CN109692502A - A kind of water-oil separating filter structure and preparation method thereof - Google Patents

A kind of water-oil separating filter structure and preparation method thereof Download PDF

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Publication number
CN109692502A
CN109692502A CN201910141082.4A CN201910141082A CN109692502A CN 109692502 A CN109692502 A CN 109692502A CN 201910141082 A CN201910141082 A CN 201910141082A CN 109692502 A CN109692502 A CN 109692502A
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water
oil
oil separating
particle
separation
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文秀芳
曾新娟
杨康铨
皮丕辉
徐守萍
程江
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South China University of Technology SCUT
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South China University of Technology SCUT
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D17/00Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
    • B01D17/02Separation of non-miscible liquids
    • B01D17/0202Separation of non-miscible liquids by ab- or adsorption
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D17/00Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
    • B01D17/02Separation of non-miscible liquids
    • B01D17/0208Separation of non-miscible liquids by sedimentation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D17/00Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
    • B01D17/02Separation of non-miscible liquids
    • B01D17/04Breaking emulsions
    • B01D17/041Breaking emulsions with moving devices

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  • Thermal Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)

Abstract

The invention discloses a kind of water-oil separating filter structures and preparation method thereof;Water-oil separating filter structure includes filter device main body, filter device main body is equipped with filtration channel, filtration channel is equipped with support plate with holes, and water-oil separating dielectric layer is filled in filtration channel support plate with holes, and water-oil separating dielectric layer is the mixture of hydrocolloid particle and hydrophobic particles;Hydrocolloid particle is the one or more of silica, sand, ore, attapulgite;Hydrophobic particles are the one or more with the modified silica such as hexamethyldisilazane, sand, ore and attapulgite.Preparation process of the present invention is simple, raw material is environmentally friendly, at low cost, has good recycling rate of waterused, the efficiency of separation emulsification Water-In-Oil is up to 99.99%, and oil content can be down to 5ppm in water after the separation of emulsified water packet oil.

Description

A kind of water-oil separating filter structure and preparation method thereof
Technical field
The present invention relates to oily water separation technique fields, more particularly to a kind of water-oil separating filter structure and its preparation side Method belongs to chemical and technical field of function materials.
Background technique
The separation for emulsifying grease is always an important research direction of water-oil separating field, meanwhile, in industrial production In, the discharge of emulsified oily watewater will cause the pollution of environmental pollution, especially water resource.In fuel oil field, fuel oil purity The problem of also be always influence aircraft, internal combustion engine, the reliability of ship equal power device working performance and its service life weight Want one of factor.However, in traditional oily water separation technique, that there is also separative efficiencies is insufficient to the separation of emulsification grease, point From the problems such as energy consumption is high, flow resistance is excessive, also rarely has technology or material not only and can separate emulsification oil-in-water but also can be with Separation emulsification Water-In-Oil, therefore be badly in need of developing and a kind of can purify oily waste water also and can improve the efficient emulsification grease of oil product purity Separation technology.
Chinese invention patent application 2015109277283 discloses a kind of structured packing and its preparation for water-oil separating Method, the structured packing for water-oil separating include retainer, particle I, partition, particle II, axis, cover board, fastener;Retainer It is connected firmly with axis;I ordered arrangement of particle in the upper area of retainer, II ordered arrangement of particle in the lower area of retainer, and I region of particle and II region of particle are partitioned into two regions;Cover board is located at the upper table that particle I constitutes region Face;Partition and cover plate central are provided with through-hole, and axis is pierced by by through hole;Fastener is located at the upper surface center of cover board and locks cover board Tightly.This kind of structured packing is by layering filling with I layer super-hydrophobic of performance particle of super oleophylic and with superhydrophilic superoleophobic II layer of performance particle is prepared.Water quilt when oil water mixture passes through I layers of superhydrophilic superoleophobic particle, in oil water mixture Adhere to, condense into big water droplet, and oil then continues up to enter super II layers of oleophylic super-hydrophobic particle, and then utilizes the close of water-oil phase Degree difference realizes the separation of water-oil phase.Due to I layers of superhydrophilic superoleophobic particle the oil in oil water mixture can be generated it is very big Resistance, it is necessary to providing enough outside energies could allow oil to overcome resistance by superhydrophilic superoleophobic particle layer, into super oleophylic II layers of super-hydrophobic particle carries out water-oil separating.Moreover, because the blocking effect of emulsifier, under without other active forces, emulsification Droplet and oil droplet are difficult to sprawl on particle, adhere to, and therefore, which is difficult to realize the separation to stable emulsion grease.
Chinese invention patent 2016100238023 is using copper mesh as material, using carbon black film as template, is existed using chemical reaction Microcosmic surface is constructed on copper mesh, and the special wellability surface that can be used for water-oil separating is obtained by silicic acid anhydride.Before modification, The copper mesh of the invention be it is super hydrophilic, superoleophobic, after modification, the copper mesh of the invention is super-hydrophobic, super oleophylic, therefore corresponding Different actual conditions can achieve different water-oil separating purposes.The invention utilizes super hydrophilic, the underwater superoleophobic copper prepared Net and super-hydrophobic oleophylic copper mesh realize water-oil separating, but preparation method needs high-temperature baking, prepare it is more complicated, and only By special wettable surfaces come oil-water separation mixture, different wetting surface is not applied in combination, therefore excessive Copper mesh mesh aperture can largely effect on the separative efficiency to micro/nano level emulsification grease.
Summary of the invention
For overcome the deficiencies in the prior art, the first purpose of this invention is to provide a kind of water-oil separating filtering knot Structure, structure is simple, easy to use, save the cost, and separative efficiency is high.
Second is designed to provide a kind of preparation method of water-oil separating filter structure, and preparation is convenient, and preparation cost is low.
To realize goal of the invention, the technical solution of use are as follows:
A kind of water-oil separating filter structure, including filter device main body, the filter device main body are equipped with filtration channel, institute The filtration channel stated is equipped with support plate with holes, and water-oil separating dielectric layer is filled in the filtration channel support plate with holes, described Water-oil separating dielectric layer is the mixture of hydrocolloid particle and hydrophobic particles;The water-oil separating medium layer height is in 1~10cm;
The hydrocolloid particle is the one or more of silica, sand, ore, attapulgite, and described is hydrophilic Particle diameter is 25~250 μm;
The hydrophobic particles are with hexamethyldisilazane, tetramethyl-disilazane, vinyl silazane, hexamethyl two Siloxanes, dimethyl silicone polymer, dodecyltrimethoxysilane, dodecyltrichlorosilane or octadecyldimethyl The one or more of the modified silica of one or more of chlorosilane, sand, ore and attapulgite;Described Hydrophobic particles partial size is 25~250 μm;
The mass ratio of the hydrocolloid particle and hydrophobic particles is 1:9-8:1;The water-oil separating filter structure is applied in cream Change oil-in-water separation, after separation in water oil content down to 5ppm;
The mass ratio of the hydrocolloid particle and hydrophobic particles is 1:99-9:1;The water-oil separating filter structure is applied The separation for emulsifying Water-In-Oil, oily purity is up to 99.99% after separation.
To further realize the object of the invention, it is preferable that the filter device main body is glass column, plastic tube, stainless steel Pipe, ceramic tube, copper pipe or aluminum pipe.
Preferably, the filter device body shape is cylindrical, triangular prism shaped or square column type;The filtration channel is cut Face shape is cylindrical, triangular prism shaped or square column type.
Preferably, the support plate with holes is sand core gasket, stainless steel gasket with holes;In the support plate with holes Aperture is 1-250 μm.
Preferably, the oil-in-water be water respectively with chloroform, methylene chloride, n-hexane, hexamethylene, hexadecane, petroleum The oil-in-water that one of ether, toluene, vegetable oil, diesel oil, kerosene, gasoline, machine oil, crude oil and aviation kerosine are formed.
Preferably, the Water-In-Oil be chloroform, methylene chloride, n-hexane, hexamethylene, hexadecane, petroleum ether, toluene, The Water-In-Oil that one of vegetable oil, diesel oil, kerosene, gasoline, machine oil, crude oil and aviation kerosine are formed with water.
Preferably, the water-oil separating medium layer height is 2~8cm.
A kind of preparation method of water-oil separating filter structure, comprising the following steps:
1) it takes hydrocolloid particle and hydrophobic particles to mix, is stirred evenly after ethyl alcohol is added, obtain mixed liquor A;
2) a filter device main body with support plate filtration channel with holes is taken, mixed liquor A prepared by step 1) is poured into It in filtration channel, stands, hydrocolloid particle and hydrophobic particles is made to be precipitated as water-oil separating dielectric layer;
3) hydrocolloid particle, hydrophobic particles are deposited in the support plate in filtration channel by gravity, are completed separation and are situated between Matter filling.
Preferably, described stir evenly of step 1) is that 5-8min is stirred in blender.
A kind of water-oil separating filter structure provided by the invention is can to collect mist in air from the crust of desert chafer It gains enlightenment in the phenomenon that water.It is situated between in the water-oil separating filter structure by the separation that hydrocolloid particle and hydrophobic particles mixing form Matter.By adjusting the ratio of hydrocolloid particle and hydrophobic particles, emulsification Water-In-Oil or the separation of emulsified water packet oil are realized.It is hydrophilic when adjusting When the ratio of particle and hydrophobic particles is 1:99-9:1, hydrocolloid particle will emulsify nano-micro level droplet in Water-In-Oil and be gathered into greatly Droplet, and the duct formed between particle makes oil pass through separating medium layer, and prevents to be led to by the large water drop that hydrocolloid particle is assembled It crosses, to realize efficient oil emulsion packet water separation;Equally, when the ratio of adjustment hydrocolloid particle and hydrophobic particles is 1:9-8:1 When, hydrophobic oleophilic oil particle will emulsify the small oil droplet of nano-micro level in oil-in-water and be gathered into big oil droplet, and super hydrophilic-underwater superoleophobic grain The duct that son is formed makes water pass through separating medium layer, and prevents to be passed through by the big oil droplet of hydrophobic oleophilic oil particle buildup, thus Realize efficient emulsified water packet oil separation.
Oil emulsion packet aqueous mixtures pour into filtration channel by a kind of end suitable for reading of oil-water separating structure, are passing through separating medium When layer, generate one of wettability gradient between hydrocolloid particle and hydrophobic particles is unbalanced to make every effort to promote into receiving in emulsification Water-In-Oil Micron order droplet is gathered into large water drop on hydrocolloid particle surface, and super-hydrophobic oleophylic particle and hydrocolloid particle all have it is super Lipophilicity, the duct formed between all particles makes oil pass through separating medium layer, and prevents the flood assembled by hydrocolloid particle Pearl passes through, and pure oil is finally obtained in the lower port of oil-water separating structure, to realize efficient oil emulsion packet water separation;
Emulsified water packet oil mixture pours into filtration channel by a kind of end suitable for reading of oil-water separating structure, is passing through separating medium When layer, generate one of wettability gradient between hydrocolloid particle and hydrophobic particles is unbalanced to make every effort to promote into receiving in emulsification oil-in-water The small oil droplet of micron order is gathered into big oil droplet in hydrophobic oleophilic oil particle surface, makes to emulsify oil-in-water demulsification, and super hydrophilic particle shape At duct so that water is passed through separating medium layer, and prevent to be passed through by the big oil droplet of oleophylic particle buildup, finally in grease point Pure water is obtained from the lower port of structure, to realize efficient emulsified water packet oil separation.
Compared with prior art, it has the following advantages that and technical effect:
1) present invention is not needed using highly acid, strong basic reagent, no in the preparation process of water-oil separating filter structure Palpus high-temperature calcination, institute is easy to get using material, low in cost, easy to operate, does not need special equipment and instrument, and pressure resistance is had excellent performance, So as to obtain big separation flux by increasing pressure.
2) the resulting water-oil separating filter structure of the present invention passes through the wetting ladder between mixed hydrophobic particles and hydrocolloid particle Emulsified water aggregation in degree difference driving water in oil emulsion and oil is merged into big liquid pearl, and passes through hydrocolloid particle and hydrophobic particles Mixed proportion substantially reduces oil or the resistance that passes through of water, realize without the lower emulsification oil-in-water of extraneous energy consumption and emulsifies Water-In-Oil Separation.Chloroform, methylene chloride, n-hexane, hexamethylene, hexadecane, petroleum ether, benzene, vegetable oil, diesel oil, coal can be achieved in the present invention The emulsification oil-in-water and emulsify efficiently separating for Water-In-Oil that oil, gasoline, machine oil, crude oil and aviation kerosine are formed with water.
Detailed description of the invention
Fig. 1 is water-oil separating filter structure schematic diagram prepared by the embodiment of the present invention 1.
Fig. 2 is water-oil separating filter structure schematic diagram prepared by the embodiment of the present invention 2.
Fig. 3 is the particle diameter distribution of emulsified water packet oil separation front and back prepared by the embodiment of the present invention 1.
Fig. 4 is the particle diameter distribution of oil emulsion packet water separation front and back prepared by the embodiment of the present invention 2.
Specific embodiment
For a better understanding of the invention, the present invention is further illustrated with reference to the accompanying drawings and examples, but this hair Bright embodiment is unlimited so.
Embodiment 1
A kind of preparation method of water-oil separating filter structure, includes the following steps:
1) silicon dioxide granule and hexamethyldisilazane are added in round-bottomed flask, after being stirred 2 hours at 80 DEG C, It is modified as super-hydrophobic silica particle;Hydrophobic particles in all embodiments of the invention are modified referring to the method system It is standby.
2) taking partial size is 25~50 μm of hydrophilic silicon dioxide particles, takes the modified obtained partial size of hexamethyldisilazane and is 25~50 μm of hydrophobic silicon dioxide granules, by the mass ratio of 8:1 by hydrophilic silicon dioxide particle and hydrophobic silica particle It mixes, stirs 5min in blender after addition ethyl alcohol.
3) the tool sand formula glass column that aperture is 25 μm is fixed on iron stand.By step 1) preparation stuff and other stuff together with Ethyl alcohol pours into column;It stands, hydrophilic silicon dioxide particle and hydrophobic silica particle is made to be precipitated as water-oil separating dielectric layer.It crosses Filter body shape and the shape of filtration channel in this embodiment, do not do specific restriction, in actual operation may be used To be arranged to arbitrary shape, filtration body outer shape is cylindrical or triangular prism shaped or square column type;The section of filtration channel Shape is cylindrical or triangular prism shaped or square column type etc..Filter device main body and filtration channel diameter this specific implementation Do not limited specifically in mode, according to the actual situation in need it is to be separated emulsification grease amount be configured.
4) hydrophilic silicon dioxide particle, hydrophobic silica particle are deposited on glass column sand core by gravity, i.e., Separating medium filling is completed, separating medium height is 3cm;
Fig. 1 is the structural schematic diagram of the present embodiment 1, and after silicon dioxide granule filling, gap is formed between particle and particle Split tunnel, while being filled after hydrophilic silicon dioxide particle and hydrophobic silica particle stirring, hydrophobic particles are evenly distributed on Between hydrocolloid particle, the separating medium layer of hydrophobe-hydrophile is formd.
The grease filter structure separation of separating medium layer with hydrophobe-hydrophile emulsifies oil-in-water test:
It takes 3g Tween 80 to be placed in a beaker, and 500mL deionized water and 10mL isooctane is added, magnetic agitation is added and turns Son continuously stirs and prepares milky stable emulsion oil-in-water for 24 hours.Pour into the grease of the present embodiment from top to bottom with deionized water Filter structure pours into stable oil-in-water emulsion after separating medium layer rinse three times, due to super hydrophilic silicon dioxide granule and Assemble in dissolved oil and emulsified oil bead to hydrophobic silica particle in super-hydrophobic particle surface wetting gradient difference driving water and closes And at big oil droplet.Meanwhile accounting can allow water to pass through for the split tunnel of 8/9 hydrocolloid particle formation, and prevent to be dredged The big oil droplet of water silica aggregate realizes efficient emulsified water packet oil separation by separating medium layer.
Oil water mixture successively passes sequentially through super-hydrophobic particle layer and surpasses in Chinese invention patent application 2015109277283 Hydrocolloid particle layer, the method separated using the density contrast of oil and water emulsify the micro-nano in grease when separation emulsifies grease Meter level droplet can be by inter-particle voids, and the weight of micro/nano level droplet is too small, can not be by density contrast come real Now separate.
The present invention using hydrocolloid particle and it is hydrophobic between wettability gradient difference to emulsification grease in micro/nano level droplet Unbalanced force is generated, so that it is demulsified and is gathered into big drop, common material can not only be separated and be difficult to isolated nanoscale emulsification Grease, and be emulsify grease be demulsified in advance can reduce emulsification water-oil separating during resistance, increase its separation flux.It is logical The particle diameter distribution of oil droplet in the emulsified water packet oil separation front and back emulsification oil-in-water of Ma Erwei particle size analyzer survey is crossed, as shown in figure 3, It is 100-1000nm that (a), which emulsifies oil-in-water particle diameter distribution, before separation, and it is 10- that (b), which emulsifies oil-in-water particle diameter distribution, after separation 60nm, measuring oil content in water with Infrared Oil Determination Instrument is 5ppm.
The test of the grease filter structure separation emulsification Water-In-Oil of separating medium layer with hydrophilic-hydrophobic:
It takes 3g span80 in beaker, and the hexadecane of 500mL and the deionized water of 10ml is added, magnetic agitation is added Rotor continuously stirs and prepares milky white colour-stable emulsification Water-In-Oil for 24 hours.The stabilization water-in-oil emulsion for pouring into preparation, due to super close Assemble on emulsification droplet to hydrophilic silicon dioxide in water particle and super-hydrophobic particle surface wetting gradient difference driving oil and is merged into Large water drop.Meanwhile because hydrocolloid particle and hydrophobic particles are all super close, hydrocolloid particle and hydrophobic particles in separating medium to oil Accounting will not be to there is oil to cause resistance, the channel that partial size is formed can allow oil to pass through, and prevent by hydrophilic silicon dioxide The large water drop of aggregation realizes efficient oil emulsion packet water separation by separating medium layer.Therefore pass through Ma Erwei particle size analyzer The particle diameter distribution of droplet in the oil emulsion packet water separation front and back emulsification Water-In-Oil of survey, as shown in figure 4, (a) oil emulsion packet before separation The particle diameter distribution of water is 200-2800nm, and the particle diameter distribution that (b) emulsifies Water-In-Oil after separation is 30-100nm, passes through karl Fischer Oily purity is 98.0% before the separation that drimeter is surveyed, and oily purity has reached 99.99% after separation.
Embodiment 2
A kind of preparation method of water-oil separating filter structure, includes the following steps:
1) partial size is taken to be 200~250 μm of hydrophilic sands and with the modified obtained partial size of octadecyldimethylchlorosilane be 200~250 μm of hydrophobic sands are mixed by the mass ratio of 1:99, stir 5min in blender after addition ethyl alcohol;
It 2) is to be fixed in ceramic tube passage that 200 μm of stainless steel bracing plate with holes is mounted on and by ceramic tube by aperture On iron stand.Stuff and other stuff prepared by step 1 is poured into pipe together with ethyl alcohol, is stood, and hydrophilic sand and hydrophobic sand are precipitated For water-oil separating dielectric layer;
3) hydrophilic sand, hydrophobic sand are deposited in ceramic tube inner support plate by gravity, i.e. completion separating medium Filling, separating medium height are 10cm.
Fig. 2 is the structural schematic diagram of the present embodiment.After sand filling, gap forms split tunnel between sand and sand, It is filled after hydrophilic sand and the stirring of hydrophobic sand simultaneously, hydrophilic sand is evenly distributed between hydrophobic sand, is formd hydrophilic-thin The separating medium layer of water.
It takes 3g Tween 80 to be placed in a beaker, and 500mL deionized water and 10mL diesel oil is added, magnetic agitation rotor is added, It continuously stirs and prepares stable emulsion oil-in-water for 24 hours.It takes 3g span80 in beaker, and the diesel oil of 500mL and going for 10ml is added Ionized water is added magnetic agitation rotor, continuously stirs and prepare stable emulsion Water-In-Oil for 24 hours;Grease filtering is prepared with above-mentioned steps The stable emulsion oil-in-water that diesel oil is prepared in structure separation and deionized water is formed, pours into filtering for the stable emulsion oil-in-water of preparation After structure, stable emulsification oil-in-water is trapped.Because the accounting of hydrophobic particles is too big, cause the resistance to water big, is not suitable for Separate stable emulsion oil-in-water.The oil emulsion packet that above-mentioned steps prepare grease filter structure separation diesel oil and deionized water is formed Water, after separation, surveying oily purity by karl Fischer drimeter is 99.99%.Illustrate point of the big formation of hydrophobic particles accounting The separation to stable emulsion Water-In-Oil may be implemented from structure.
Embodiment 3
A kind of preparation method of water-oil separating filter structure, includes the following steps:
1) partial size is taken to be 30~60 μm of hydrophilic ores and be 50~100 with the modified obtained partial size of dodecyltrichlorosilane μm hydrophobic ore is mixed by the mass ratio of 9:1, is added after ethyl alcohol and is stirred 5min in blender;
2) the stainless steel bracing plate with holes that aperture is 60 μm is mounted in copper pipe channel, and be fixed on iron stand.It will Mixed ore prepared by step 1 pours into pipe together with ethyl alcohol;It stands, mixed ore is made to be precipitated as water-oil separating dielectric layer;
3) hydrophilic ore, hydrophobic ore are deposited on plastics tube support plate by gravity, i.e. completion separating medium is filled out It fills, separating medium height is 4cm.
It takes 3g Tween 80 to be placed in a beaker, and 500mL deionized water and 10mL chloroform is added, magnetic agitation rotor is added, It continuously stirs and prepares milky stable emulsion oil-in-water for 24 hours.Take 3g span80 in beaker, and be added 500mL chloroform and The deionized water of 10ml is added magnetic agitation rotor, continuously stirs and prepare milky stable emulsion Water-In-Oil for 24 hours, with above-mentioned step Suddenly the stable emulsion oil-in-water that chloroform is prepared in the separation of grease filter structure and deionized water is formed is prepared, by the stable emulsion of preparation After oil-in-water pours into filter structure, the liquid come out from filter structure lower port is collected, milky is remained, uses Infrared Oil Determination Instrument Measuring oil content in water is 1009ppm, illustrates stable emulsion oil-in-water not by separating-purifying.Main cause is stable emulsification Oil-in-water is demulsified, and resistance is very big, and hydrophobic particles accounting is very little, and the demulsification for generating wettability gradient difference with hydrocolloid particle is too weak, Therefore inferior separating effect.To further illustrate in embodiment 1, the wettability gradient difference between hydrocolloid particle and hydrophobic particles is to cream The micro/nano level droplet changed in oil-in-water generates unbalanced force, so that it is demulsified and is gathered into this process of big drop to stable cream It is vital for changing oil-in-water separation.The stable emulsion Water-In-Oil for separating chloroform and deionized water formation, after separation, passes through It is 99.99% that karl Fischer drimeter, which surveys oily purity,.The separated structure for illustrating that simple hydrocolloid particle is formed may be implemented Separation to stable emulsion Water-In-Oil.
Embodiment 4
A kind of preparation method of water-oil separating filter structure, includes the following steps:
1) take partial size be 100~150 μm of hydrophilic attapulgites and with the modified obtained partial size of vinyl silazane be 150~ 200 μm of hydrophobic attapulgites are mixed by the mass ratio of 1:1, stir 5min in blender after addition ethyl alcohol;
2) sand core that aperture is 30 μm is mounted in plastics tube passage and is fixed on iron stand, is prepared by step 1 Mixed Concave convex stick soil pours into pipe together with ethyl alcohol;It stands, Mixed Concave convex stick soil is made to be precipitated as water-oil separating dielectric layer;
3) hydrophilic attapulgite, hydrophobic attapulgite are deposited on plastics tube support plate by gravity, that is, complete to divide From media filler, separating medium height is 1cm.
It takes 3g Tween 80 to be placed in a beaker, and 500mL deionized water and 10mL toluene is added, magnetic agitation rotor is added, It continuously stirs and prepares milky stable emulsion oil-in-water for 24 hours.Take 3g span80 in beaker, and be added 500mL toluene and The deionized water of 10ml is added magnetic agitation rotor, continuously stirs and prepare milky stable emulsion Water-In-Oil for 24 hours, with above-mentioned step Suddenly the stable emulsion oil-in-water that the separation of grease filter structure is formed with preparing methylbenzene and deionized water is prepared, with infrared survey oil after separation It is 6ppm that instrument, which measures oil content in water, and the stable emulsion Water-In-Oil that separation of methylbenzene and deionized water are formed after separation, passes through karr Taking the not oily purity of drimeter survey is 99.99%.
Embodiment 5
A kind of preparation method of water-oil separating filter structure, includes the following steps:
1) partial size is taken to be 160~200 μm of hydrophilic attapulgites and be 70 with the partial size that polydimethylsiloxane--modified obtains ~100 μm of hydrophobic silicas are mixed by the mass ratio of 4:1, stir 5min in blender after addition ethyl alcohol;
2) the tool sand formula glass column that aperture is 70 μm is fixed on iron stand.Stuff and other stuff prepared by step 1 together with Ethyl alcohol pours into pipe;It stands, stuff and other stuff is made to be precipitated as water-oil separating dielectric layer;
3) hydrophilic attapulgite, hydrophobic silica are deposited on glass column sand core by gravity, that is, complete separation Media filler, separating medium height are 6cm.
It takes 3g Tween 80 to be placed in a beaker, and 500mL deionized water and 10mL aviation kerosine is added, magnetic agitation is added and turns Son continuously stirs and prepares stable emulsion oil-in-water for 24 hours.Take 3g span80 in beaker, and be added 500mL aviation kerosine and The deionized water of 10ml is added magnetic agitation rotor, continuously stirs and prepare stable emulsion Water-In-Oil for 24 hours, prepared with above-mentioned steps The stable emulsion oil-in-water that aviation kerosine is prepared in the separation of grease filter structure and deionized water is formed, uses Infrared Oil Determination Instrument after separation Measuring oil content in water is 5ppm, separates the stable emulsion Water-In-Oil of aviation kerosine and deionized water formation, after separation, passes through card It is 99.99% that Er Feixiu drimeter, which surveys oily purity,.
Embodiment 6
A kind of preparation method of water-oil separating filter structure, includes the following steps:
1) take partial size be 25~50 μm of hydrophilic silicon dioxides and with the partial size that polydimethylsiloxane--modified obtains be 60~ 80 μm of hydrophobic silicas are mixed by the mass ratio of 1:1, stir 5min in blender after addition ethyl alcohol;
2) the stainless steel bracing plate with holes that aperture is 25 μm is mounted in stainless steel tube channel, and stainless steel tube is fixed On iron stand.Mixing silica prepared by step 1 is poured into pipe together with ethyl alcohol;It stands, makes to mix precipitation of silica For water-oil separating dielectric layer;
3) hydrophilic silicon dioxide, hydrophobic silica are deposited on stainless steel bracing plate by gravity, that is, complete to divide From media filler, separating medium height is 9cm.
It takes 3g Tween 80 to be placed in a beaker, and 500mL deionized water and 10mL kerosene is added, magnetic agitation rotor is added, It continuously stirs and prepares milky stable emulsion oil-in-water for 24 hours.Take 3g span80 in beaker, and be added 500mL kerosene and The deionized water of 10ml is added magnetic agitation rotor, continuously stirs and prepare milky stable emulsion Water-In-Oil for 24 hours, with above-mentioned step Suddenly the stable emulsion oil-in-water that kerosene is prepared in the separation of grease filter structure and deionized water is formed is prepared, with infrared survey oil after separation It is 5ppm that instrument, which measures oil content in water, and separation flux is 1200L/ (m2*h);Separate the stable cream of kerosene and deionized water formation Change Water-In-Oil, after separation, surveying oily purity by karl Fischer drimeter is 99.99%, and flux is 2300L/ (m2*h).
Pass through the emulsified water for after the stainless steel tube 10kpa suitable for reading with force (forcing) pump pressurization, separating kerosene and deionized water is formed Packet oil, oil content is 8ppm in water after separation, and separation flux is 5400L/ (m2*h), the cream that separation kerosene and deionized water are formed Change Water-In-Oil, oily purity is 99.99% after separation, and flux is 10000L/ (m2*h).It follows that by increasing pressure, it can be with The flux of separation emulsification grease is greatly increased, and oil, the impurities affect of water are little after meeting separative efficiency and separation.And because The separated structure is had excellent performance using the pressure-resistant material such as stainless steel tube and inorganic micro particles, pressure resistance.
The ratio of hydrocolloid particle and hydrophobic particles is 8:1 in embodiment 1, can both separate emulsification oil-in-water, can also divide Being separated from milk Water-In-Oil.
The ratio of hydrocolloid particle and hydrophobic particles is 1:99 in embodiment 2, and the separation for efficiently emulsifying Water-In-Oil may be implemented. Because the accounting of hydrophobic particles is big, unsuitable separation stable emulsion oil-in-water big to the resistance of water will lead to.
The ratio of hydrocolloid particle and hydrophobic particles is 9:1 in embodiment 3, because the demulsification resistance of emulsification Water-In-Oil is smaller, And hydrocolloid particle has the property of oleophylic, can be efficiently separated.And it is big to emulsify oil-in-water demulsification resistance, hydrophobic particles Accounting is very little, and the demulsification for generating wettability gradient difference with hydrocolloid particle is too weak, therefore inferior separating effect.
The ratio of hydrocolloid particle and hydrophobic particles is 1:1 in embodiment 4, can both separate emulsification oil-in-water, can also divide Being separated from milk Water-In-Oil.
The ratio of hydrocolloid particle and hydrophobic particles is 4:1 in embodiment 5, can both separate emulsification oil-in-water, can also divide Being separated from milk Water-In-Oil.And the hydrocolloid particle of variety classes, different-grain diameter is mixed with hydrophobic particles, may be implemented to emulsification grease It efficiently separates.Therefore, when hydrocolloid particle and hydrophobic particles are that ratio can efficiently separate oil emulsion packet between 1:99 to 9:1 The ratio of water, hydrocolloid particle and hydrophobic particles can both separate emulsification Water-In-Oil between 1:9 to 8:1, can also efficiently separate Emulsify oil-in-water.
Embodiment of the present invention are not limited by the above embodiments, other any real without departing from spirit of the invention Made changes, modifications, substitutions, combinations, simplifications under matter and principle, should be equivalent substitute mode, are included in the present invention Protection scope within.

Claims (9)

1. a kind of water-oil separating filter structure, it is characterised in that: including filter device main body, the filter device main body was equipped with Channel is filtered, the filtration channel is equipped with support plate with holes, is situated between in the filtration channel support plate with holes filled with water-oil separating Matter layer, the water-oil separating dielectric layer are the mixture of hydrocolloid particle and hydrophobic particles;The water-oil separating medium layer height is 1 ~10cm;
The hydrocolloid particle is the one or more of silica, sand, ore, attapulgite, the hydrocolloid particle Partial size is 25~250 μm;
The hydrophobic particles are with hexamethyldisilazane, tetramethyl-disilazane, vinyl silazane, two silicon oxygen of hexamethyl Alkane, dimethyl silicone polymer, dodecyltrimethoxysilane, dodecyltrichlorosilane or octadecyldimethyl chlorine silicon The one or more of the modified silica of one or more of alkane, sand, ore and attapulgite;Described is hydrophobic Particle diameter is 25~250 μm;
The mass ratio of the hydrocolloid particle and hydrophobic particles is 1:9-8:1;The water-oil separating filter structure is applied in emulsified water Packet oil separation, after separation in water oil content down to 5ppm;
The mass ratio of the hydrocolloid particle and hydrophobic particles is 1:99-9:1;The water-oil separating filter structure is applied in oil emulsion The separation of Bao Shui, oily purity is up to 99.99% after separation.
2. water-oil separating filter structure according to claim 1, it is characterised in that: the filter device main body is glass Column, plastic tube, stainless steel tube, ceramic tube, copper pipe or aluminum pipe.
3. water-oil separating filter structure according to claim 1, it is characterised in that: the filter device body shape is circle Cylindricality, triangular prism shaped or square column type;The cross sectional shape of the filtration channel is cylindrical, triangular prism shaped or square column type.
4. water-oil separating filter structure according to claim 1, it is characterised in that: the support plate with holes is sand core pad Piece, stainless steel gasket with holes;Aperture in the support plate with holes is 1-250 μm.
5. water-oil separating filter structure according to claim 1, it is characterised in that: the oil-in-water be water respectively with chlorine Imitative, methylene chloride, n-hexane, hexamethylene, hexadecane, petroleum ether, toluene, vegetable oil, diesel oil, kerosene, gasoline, machine oil, crude oil The oil-in-water formed with one of aviation kerosine.
6. water-oil separating filter structure according to claim 1, it is characterised in that: the Water-In-Oil is chloroform, dichloro Methane, n-hexane, hexamethylene, hexadecane, petroleum ether, toluene, vegetable oil, diesel oil, kerosene, gasoline, machine oil, crude oil and aviation coal The Water-In-Oil that one of oil is formed with water.
7. a kind of water-oil separating filter structure according to claim 1, it is characterised in that: the water-oil separating dielectric layer is high Degree is 2~8cm.
8. the preparation method of the described in any item water-oil separating filter structures of claim 1-7, it is characterised in that including following step It is rapid:
1) it takes hydrocolloid particle and hydrophobic particles to mix, is stirred evenly after ethyl alcohol is added, obtain mixed liquor A;
2) a filter device main body with support plate filtration channel with holes is taken, mixed liquor A prepared by step 1) is poured into filtering It in channel, stands, hydrocolloid particle and hydrophobic particles is made to be precipitated as water-oil separating dielectric layer;
3) hydrocolloid particle, hydrophobic particles are deposited in the support plate in filtration channel by gravity, are completed separating medium and are filled out It fills.
9. the preparation method of water-oil separating filter structure according to claim 8, it is characterised in that: the step 1) stirring It is uniformly that 5-8min is stirred in blender.
CN201910141082.4A 2019-02-26 2019-02-26 A kind of water-oil separating filter structure and preparation method thereof Pending CN109692502A (en)

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CN112499858A (en) * 2020-12-01 2021-03-16 华东理工大学 Demulsification device and method for coalescence of coupling medium of non-uniform electric field
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CN112473188A (en) * 2020-12-01 2021-03-12 华东理工大学 Electric field enhanced O/W emulsion demulsification and oil removal device and method
CN112505302A (en) * 2020-12-01 2021-03-16 华东理工大学 Continuous-flow electric field and medium synergistic coalescence demulsification effect evaluation system
CN112499858A (en) * 2020-12-01 2021-03-16 华东理工大学 Demulsification device and method for coalescence of coupling medium of non-uniform electric field
CN112526110A (en) * 2020-12-01 2021-03-19 华东理工大学 System and method for evaluating coalescence demulsification effect of continuously flowing electric field strengthening medium
CN115748237A (en) * 2022-11-08 2023-03-07 杭州传化精细化工有限公司 Fluoride-free super-hydrophobic material and preparation method thereof

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Application publication date: 20190430