipment is reduced, and the later maintenance cost of the equipment is increased; the existing reverse osmosis membrane for treating salt-containing wastewater comprises an inorganic molecular sieve membrane, an organic membrane and an organic/inorganic composite membrane. However, the inorganic molecular sieve membrane has small aperture, small water flux and low hydrophilicity, is not beneficial to dispersion, and has high preparation cost and complex preparation process; the hydrothermal stability of the organic membranes such as polyvinyl alcohol and the like for treating the high-salt-content wastewater is not high, the salt rejection rate and the permeation flux of the polyamide composite membrane are greatly improved, and the problems of high energy consumption, and poor pollution resistance and anti-scaling performance exist.
Disclosure of Invention
In order to solve the technical problems, the invention provides a reverse osmosis system applied to industrial strong brine sewage, which solves the problems of high investment cost, high energy consumption and larger occupied area of the existing reverse osmosis treatment system; the reverse osmosis device is easy to block, the maintenance cost is high, the operation energy consumption is high, the hydrothermal stability of the organic membrane is not high, the salt rejection rate and flux are lower, the water flux of the inorganic membrane is small, the preparation process is complex and the like.
The technical scheme adopted by the invention is as follows:
the utility model provides a reverse osmosis system for industry strong brine sewage, the key lies in: the device comprises a tank body, wherein two horizontal partition plates are oppositely arranged in the tank body, the tank body is divided into a raw water chamber, a primary reverse osmosis chamber and a secondary reverse osmosis chamber by the two horizontal partition plates, the raw water chamber, the primary reverse osmosis chamber and the secondary reverse osmosis chamber are communicated through pipelines, and at least one reverse osmosis device is arranged in the primary reverse osmosis chamber;
the reverse osmosis device comprises an upper mounting seat and a lower mounting seat which are arranged oppositely, a reverse osmosis membrane is arranged between the upper mounting seat and the lower mounting seat, a liquid containing area is enclosed among the upper mounting seat, the lower mounting seat and the reverse osmosis membrane, the liquid containing area is vertically provided with a filter cylinder which divides the liquid containing area into an outer infiltration area and an inner infiltration area, a cleaning component is arranged in the outer infiltration area, a liquid inlet is arranged on the upper mounting seat and is communicated with the raw water chamber through a first liquid conveying pipe, the lower mounting seat is provided with a concentrated water outlet and a waste residue outlet, the concentrated water outlet is communicated with the secondary reverse osmosis chamber through a second liquid conveying pipe, the liquid inlet and the waste residue outlet are both positioned in the outer osmosis area, the concentrated water outlet is positioned in the inner infiltration area, and the first infusion tube and the second infusion tube are respectively provided with a high-pressure pump and a booster pump;
the reverse osmosis membrane is prepared from the following components in percentage by mass of 1: (0.6-1.3) self-assembly of polyquaternium cationic PVA and polysulfonic group substituted anion PVA to form self-assembly PVA base film and aminated mesoporous SiO2Is prepared by interfacial polymerization.
Preferably, the substitution degree of the polyquaternium cationic PVA is 2.5-7; the degree of substitution of the polysulfonic group-substituted anionic PVA is 2.5-4.
Preferably, the polyquaternium cationic PVA is obtained by the following method: dropwise adding a KOH solution with the mass concentration of 5-10mol/L into a PVA aqueous solution to be alkalized, and then adding (3-chloro-2-hydroxymethyl) trimethyl ammonium chloride, wherein the mass-volume ratio of the (3-chloro-2-hydroxymethyl) trimethyl ammonium chloride to the KOH solution to the PVA aqueous solution is (0.5-5) g: (1-10) ml: 100ml, stirring and reacting for 1-3h at 60-85 ℃, adding 95% ethanol by mass fraction after the reaction is finished, separating out precipitate, and separating, washing and drying the precipitate to obtain the polyquaternium cationic PVA.
Preferably, the polysulfonate-substituted anionic PVA is obtained by the following method: stirring and dropwise adding concentrated sulfuric acid into a PVA aqueous solution, stirring and reacting for 1-3h at 60-85 ℃, adding 95% ethanol by mass after the reaction is finished, separating out a precipitate, separating, washing to be neutral, and drying the precipitate to obtain the polysulfonyl group-substituted anion PVA.
Preferably, the mesoporous SiO is aminated2The method comprises the following steps: adding sodium hydroxide solution with mass concentration of 2-4.5mol/L and absolute ethyl alcohol into CTAB aqueous solution with mass fraction of 0.005-0.01mol/L, violently stirring at 60-85 ℃ to obtain premixed solution, and then mixing the premixed solution with the water according to the molar ratio of 1: (0.05-0.3) stirring tetraethyl orthosilicate and 3-aminopropyltriethoxysilane, adding into the premixed solution, continuing to stir vigorously for reaction for 1-3h, after the reaction is finished, filtering, separating, washing and drying the reactant in vacuum to obtain SiO2Precursor, then SiO2The input volume ratio of the precursor is (5-8): 1, carrying out reflux reaction for 4-7h in a water bath at 65-80 ℃, filtering, separating, washing and vacuum drying the reactant to obtain the aminated mesoporous SiO2。
Preferably, be equipped with reverse osmosis membrane in the secondary reverse osmosis room, reverse osmosis membrane will secondary reverse osmosis room separates into second infiltration district and second clean liquid district, dense water export with second infiltration district passes through second transfer line pipeline intercommunication, second clean liquid district with primary reverse osmosis room passes through the clean water pipe intercommunication, be equipped with the three-way valve on the clean water pipe.
Preferably, the cleaning assembly comprises an ultrasonic vibration device and an aeration device, the ultrasonic vibration device is arranged on the upper mounting seat, and the aeration device is arranged close to the lower mounting seat; the aeration device comprises an annular air pipe, the annular air pipe surrounds the filter cylinder in a circle, at least one aerator is arranged on the annular air pipe, and the annular air pipe is connected with a fan.
Preferably, go up all to be equipped with membrane fixed subassembly on mount pad and the lower mount pad, membrane fixed subassembly includes annular mount pad, two annular mount pad respectively with the lower surface of going up the mount pad and the last fixed surface of mount pad down are connected, two be equipped with raw water diversion net between the annular mount pad and see through the water course net, the annular fixed slot has vertically been seted up on the annular mount pad, raw water diversion net with see through the upper and lower border of water course net respectively with the tank bottom fixed connection of annular fixed slot, the reverse osmosis membrane laminating is in raw water diversion net and see through between the water course net.
Preferably, the raw water diversion net is arranged close to the filter cylinder, the permeable water channel net is arranged far away from the filter cylinder, and the aperture of the raw water diversion net is smaller than that of the permeable water channel net.
Preferably, the filter cylinder is a stainless steel filter screen, the upper end and the lower end of the filter cylinder are respectively and fixedly connected with the lower surface of the upper mounting seat and the upper surface of the lower mounting seat, and the aperture of the stainless steel filter screen is smaller than 100 μm.
Has the advantages that: compared with the prior art, the reverse osmosis system applied to the industrial strong brine sewage provided by the invention has the advantages that the multiple reverse osmosis devices work simultaneously, so that the production efficiency is improved, the intermediate water tank and the supercharging equipment are reduced, and the purposes of reducing the investment cost, reducing the energy consumption and reducing the occupied area are realized;
the reverse osmosis device has large water flux, less scale and difficult blockage, and the ultrasonic vibration device and the aeration device drive the liquid in the liquid containing area to gradually clean the reverse osmosis membrane, so that the blockage of the reverse osmosis device is prevented, the water yield of purified water is effectively improved, and the energy consumption required by operation is greatly reduced; the washed insoluble matters are isolated outside the filter cylinder, are deposited in an outer permeation area and then are discharged from a waste residue outlet, and the concentrated water enters an inner permeation area through the filter cylinder and then enters a secondary reverse osmosis chamber through a concentrated water outlet, so that the pollution of suspended matters to the concentrated water is prevented;
the polyanion and polycation of the self-assembled PVA-based membrane of the reverse osmosis membrane approach each other due to electrostatic attraction to form a strong-polarity ion pair which can divide substances with strong polarity in a separation systemThe PVA base film has strong adsorption capacity, is beneficial to separating liquid mixtures with different polarities, improves the compactness of the PVA base film by crosslinking cation and anion pairs into a website structure, and has the advantages of sparser website structure, easy passage of polar molecules, large permeation flux and contribution to the implementation of a pervaporation process because the charge density is lower; because the polyanion and the polycation are water-soluble, the polyion compound precipitation can not be generated after the mixing, the film can be formed by adopting a one-time coating method, and the thickness of the film and the reaction degree of the polyion compound are easy to control; aminated mesoporous SiO2Mesoporous SiO of2The inner and outer surfaces of the particles contain a large amount of hydroxyl, the hydrophilic property of the membrane is increased by doping the hydroxyl into the base membrane, water molecules can pass preferentially, the water flux can be improved to a large extent under the condition of keeping high salt rejection rate, hydrophilic amino is introduced, the hydrophilic amino can be firmly combined with the base membrane by chemical bonds after reacting with groups in the base membrane, the stability of the composite membrane and the safety and purity of a separation system are ensured, and the service life of the composite membrane is prolonged.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a schematic structural diagram of a reverse osmosis device d in FIG. 1;
fig. 3 is a sectional view a-a of fig. 2.
Detailed Description
In order to make the technical solution of the present invention better understood by those skilled in the art, the present invention will be described in detail below with reference to the accompanying tables and specific embodiments.
Example 1 reverse osmosis System I applied to Industrial concentrated salt wastewater
As shown in fig. 1 to 3, a reverse osmosis system applied to industrial concentrated salt wastewater comprises a tank body a, wherein two horizontal partition plates are oppositely arranged in the tank body a, the tank body a is divided into a raw water chamber a1, a primary reverse osmosis chamber a2 and a secondary reverse osmosis chamber by the two horizontal partition plates, the raw water chamber a1, the primary reverse osmosis chamber a2 and the secondary reverse osmosis chamber are communicated through pipelines, at least one reverse osmosis device d is arranged in the primary reverse osmosis chamber a2, a reverse osmosis membrane I is arranged in the secondary reverse osmosis chamber, and the secondary reverse osmosis chamber is divided into a second osmosis area a31 and a second purified liquid area a32 by the reverse osmosis membrane I;
as can be seen from fig. 2 and 3, the reverse osmosis device d includes an upper mounting seat 1 and a lower mounting seat 2 which are oppositely arranged, a reverse osmosis membrane I is arranged between the upper mounting seat 1 and the lower mounting seat 2, a liquid containing area is defined between the upper mounting seat 1, the lower mounting seat 2 and the reverse osmosis membrane I, a vertically arranged filter cartridge 4 is arranged in the liquid containing area, the filter cartridge 4 is a stainless steel filter screen, the upper end and the lower end of the filter cartridge 4 are respectively fixedly connected with the lower surface of the upper mounting seat 1 and the upper surface of the lower mounting seat 2, the aperture of the stainless steel filter screen is smaller than 100 μm, the filter cartridge 4 divides the liquid containing area into an outer permeable area b and an inner permeable area c, a cleaning assembly is arranged in the outer permeable area b, a liquid inlet 7 is arranged on the upper mounting seat 1, and the liquid inlet 7 is communicated with the raw water chamber a1 through a first liquid transport tube f, a concentrated water outlet 8 and a waste residue outlet 6 are formed in the lower mounting seat 2, the concentrated water outlet 8 is communicated with the second osmosis area a31 through a second infusion tube g, the second liquid purification area a32 is communicated with the primary reverse osmosis chamber a2 through a purified water tube h, a three-way valve is arranged on the purified water tube h, the liquid inlet 7 and the waste residue outlet 6 are both located in the outer osmosis area b, the concentrated water outlet 8 is located in the inner osmosis area c, and a high-pressure pump and a pressure pump are respectively arranged on the first infusion tube f and the second infusion tube g;
as can be seen in fig. 2, the upper mount 1 and the lower mount 2 are each provided with a membrane fixing assembly 9, the membrane fixing component 9 comprises annular mounting seats 91, two annular mounting seats 91 are respectively and fixedly connected with the lower surface of the upper mounting seat 1 and the upper surface of the lower mounting seat 2, a raw water guide net 92 and a permeable water channel net 93 are arranged between the two annular mounting seats 91, the raw water guide net 92 is disposed close to the filter cartridge 4, the permeated water passage net 93 is disposed far from the filter cartridge 4, and the aperture of the raw water diversion net 92 is smaller than that of the permeated water channel net 93, an annular fixing groove is vertically arranged on the annular mounting seat 91, the upper edge and the lower edge of the raw water diversion net 92 and the upper edge and the lower edge of the permeable water channel net 93 are respectively fixedly connected with the groove bottom of the annular fixing groove, and the reverse osmosis membrane is attached between the raw water diversion net 92 and the permeable water channel net 93;
as can be seen in fig. 3, the aeration device 52 comprises an annular air pipe 521, the annular air pipe 521 is arranged around the filter cartridge 4, at least one aerator 522 is arranged on the annular air pipe 521, and a fan is connected to the annular air pipe 521.
The reverse osmosis membrane I is prepared by adopting the following method:
step one, preparing polyquaternium cationic PVA: dropwise adding a KOH solution with the mass concentration of 5mol/L into a PVA aqueous solution to be alkalized, and then adding (3-chloro-2-hydroxymethyl) trimethyl ammonium chloride, wherein the mass-volume ratio of the (3-chloro-2-hydroxymethyl) trimethyl ammonium chloride to the KOH solution to the PVA aqueous solution is 0.5 g: 1 ml: 100ml, stirring and reacting for 1-3h at 60-85 ℃, adding 95% ethanol by mass fraction after the reaction is finished, separating out precipitate, separating, washing and drying the precipitate to obtain polyquaternium cationic PVA with the degree of substitution of 2.5;
preparation of polysulfonate-substituted anionic PVA: stirring and dropwise adding concentrated sulfuric acid into the PVA aqueous solution, wherein the mass-to-volume ratio of the concentrated sulfuric acid to the PVA aqueous solution is 0.2 g: 100ml, stirring and reacting for 1-3h at 60-85 ℃, adding 95% ethanol by mass fraction after the reaction is finished, separating out precipitate, separating, washing to be neutral, and drying the precipitate to obtain the polysulfonate-substituted anion PVA with the substitution degree of 2.5;
aminated mesoporous SiO2The preparation of (1): adding a sodium hydroxide solution with the mass concentration of 2mol/L and absolute ethyl alcohol into a CTAB aqueous solution with the mass fraction of 0.005mol/L, violently stirring at 60-85 ℃ to obtain a premixed solution, and then mixing the premixed solution with a water-soluble polymer in a molar ratio of 1: stirring 0.05 tetraethyl orthosilicate and 3-aminopropyltriethoxysilane, adding into the premixed solution, continuously and violently stirring for reacting for 1-3h, and after the reaction is finished, filtering, separating, washing and vacuum drying the reactant to obtain SiO2Precursor, then SiO2The input volume ratio of the precursor is 5: 1, carrying out reflux reaction for 4-7h in a water bath at 65-80 ℃, filtering, separating, washing and vacuum drying the reactant to obtain the aminated mesoporous SiO2；
Step two, dissolving the polyquaternium cationic PVA prepared in the step one in water to obtain a PVA cationic solution with the mass fraction of 5% wt, dissolving the polysulfonate group substituted anion PVA prepared in the step one in water to obtain a PVA anionic solution with the mass fraction of 5% wt, and mixing the components in a mass ratio of 1: mixing 0.6 of PVA cationic solution and PVA anionic solution, stirring uniformly, adjusting the pH value to 7, standing for 24 hours at room temperature for defoaming treatment to obtain a PVA-based membrane casting solution, scraping the membrane casting solution on a polytetrafluoroethylene plate, and air-drying to obtain a self-assembled PVA-based membrane;
step three, aminated mesoporous SiO prepared in step one2Placing the mixture into a normal hexane solution of trimesoyl chloride with the mass fraction of 0.2 percent by weight, wherein the mesoporous SiO is aminated2And the mass volume ratio of the n-hexane solution of trimesoyl chloride is 0.01 g: 100ml, and obtaining the aminated mesoporous SiO by the action of ultrasonic wave for 50min with the ultrasonic power of 150W2And (3) sol.
Step four, adding triethylamine and dilute hydrochloric acid into deionized water, adjusting the pH value to 8, then adding m-phenylenediamine to prepare a m-phenylenediamine aqueous solution with the mass fraction of 0.5 wt%, uniformly coating the m-phenylenediamine aqueous solution on the self-assembled PVA base film prepared in the step two to reach saturation to form a pre-polymerization layer, and then uniformly coating the aminated mesoporous SiO prepared in the step three2And coating the sol on the pre-polymerization layer, performing interfacial polymerization reaction, and finally performing heat treatment at 100 ℃ to obtain the PVA-based polyion composite membrane I.
And (3) testing results: the water recovery rate of the reverse osmosis system is more than 70 percent, and the desalination rate is more than or equal to 98 percent within 1 year.
As shown in fig. 1 to 3, a reverse osmosis system applied to industrial concentrated salt wastewater comprises a tank body a, wherein two horizontal partition plates are oppositely arranged in the tank body a, the tank body a is divided into a raw water chamber a1, a primary reverse osmosis chamber a2 and a secondary reverse osmosis chamber by the two horizontal partition plates, the raw water chamber a1, the primary reverse osmosis chamber a2 and the secondary reverse osmosis chamber are communicated through pipelines, at least one reverse osmosis device d is arranged in the primary reverse osmosis chamber a2, a reverse osmosis membrane II is arranged in the secondary reverse osmosis chamber, and the secondary reverse osmosis chamber is divided into a second osmosis area a31 and a second purified liquid area a32 by the reverse osmosis membrane II;
as can be seen from fig. 2 and 3, the reverse osmosis device d includes an upper mounting seat 1 and a lower mounting seat 2 which are oppositely arranged, a reverse osmosis membrane II is arranged between the upper mounting seat 1 and the lower mounting seat 2, a liquid containing area is defined between the upper mounting seat 1, the lower mounting seat 2 and the reverse osmosis membrane II, a vertically arranged filter cartridge 4 is arranged in the liquid containing area, the filter cartridge 4 is a stainless steel filter screen, the upper end and the lower end of the filter cartridge 4 are respectively fixedly connected with the lower surface of the upper mounting seat 1 and the upper surface of the lower mounting seat 2, the aperture of the stainless steel filter screen is smaller than 100 μm, the filter cartridge 4 divides the liquid containing area into an outer permeable area b and an inner permeable area c, a cleaning assembly is arranged in the outer permeable area b, a liquid inlet 7 is arranged on the upper mounting seat 1, and the liquid inlet 7 is communicated with the raw water chamber a1 through a first liquid transport tube f, a concentrated water outlet 8 and a waste residue outlet 6 are formed in the lower mounting seat 2, the concentrated water outlet 8 is communicated with the second osmosis area a31 through a second infusion tube g, the second liquid purification area a32 is communicated with the primary reverse osmosis chamber a2 through a purified water tube h, a three-way valve is arranged on the purified water tube h, the liquid inlet 7 and the waste residue outlet 6 are both located in the outer osmosis area b, the concentrated water outlet 8 is located in the inner osmosis area c, and a high-pressure pump and a pressure pump are respectively arranged on the first infusion tube f and the second infusion tube g;
as can be seen in fig. 2, the upper mount 1 and the lower mount 2 are each provided with a membrane fixing assembly 9, the membrane fixing component 9 comprises annular mounting seats 91, two annular mounting seats 91 are respectively and fixedly connected with the lower surface of the upper mounting seat 1 and the upper surface of the lower mounting seat 2, a raw water guide net 92 and a permeable water channel net 93 are arranged between the two annular mounting seats 91, the raw water guide net 92 is disposed close to the filter cartridge 4, the permeated water passage net 93 is disposed far from the filter cartridge 4, and the aperture of the raw water diversion net 92 is smaller than that of the permeated water channel net 93, an annular fixing groove is vertically arranged on the annular mounting seat 91, the upper edge and the lower edge of the raw water diversion net 92 and the upper edge and the lower edge of the permeable water channel net 93 are respectively fixedly connected with the groove bottom of the annular fixing groove, and the reverse osmosis membrane is attached between the raw water diversion net 92 and the permeable water channel net 93;
as can be seen in fig. 3, the aeration device 52 comprises an annular air pipe 521, the annular air pipe 521 is arranged around the filter cartridge 4, at least one aerator 522 is arranged on the annular air pipe 521, and a fan is connected to the annular air pipe 521.
The reverse osmosis membrane II is prepared by adopting the following method:
step one, preparing polyquaternium cationic PVA: dropwise adding a KOH solution with the mass concentration of 10mol/L into a PVA aqueous solution to be alkalized, and then adding (3-chloro-2-hydroxymethyl) trimethyl ammonium chloride, wherein the mass-volume ratio of the (3-chloro-2-hydroxymethyl) trimethyl ammonium chloride to the KOH solution to the PVA aqueous solution is 5 g: 10 ml: 100ml, stirring and reacting for 1-3h at 60-85 ℃, adding 95% ethanol by mass fraction after the reaction is finished, separating out precipitate, separating, washing and drying the precipitate to obtain polyquaternium cationic PVA with the degree of substitution of 7;
preparation of polysulfonate-substituted anionic PVA: stirring and dropwise adding concentrated sulfuric acid into a PVA aqueous solution, wherein the mass-to-volume ratio of the concentrated sulfuric acid to the PVA aqueous solution is 3 g: 100ml, stirring and reacting for 1-3h at 60-85 ℃, adding 95% ethanol by mass fraction after the reaction is finished, separating out precipitate, separating, washing to be neutral, and drying the precipitate to obtain the polysulfonate-substituted anion PVA with the degree of substitution of 4;
aminated mesoporous SiO2The preparation of (1): adding sodium hydroxide solution with mass concentration of 4.5mol/L and absolute ethyl alcohol into CTAB aqueous solution with mass fraction of 0.01mol/L, violently stirring at 60-85 ℃ to obtain premixed liquid, and then mixing the premixed liquid with the water according to a molar ratio of 1: 0.3 of tetraethyl orthosilicate and 3-aminopropyltriethoxysilane are stirred and put into the premixed solution, the mixture is stirred vigorously and reacts for 1 to 3 hours, and after the reaction is finished, the reactant is filtered, separated, washed and dried in vacuum to obtain SiO2Precursor, then SiO2The input volume ratio of the precursor is 8: 1, carrying out reflux reaction for 4-7h in a water bath at 65-80 ℃, filtering, separating, washing and vacuum drying the reactant to obtain the aminated mesoporous SiO2；
Step two, dissolving the polyquaternium cationic PVA prepared in the step one in water to obtain a PVA cationic solution with the mass fraction of 10% wt, dissolving the polysulfonate group substituted anion PVA prepared in the step one in water to obtain a PVA anionic solution with the mass fraction of 10% wt, and mixing the PVA anionic solution and the PVA cationic solution in a mass ratio of 1: 1.3, mixing the PVA cationic solution and the PVA anionic solution, uniformly stirring, adjusting the pH value to 7, standing for 24 hours at room temperature for defoaming treatment to obtain a PVA-based membrane casting solution, scraping the membrane casting solution on a polytetrafluoroethylene plate, and air-drying to obtain a self-assembled PVA-based membrane;
step three, aminated mesoporous SiO prepared in step one2Placing the mixture into a normal hexane solution of trimesoyl chloride with the mass fraction of 1 percent by weight, wherein the mesoporous SiO is aminated2And the mass volume ratio of the n-hexane solution of trimesoyl chloride is 0.07 g: 100ml, and obtaining the aminated mesoporous SiO by the action of ultrasonic waves for 100min with the ultrasonic power of 150W2And (3) sol.
Step four, adding triethylamine and dilute hydrochloric acid into deionized water, adjusting the pH value to 8, then adding m-phenylenediamine to prepare a 5 wt% m-phenylenediamine aqueous solution, uniformly coating the m-phenylenediamine aqueous solution on the self-assembled PVA base film prepared in the step two to reach saturation to form a pre-polymerization layer, and then uniformly coating the aminated mesoporous SiO prepared in the step three on the self-assembled PVA base film to form a pre-polymerization layer2And coating the sol on the pre-polymerization layer, performing interfacial polymerization reaction, and finally performing heat treatment at 150 ℃ to obtain the PVA-based polyion composite membrane II.
And (3) testing results: the water recovery rate of the reverse osmosis system is more than 75.5 percent, and the desalination rate is more than or equal to 96.4 percent within 1 year.
Embodiment 3 reverse osmosis system II applied to industrial concentrated salt sewage
As shown in fig. 1 to 3, a reverse osmosis system applied to industrial concentrated salt wastewater comprises a tank body a, wherein two horizontal partition plates are oppositely arranged in the tank body a, the tank body a is divided into a raw water chamber a1, a primary reverse osmosis chamber a2 and a secondary reverse osmosis chamber by the two horizontal partition plates, the raw water chamber a1, the primary reverse osmosis chamber a2 and the secondary reverse osmosis chamber are communicated through pipelines, at least one reverse osmosis device d is arranged in the primary reverse osmosis chamber a2, a reverse osmosis membrane III is arranged in the secondary reverse osmosis chamber, and the secondary reverse osmosis chamber is divided into a second osmosis area a31 and a second purified liquid area a32 by the reverse osmosis membrane III;
as can be seen from fig. 2 and 3, the reverse osmosis device d includes an upper mounting seat 1 and a lower mounting seat 2 which are oppositely arranged, a reverse osmosis membrane III is arranged between the upper mounting seat 1 and the lower mounting seat 2, a liquid containing area is defined between the upper mounting seat 1, the lower mounting seat 2 and the reverse osmosis membrane III, a vertically arranged filter cartridge 4 is arranged in the liquid containing area, the filter cartridge 4 is a stainless steel filter screen, the upper end and the lower end of the filter cartridge 4 are respectively fixedly connected with the lower surface of the upper mounting seat 1 and the upper surface of the lower mounting seat 2, the aperture of the stainless steel filter screen is smaller than 100 μm, the filter cartridge 4 divides the liquid containing area into an outer permeable area b and an inner permeable area c, a cleaning assembly is arranged in the outer permeable area b, a liquid inlet 7 is arranged on the upper mounting seat 1, and the liquid inlet 7 is communicated with the raw water chamber a1 through a first liquid transport tube f, a concentrated water outlet 8 and a waste residue outlet 6 are formed in the lower mounting seat 2, the concentrated water outlet 8 is communicated with the second osmosis area a31 through a second infusion tube g, the second liquid purification area a32 is communicated with the primary reverse osmosis chamber a2 through a purified water tube h, a three-way valve is arranged on the purified water tube h, the liquid inlet 7 and the waste residue outlet 6 are both located in the outer osmosis area b, the concentrated water outlet 8 is located in the inner osmosis area c, and a high-pressure pump and a pressure pump are respectively arranged on the first infusion tube f and the second infusion tube g;
as can be seen in fig. 2, the upper mount 1 and the lower mount 2 are each provided with a membrane fixing assembly 9, the membrane fixing component 9 comprises annular mounting seats 91, two annular mounting seats 91 are respectively and fixedly connected with the lower surface of the upper mounting seat 1 and the upper surface of the lower mounting seat 2, a raw water guide net 92 and a permeable water channel net 93 are arranged between the two annular mounting seats 91, the raw water guide net 92 is disposed close to the filter cartridge 4, the permeated water passage net 93 is disposed far from the filter cartridge 4, and the aperture of the raw water diversion net 92 is smaller than that of the permeated water channel net 93, an annular fixing groove is vertically arranged on the annular mounting seat 91, the upper edge and the lower edge of the raw water diversion net 92 and the upper edge and the lower edge of the permeable water channel net 93 are respectively fixedly connected with the groove bottom of the annular fixing groove, and the reverse osmosis membrane is attached between the raw water diversion net 92 and the permeable water channel net 93;
as can be seen in fig. 3, the aeration device 52 comprises an annular air pipe 521, the annular air pipe 521 is arranged around the filter cartridge 4, at least one aerator 522 is arranged on the annular air pipe 521, and a fan is connected to the annular air pipe 521.
The reverse osmosis membrane III is prepared by adopting the following method:
step one, preparing polyquaternium cationic PVA: dropwise adding a KOH solution with the mass concentration of 6.5mol/L into a PVA aqueous solution to be alkalized, and then adding (3-chloro-2-hydroxymethyl) trimethyl ammonium chloride, wherein the mass-volume ratio of the (3-chloro-2-hydroxymethyl) trimethyl ammonium chloride to the KOH solution to the PVA aqueous solution is 1.5 g: 4 ml: 100ml, stirring and reacting for 1-3h at 60-85 ℃, adding 95% ethanol by mass fraction after the reaction is finished, separating out precipitate, separating, washing and drying the precipitate to obtain polyquaternium cationic PVA with the degree of substitution of 3.5;
preparation of polysulfonate-substituted anionic PVA: stirring and dropwise adding concentrated sulfuric acid into the PVA aqueous solution, wherein the mass-to-volume ratio of the concentrated sulfuric acid to the PVA aqueous solution is 1.5 g: 100ml, stirring and reacting for 1-3h at 60-85 ℃, adding 95% ethanol by mass fraction after the reaction is finished, separating out precipitate, separating, washing to be neutral, and drying the precipitate to obtain the polysulfonate-substituted anion PVA with the substitution degree of 3.5;
aminated mesoporous SiO2The preparation of (1): adding sodium hydroxide solution with mass concentration of 2-4.5mol/L and absolute ethyl alcohol into CTAB aqueous solution with mass fraction of 0.0075mol/L, violently stirring at 60-85 ℃ to obtain premixed solution, and then mixing the premixed solution with a molar ratio of 1: 0.18 of tetraethyl orthosilicate and 3-aminopropyltriethoxysilane are stirred and put into the premixed solution, the mixture is stirred vigorously and reacts for 1 to 3 hours, and after the reaction is finished, the reactant is filtered, separated, washed and dried in vacuum to obtain SiO2Precursor, then SiO2The input volume ratio of the precursor is 5.5: 1, refluxing and reacting for 4-7h in a water bath at 65-80 ℃, filtering, separating and washing reactantsWashing and vacuum drying to obtain the aminated mesoporous SiO 2;
step two, dissolving the polyquaternium cationic PVA prepared in the step one in water to obtain a PVA cationic solution with the mass fraction of 7 wt%, dissolving the polysulfonate group substituted anion PVA prepared in the step one in water to obtain a PVA anionic solution with the mass fraction of 7 wt%, and mixing the components in a mass ratio of 1: 1, mixing the PVA cationic solution and the PVA anionic solution, uniformly stirring, adjusting the pH value to 7, standing for 24 hours at room temperature for defoaming treatment to obtain a PVA-based membrane casting solution, scraping the membrane casting solution on a polytetrafluoroethylene plate, and air-drying to obtain a self-assembled PVA-based membrane;
step three, aminated mesoporous SiO prepared in step one2Placing the mixture into a normal hexane solution of trimesoyl chloride with the mass fraction of 0.6 percent by weight, wherein the mesoporous SiO is aminated2And the mass volume ratio of the n-hexane solution of trimesoyl chloride is 0.1 g: 100ml, and obtaining the aminated mesoporous SiO by ultrasonic action for 60min with the ultrasonic power of 150W2Sol;
step four, adding triethylamine and dilute hydrochloric acid into deionized water, adjusting the pH value to 8, then adding m-phenylenediamine to prepare a m-phenylenediamine aqueous solution with the mass fraction of 0.6 wt%, uniformly coating the m-phenylenediamine aqueous solution on the self-assembled PVA base film prepared in the step two to reach saturation to form a pre-polymerization layer, and then uniformly coating the aminated mesoporous SiO prepared in the step three2And coating the sol on the pre-polymerization layer, performing interfacial polymerization reaction, and finally performing heat treatment at 120 ℃ to obtain the PVA-based polyion composite membrane III.
And (3) testing results: the water recovery rate of the reverse osmosis system is more than 81.7 percent, and the desalination rate is more than or equal to 95.4 percent within 1 year.
Finally, it should be noted that the above-mentioned description is only a preferred embodiment of the present invention, and those skilled in the art can make various similar representations without departing from the spirit and scope of the present invention.
Claims (10)
1. The utility model provides a reverse osmosis system for industry strong brine sewage which characterized in that: the device comprises a tank body (a), wherein two horizontal partition plates are oppositely arranged in the tank body (a), the tank body (a) is divided into a raw water chamber (a1), a primary reverse osmosis chamber (a2) and a secondary reverse osmosis chamber by the two horizontal partition plates, the raw water chamber (a1), the primary reverse osmosis chamber (a2) and the secondary reverse osmosis chamber are communicated through pipelines, and at least one reverse osmosis device (d) is arranged in the primary reverse osmosis chamber (a 2);
the reverse osmosis device (d) comprises an upper mounting seat (1) and a lower mounting seat (2) which are opposite to each other, a reverse osmosis membrane is arranged between the upper mounting seat (1) and the lower mounting seat (2), a liquid containing area is defined among the upper mounting seat (1), the lower mounting seat (2) and the reverse osmosis membrane, a filter cartridge (4) is vertically arranged in the liquid containing area, the liquid containing area is divided into an outer osmosis area (b) and an inner osmosis area (c) by the filter cartridge (4), a cleaning component is arranged in the outer osmosis area (b), a liquid inlet (7) is formed in the upper mounting seat (1), the liquid inlet (7) is communicated with the raw water chamber (a1) through a first liquid conveying pipe (f), a concentrated water outlet (8) and a waste residue outlet (6) are formed in the lower mounting seat (2), and the concentrated water outlet (8) is communicated with the reverse osmosis secondary chamber through a second liquid conveying pipe (g), the liquid inlet (7) and the waste residue outlet (6) are both positioned in the outer penetration zone (b), the concentrated water outlet (8) is positioned in the inner penetration zone (c), and the first infusion tube (f) and the second infusion tube (g) are respectively provided with a high-pressure pump and a booster pump;
the reverse osmosis membrane is prepared from the following components in percentage by mass of 1: (0.6-1.3) self-assembly of polyquaternium cationic PVA and polysulfonic group substituted anion PVA to form self-assembly PVA base film and aminated mesoporous SiO2The polymer is prepared by interfacial polymerization, and the polymerization process specifically comprises the following steps: adding triethylamine and dilute hydrochloric acid into deionized water, adjusting the pH value to 8, then adding m-phenylenediamine to prepare m-phenylenediamine aqueous solution, uniformly coating the self-assembled PVA base film with the m-phenylenediamine aqueous solution to saturation to form a pre-polymerization layer, then coating aminated mesoporous SiO2 sol on the pre-polymerization layer, carrying out interfacial polymerization reaction, and finally carrying out heat treatment.
2. The reverse osmosis system applied to industrial concentrated salt wastewater according to claim 1, wherein: the substitution degree of the polyquaternium cationic PVA is 2.5-7; the degree of substitution of the polysulfonic group-substituted anionic PVA is 2.5-4.
3. A reverse osmosis system applied to industrial concentrated salt wastewater according to claim 1 or 2, wherein the polyquaternium cationic PVA is obtained by the following method: dropwise adding a KOH solution with the mass concentration of 5-10mol/L into a PVA aqueous solution to be alkalized, and then adding (3-chloro-2-hydroxymethyl) trimethyl ammonium chloride, wherein the mass-volume ratio of the (3-chloro-2-hydroxymethyl) trimethyl ammonium chloride to the KOH solution to the PVA aqueous solution is (0.5-5) g: (1-10) ml: 100ml, stirring and reacting for 1-3h at 60-85 ℃, adding 95% ethanol by mass fraction after the reaction is finished, separating out precipitate, and separating, washing and drying the precipitate to obtain the polyquaternium cationic PVA.
4. The reverse osmosis system applied to industrial concentrated salt wastewater according to claim 3, wherein the polysulfonate-substituted anion PVA is obtained by the following method: stirring and dropwise adding concentrated sulfuric acid into the PVA aqueous solution, wherein the mass-to-volume ratio of the concentrated sulfuric acid to the PVA aqueous solution is (0.2-3) g: 100ml, stirring and reacting for 1-3h at 60-85 ℃, adding 95% ethanol by mass fraction after the reaction is finished, separating out precipitate, separating the precipitate, washing to be neutral, and drying to obtain the polysulfonyl radical substituted anion PVA.
5. A reverse osmosis system applied to industrial concentrated salt wastewater according to claim 1 or 4, wherein the SiO is aminated to form mesoporous SiO2The method comprises the following steps: adding sodium hydroxide solution with mass concentration of 2-4.5mol/L and absolute ethyl alcohol into CTAB aqueous solution with mass fraction of 0.005-0.01mol/L, violently stirring at 60-85 ℃ to obtain premixed solution, and then mixing the premixed solution with the water according to the molar ratio of 1: (0.05-0.3) stirring tetraethyl orthosilicate and 3-aminopropyltriethoxysilane, adding into the premixed solution, continuing to stir vigorously for reaction for 1-3h, after the reaction is finished, filtering, separating, washing and drying the reactant in vacuum to obtain SiO2Precursor, then SiO2The input volume ratio of the precursor is (5-8): 1 Anhydrous ethanol and concentrated saltIn the acid mixed solution, carrying out reflux reaction for 4-7h at the temperature of 65-80 ℃ in a water bath, filtering, separating, washing and vacuum drying the reactant to obtain the aminated mesoporous SiO2。
6. The reverse osmosis system applied to industrial concentrated salt wastewater according to claim 5, wherein the reverse osmosis system comprises: be equipped with reverse osmosis membrane in the secondary reverse osmosis room, reverse osmosis membrane will secondary reverse osmosis room separates into second infiltration district (a31) and second clean liquid district (a32), dense water export (8) with second infiltration district (a31) passes through second transfer line (g) pipeline intercommunication, second clean liquid district (a32) with first reverse osmosis room (a2) passes through water purification pipe (h) intercommunication, be equipped with the three-way valve on water purification pipe (h).
7. A reverse osmosis system applied to industrial concentrated salt wastewater according to claim 1 or 6, wherein the reverse osmosis system comprises: the cleaning assembly comprises an ultrasonic vibration device (51) and an aeration device (52), the ultrasonic vibration device (51) is arranged on the upper mounting seat (1), and the aeration device (52) is arranged close to the lower mounting seat (2); aeration equipment (52) include annular air pipe (521), annular air pipe (521) center on strain a section of cloth (4) and set up, be equipped with at least one aerator (522) on annular air pipe (521), annular air pipe (521) are connected with the fan.
8. The reverse osmosis system applied to industrial concentrated salt wastewater according to claim 7, wherein the reverse osmosis system comprises: go up mount pad (1) and all be equipped with membrane fixed subassembly (9) down on mount pad (2), membrane fixed subassembly (9) include annular mount pad (91), two annular mount pad (91) respectively with go up the lower surface of mount pad (1) and the last fixed surface of lower mount pad (2) and be connected, two be equipped with raw water diversion net (92) between annular mount pad (91) and see through water course net (93), annular mount pad (91) are gone up the vertical annular fixed slot of having seted up, raw water diversion net (92) with see through the upper and lower border of water course net (93) respectively with the tank bottom fixed connection of annular fixed slot, the reverse osmosis membrane laminating is in between raw water diversion net (92) and the water course net (93).
9. The reverse osmosis system applied to industrial concentrated salt wastewater according to claim 8, wherein: the raw water diversion net (92) is arranged close to the filter cartridge (4), the permeable water channel net (93) is arranged far away from the filter cartridge (4), and the aperture of the raw water diversion net (92) is smaller than that of the permeable water channel net (93).
10. A reverse osmosis system applied to industrial concentrated salt wastewater according to any one of claims 6, 8 or 9, wherein: the filter cylinder (4) is a stainless steel filter screen, the upper end and the lower end of the filter cylinder (4) are respectively and fixedly connected with the lower surface of the upper mounting seat (1) and the upper surface of the lower mounting seat (2), and the aperture of the stainless steel filter screen is smaller than 100 mu m.
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| JPH11253968A (en) * | 1998-03-12 | 1999-09-21 | Hitachi Chemical Techno Plant Co Ltd | Water recovery equipment |
| ES2183743B2 (en) * | 2001-08-17 | 2004-03-01 | Thomassen Johannes Adria | INSTALLATION OF RECYCLING OF AGRICULTURAL AND SIMILAR WASTE. |
| IL162713A (en) * | 2004-06-24 | 2011-04-28 | Desalitech Ltd | Apparatus and methods for continuous desalination in closed circuit without containers |
| CN1328179C (en) * | 2005-04-29 | 2007-07-25 | 国家海洋局天津海水淡化与综合利用研究所 | Reverse osmosis desalinization system capable of on-line back washing |
| CN201080447Y (en) * | 2007-07-26 | 2008-07-02 | 施国梁 | Reverse osmosis unit displaced in deep water |
| CN107530631B (en) * | 2015-04-16 | 2020-11-03 | 陶氏环球技术有限责任公司 | Filtration assembly comprising a spiral wound bioreactor and membrane module positioned in separate pressure vessels |
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