CN111686589A - Filter structure and preparation method thereof - Google Patents
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- CN111686589A CN111686589A CN202010693860.3A CN202010693860A CN111686589A CN 111686589 A CN111686589 A CN 111686589A CN 202010693860 A CN202010693860 A CN 202010693860A CN 111686589 A CN111686589 A CN 111686589A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 230000008878 coupling Effects 0.000 claims abstract description 104
- 238000010168 coupling process Methods 0.000 claims abstract description 104
- 238000005859 coupling reaction Methods 0.000 claims abstract description 104
- 239000000758 substrate Substances 0.000 claims abstract description 48
- 239000012528 membrane Substances 0.000 claims abstract description 37
- 229920002492 poly(sulfone) Polymers 0.000 claims abstract description 36
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims abstract description 29
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000001914 filtration Methods 0.000 claims description 132
- 239000011159 matrix material Substances 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 24
- 239000011148 porous material Substances 0.000 claims description 23
- 239000013067 intermediate product Substances 0.000 claims description 21
- 239000000463 material Substances 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- 229910052593 corundum Inorganic materials 0.000 claims description 6
- 238000007654 immersion Methods 0.000 claims description 6
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 6
- 239000000919 ceramic Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000006277 sulfonation reaction Methods 0.000 claims description 2
- 238000007598 dipping method Methods 0.000 claims 1
- 239000005416 organic matter Substances 0.000 abstract description 4
- 239000010410 layer Substances 0.000 description 47
- 230000008569 process Effects 0.000 description 13
- 239000000126 substance Substances 0.000 description 13
- 125000000524 functional group Chemical group 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 238000013329 compounding Methods 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 230000002829 reductive effect Effects 0.000 description 3
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical group [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- 230000001680 brushing effect Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
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- 238000010537 deprotonation reaction Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000036961 partial effect Effects 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 230000005588 protonation Effects 0.000 description 2
- 229910052594 sapphire Inorganic materials 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
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- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000001728 nano-filtration Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000001223 reverse osmosis Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/38—Liquid-membrane separation
- B01D61/40—Liquid-membrane separation using emulsion-type membranes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/36—Hydrophilic membranes
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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- Chemical Kinetics & Catalysis (AREA)
- Water Supply & Treatment (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
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- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a filter structure and a preparation method thereof, wherein the filter structure comprises an inorganic filter substrate and an organic coupling layer, the inorganic filter substrate is provided with a plurality of first filter holes, the aperture of each first filter hole is less than or equal to 60nm, the inorganic filter substrate comprises a support body and a membrane layer, the support body is made of alpha-Al 2O3, the membrane layer is made of ZrO2, the organic coupling layer comprises sulfonated polysulfone and dimethylacetamide, the organic coupling layer is arranged on the hole wall of each first filter hole to form a plurality of second filter holes, and the aperture value of each second filter hole is 0.8-0.95 times of the aperture value of each first filter hole. The technical scheme can solve the problem that the infrastructure cost and the equipment cost are relatively high when the inorganic membrane oil removal equipment and the organic membrane organic matter removal equipment are installed in series at present.
Description
Technical Field
The invention relates to the technical field of filtering membranes, in particular to a filtering structural part and a preparation method thereof.
Background
In the field of water treatment, it is a common filtration method to filter water by using a filtration membrane. Common filtration membrane divide into organic membrane and inorganic membrane usually, the cost of organic membrane is lower, the high temperature resistance and the corrosion resisting property of inorganic membrane are all relatively better, and mechanical strength is high, and inorganic membrane is better than organic membrane in the filterability in fields such as waste emulsion, consequently, in the processing procedure to the comparatively complicated waste water of pollutant, need use inorganic membrane and organic membrane simultaneously to filter usually, with oily substance and the organic matter that contains in the aquatic filter, but, at present, it is relatively higher to remove infrastructure cost and the equipment cost homogeneous phase when organic matter equipment is established ties to the installation with inorganic membrane deoiling equipment and organic membrane.
Disclosure of Invention
The invention discloses a filtering structural member and a preparation method thereof, which aim to solve the problem that the infrastructure cost and the equipment cost are relatively high when inorganic membrane oil removal equipment and organic membrane organic matter removal equipment are installed in series at present.
In order to solve the problems, the invention adopts the following technical scheme:
in a first aspect, an embodiment of the present invention discloses a filter structure, which includes an inorganic filter substrate and an organic coupling layer, wherein the inorganic filter substrate has a plurality of first filter holes, the pore diameters of the first filter holes are less than or equal to 60nm, the inorganic filter substrate includes a support and a membrane layer, the support is made of a-Al2O3The material of the film layer is ZrO2The organic coupling layer comprises sulfonated polysulfone and dimethylacetamide, the organic coupling layer is arranged on the wall of each first filtering hole to form a plurality of second filtering holes, and the second filtering holes are formedThe aperture value of the two filtering holes is 0.8-0.95 times of the aperture value of the first filtering hole.
In a second aspect, an embodiment of the present invention discloses a preparation method for preparing the above filter structure, where the preparation method includes:
obtaining an inorganic filtering substrate, wherein the inorganic filtering substrate is provided with a plurality of first filtering holes, the pore diameters of the first filtering holes are less than or equal to 60nm, the inorganic filtering substrate comprises a support body and a membrane layer, and the support body is made of a-Al2O3The material of the film layer is ZrO2；
Obtaining organic coupling sol, wherein the organic coupling sol comprises sulfonated polysulfone and dimethylacetamide;
immersing the inorganic filtering matrix into the organic coupling sol by adopting an immersion method, keeping the inorganic filtering matrix for a preset time, and taking out the inorganic filtering matrix to obtain a first intermediate product;
and drying the first intermediate product to obtain the filtering structural member, wherein the filtering structural member is provided with a plurality of second filtering holes, and the aperture value of the second filtering holes is 0.8-0.95 times that of the first filtering holes.
The technical scheme adopted by the invention can achieve the following beneficial effects:
the invention discloses a filtering structural member, which comprises an inorganic filtering matrix and an organic coupling multiple layer, wherein the inorganic filtering matrix is provided with a plurality of first filtering holes, the aperture of each first filtering hole is less than or equal to 60nm, and the material of a support body of the inorganic filtering matrix is alpha-Al2O3The material of the film layer is ZrO2The size of the first filtering hole is further reduced by forming the organic coupling layer in the first filtering hole of the inorganic filtering base body, the second filtering hole with smaller size is formed, and the aperture value of the second filtering hole is 0.8-0.95 times of the aperture value of the first filtering hole, so that the filtering performance of the filtering structural member is improved, and the filtering structural member formed by attaching the organic coupling layer to the inorganic filtering base body can simultaneously remove organic pollutants and oil pollutants in the treated water.
In addition, in the process of compounding the organic coupling layer and the inorganic filtering matrix, on one hand, sulfonated polysulfone and dimethylacetamide can be directly deposited on the hole wall of the first filtering hole, and on the other hand, a new chemical piece can be formed, and in detail, dimethylacetamide serving as a solvent of the sulfonated polysulfone and a non-solvent on the surface layer of the inorganic filtering matrix can perform double diffusion and electrostatic adsorption processes; meanwhile, in the compounding process, the sulfonated polysulfone is also connected with functional groups such as hydroxyl on the wall of a first filtering hole in the inorganic filtering matrix in a new chemical bond mode, and meanwhile, the organic coupling layer also chelates zirconium metal groups on the surface of the inorganic filtering matrix to generate PSF-DMA-ZrO2A composite material.
The filtering structural member disclosed by the embodiment of the invention mainly provides a filtering effect in a way of pore interception, physical adsorption and selective combination of partial functional groups, and compared with a conventional inorganic membrane, the filtering structural member disclosed by the embodiment of the invention obviously enhances the hydrophilicity of the material by combining an organic coupling layer, and also enhances the anti-pollution capacity of the filtering structural member in the separation process. In addition, the number of functional groups on the surface of the filtering structural member is also obviously increased, and the chelated metal groups can form charge factors through protonation or deprotonation, so that the electric property of the membrane surface is improved, and the filtering performance of the filtering structural member is further improved.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is a chemical block diagram of an inorganic filter matrix in a filter structure according to an embodiment of the present disclosure;
FIG. 2 is a schematic chemical diagram of a first intermediate product in a filter structure according to an embodiment of the disclosure;
FIG. 3 is a chemical schematic of a first intermediate product in a filter structure according to an embodiment of the disclosure;
FIG. 4 is a chemical block diagram of a filter construction according to an embodiment of the disclosure;
FIG. 5 is a flow chart of a method of making a filter construction according to an embodiment of the present disclosure.
Description of reference numerals:
100-inorganic filter matrix, 110-first filter hole, 120-second filter hole, 310-organic coupling sol, 320-organic coupling gel, 330-organic coupling layer.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to the specific embodiments of the present invention and the accompanying drawings. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The technical solutions disclosed in the embodiments of the present invention are described in detail below with reference to the accompanying drawings.
As shown in fig. 4, the embodiment of the present invention discloses a filter structure including an inorganic filter substrate 100 and an organic coupling layer 330.
As shown in FIG. 1, the inorganic filter substrate 100 has a plurality of first filter pores 110, the pore diameters of the first filter pores 110 are less than or equal to 60nm, the inorganic filter substrate 100 includes a support and a membrane layer, the support is made of a-Al2O3The material of the film layer is ZrO2The membrane layer is supported on a support to form an inorganic filter substrate 100. Specifically, the inorganic filter substrate 100 may be a flat plate-shaped structure, and the support and the membrane layer are formed with a plurality of first filter holes 110. In another embodiment of the present invention, the inorganic filter substrate 100 is a tubular inorganic ceramic membrane, and more specifically, the pore diameter of the first filter pores 110 is between 30nm and 50nm, the pore diameter of the channels of the inorganic filter substrate 100 may be between 3.2 mm and 3.6mm, and in addition, parameters such as the outer diameter and the length of the inorganic filter substrate 100 may be selected according to actual requirements.
The organic coupling layer 330 includes sulfonated polysulfone and dimethylacetamide, and the sulfonated polysulfone is a novel nanofiltration material and reverse osmosis organic membrane material, and has good chemical resistance and antibacterial decomposition resistance, so that the organic coupling layer 330 can be used as a material for forming the organic coupling layer, so that the overall filtering capacity of the filtering structure is good. The dimethylacetamide has good thermal stability, is not easy to hydrolyze, has low corrosivity and low toxicity, so that the dimethylacetamide is used as a solvent material of the sulfonated polysulfone, and the problem of secondary pollution in the filtering process can be prevented.
In the process of forming the organic coupling layer 330, the sulfonated polysulfone may be dissolved in dimethylacetamide to form a liquid organic coupling layer 330, the ratio of the two layers may be determined according to actual requirements, and then the organic coupling layer 330 may be formed on the inorganic filter substrate 100 by means of spraying or brushing, so that the organic coupling layer 330 is disposed on the hole wall of each first filter hole 110, after the organic coupling layer 330 blocks a part of the first filter hole 110, a plurality of second filter holes 120 having smaller hole diameters may be formed, and the hole diameter value of the formed second filter holes 120 may be 0.8 to 0.95 times the hole diameter value of the first filter hole 110.
The embodiment of the invention discloses a filter structure, which comprises an inorganic filter substrate 100 and an organic coupling layer 330, wherein the inorganic filter substrate 100 is provided with a plurality of first filter holes 110, the pore diameter of each first filter hole 110 is less than or equal to 60nm, and the material of a support body of the inorganic filter substrate 100 is alpha-Al2O3The material of the film layer is ZrO2By forming the organic coupling layer 330 in each of the first filtering holes 110 of the inorganic filtering substrate 100, the size of the first filtering holes 110 can be further reduced, the second filtering holes 120 with smaller size can be formed, and the aperture of the second filtering holes 120 is 0.8-0.95 times of the aperture of the first filtering holes 110, so that the filtering performance of the filtering structure is improved, and the organic pollutants and the oil pollutants in the treated water can be removed simultaneously by attaching the filtering structure formed by the organic coupling layer 330 to the inorganic filtering substrate 100.
In addition, in the process of compounding the organic coupling layer 330 with the inorganic filter substrate 100, on the one hand,sulfonated Polysulfone (PSF) and Dimethylacetamide (DMA) can be directly deposited on the walls of the first filter pores 110, and on the other hand, new chemical pieces can be formed during the compounding process. In detail, dimethylacetamide as a solvent for sulfonated polysulfone can undergo double diffusion (as indicated by thick and thin arrows in fig. 2) and electrostatic adsorption (as indicated by region I in fig. 2) with the surface non-solvent of the inorganic filter substrate 100, thereby making the bonding relationship between the organic coupling layer 330 and the inorganic filter substrate 100 stronger; meanwhile, in the compounding process, the sulfonated polysulfone is also connected with functional groups such as hydroxyl groups on the pore walls of the first filter pores 110 in the inorganic filter matrix 100 in a new chemical bond form (as shown in a region II in FIG. 2), and meanwhile, the organic coupling layer 330 also chelates zirconium metal groups on the surface of the inorganic filter matrix 100 to generate PSF-DMA-ZrO2A composite material. Optionally, the ratio of the sulfonated polysulfone to the dimethylacetamide is 20: 80, in this case, the bonding relationship between the inorganic filter substrate 100 and the organic coupling layer 330 can be more stabilized.
The filtering structural member disclosed by the embodiment of the invention mainly provides a filtering effect in a way of pore interception, physical adsorption and selective combination of partial functional groups, and compared with a conventional inorganic membrane, the filtering structural member disclosed by the embodiment of the invention obviously enhances the hydrophilicity of the material by combining the organic coupling layer 330, and also enhances the anti-pollution capacity of the filtering structural member in the separation process. In addition, the number of functional groups on the surface of the filtering structural member is also obviously increased, and the chelated metal groups can form charge factors through protonation or deprotonation, so that the electric property of the membrane surface is improved, and the filtering performance of the filtering structural member is further improved.
Optionally, in the filtering structural member disclosed in the embodiment of the present invention, the sulfonation degree of the sulfonated polysulfone in the organic coupling layer 330 is 35%, in this case, the number of phosphate groups contained in the sulfonated polysulfone polymer can meet the requirement, and the sulfonated substance has a relatively stable structure and a relatively high performance.
Based on the filter structure disclosed in the above embodiments, as shown in fig. 1 to 5, the present invention further discloses a preparation method for preparing the filter structure disclosed in any of the above embodiments, wherein the preparation method comprises the contents of steps S1 to S4.
S1, obtaining an inorganic filtering matrix 100, wherein the inorganic filtering matrix 100 is provided with a plurality of first filtering holes 110, the pore diameters of the first filtering holes 110 are all less than or equal to 60nm, the inorganic filtering matrix 100 comprises a support body and a membrane layer, and the support body is made of a-Al2O3The material of the film layer is ZrO2。
Specifically, in the inorganic filter substrate 100, the membrane layer is supported on a support to form the inorganic filter substrate 100, and a plurality of first filter holes 110 are formed in both the support and the membrane layer. Alternatively, the inorganic filter substrate 100 is a tubular inorganic ceramic membrane.
S2, obtaining an organic coupling sol 310, wherein the organic coupling sol 310 comprises sulfonated polysulfone and dimethylacetamide. Specifically, the organic coupling sol 310 may be formed by dissolving sulfonated polysulfone into dimethylacetamide. Alternatively, in the process of preparing the organic coupling sol 310, the ratio of the sulfonated polysulfone to the dimethylacetamide may be 20: 80 to ensure that the bonding relationship between the organic coupling sol 310 and the inorganic filter matrix 100 is more stable. It should be noted that there is no sequence relationship between step S1 and step S2, the implementation processes of both may be sequential or may be performed simultaneously, and optionally, step S1 may be performed first, and then step S2 is performed, so as to prevent the organic coupling sol 310 obtained in step S2 from being placed for a long time to generate physical or chemical changes, which affects the normal operation of the subsequent processes of the preparation method, and ensure that the formed filter structure has good filtering performance.
And S3, immersing the inorganic filter matrix 100 into the organic coupling sol 310 by adopting an immersion method, keeping for a preset time, and taking out to obtain a first intermediate product. As above, the organic coupling layer 330 may be formed on the inorganic filter substrate 100 by spraying or brushing. In this embodiment, the organic coupling sol 310 is bonded to the inorganic filtering substrate 100 by using an immersion method, so that on one hand, the organic coupling sol 310 can be covered on the hole wall of each first filtering hole 110 of the inorganic filtering substrate 100, and on the other hand, the bonding time between the organic coupling sol 310 and the inorganic filtering substrate 100 can be increased, so that the organic coupling sol 310 can be better covered in each first filtering hole 110 of the inorganic filtering substrate 100, and the yield is improved. The preset time may be determined according to the proportioning relationship between the sulfonated polysulfone and the dimethylacetamide in the organic coupling sol 310 and actual parameters such as the temperature of the organic coupling sol 310, and more specifically, the preset time may be 10min, which may basically ensure that the organic coupling sol 310 may better cover the hole walls of the first filtering holes 110, and may ensure that the processing efficiency is relatively high.
S4, drying the first intermediate product to obtain a filtering structural member, wherein the filtering structural member is provided with a plurality of second filtering holes 120, and the aperture value of the second filtering holes 120 is 0.8-0.95 times that of the first filtering holes 110.
Specifically, the organic coupling layer 330 may be formed by drying the organic coupling sol 310 by natural drying or baking, and the organic coupling layer 330 is adhered and fixed on the wall of the first filtering hole 110, so as to reduce the aperture of the first filtering hole 110 and form a plurality of second filtering holes 120 with smaller apertures.
Further, the step S2 includes:
s21, under the heating condition, obtaining the organic coupling sol 310, wherein the organic coupling sol 310 comprises sulfonated polysulfone and dimethylacetamide. Specifically, after the sulfonated polysulfone and the dimethylacetamide are put into the batching kettle in a preset ratio, the batching kettle can be heated by adopting a direct heating or water bath heating mode and the like, so that the dissolving rate of the sulfonated polysulfone is increased, and the preparation time of the organic coupling sol 310 is shortened. Further, in the process of preparing the organic coupling sol 310, the preparation efficiency of the organic coupling sol 310 can be further improved by stirring.
Further, the step S21 includes:
s22, under the heating condition of heat conducting oil at the temperature of 80-110 ℃, obtaining the organic coupling sol 310, wherein the organic coupling sol 310 comprises sulfonated polysulfone and dimethylacetamide. That is to say, the ingredient kettle is heated by means of heat conduction oil, on one hand, the heat transfer efficiency of the heat conduction oil is relatively high, and on the other hand, compared with water, the upper limit of the heated temperature of the heat conduction oil is relatively high, so that the heated temperature of the organic coupling sol 310 is higher, the dissolution rate of the sulfonated polysulfone can be further increased, and the preparation time of the organic coupling sol 310 can be further shortened. More specifically, the temperature of the heat transfer oil can be set between 90 ℃ and 100 ℃.
Optionally, between step S22 and step S3, further comprising:
s5, reducing the temperature of the organic coupling sol 310 to 50 ℃, on one hand, preventing the sulfonated polysulfone from being precipitated from dimethylacetamide when the temperature is too low, and on the other hand, preventing the structural strength or chemical properties of the inorganic filter matrix 100 from being affected by the too high temperature of the organic coupling sol 310. Specifically, after the preparation of the organic coupling sol 310 is completed, the temperature of the organic coupling sol 310 may be decreased by adopting a natural cooling manner, and the temperature of the organic coupling sol 310 may be maintained at 50 ℃ by using a heat-conducting oil heating and heat-preserving manner.
Optionally, between step S2 and step S3, further comprising:
s6, performing vacuum defoaming on the organic coupling sol 310, that is, separating bubbles mixed into the organic coupling sol 310 during the preparation of the organic coupling sol 310 by a vacuum defoaming method, which can prevent bubbles from attaching to the inorganic filtering substrate 100 in the process of combining the organic coupling sol 310 and the inorganic filtering substrate 100 due to the presence of the bubbles in the organic coupling sol 310, so that the positions corresponding to the bubbles in the inorganic filtering substrate 100 cannot be covered by the organic coupling sol 310, and further, the organic coupling layer 330 is not attached to the pore walls of some first filtering pores 110 on the formed filtering structural members, so that the filtering performance of the filtering structural members is insufficient.
Optionally, the step S4 includes:
s41, drying the first intermediate product to solidify the organic coupling sol 310 into an organic coupling gel 320, and forming a second intermediate product;
s42, roasting the second intermediate product to obtain a filtering structural member, wherein the filtering structural member is provided with a plurality of second filtering holes 120, and the aperture value of the second filtering holes 120 is 0.8-0.95 times that of the first filtering holes 110.
By adopting the above technical scheme, the drying speed of the first intermediate product can be obviously improved, the production efficiency can be improved, and the situation that the amount of the organic coupling layer 330 combined in the hole wall of each first filtering hole 110 is reduced in the drying process can be further prevented under the condition that the drying time is shortened.
Specifically, after the first intermediate product is obtained, the first intermediate product may be placed in an oven at 150 ℃ for 20min, thereby solidifying the organic coupling sol 310 to form the organic coupling gel 320. And then, placing the second intermediate product in a muffle furnace at 500 ℃ and roasting for 10min in an air atmosphere to form a filter structure, wherein the temperature of the filter structure formed after roasting is relatively high, so that the filter structure can be cooled in a natural cooling mode after being taken out of the muffle furnace.
In the above embodiments of the present invention, the difference between the embodiments is mainly described, and different optimization features between the embodiments can be combined to form a better embodiment as long as they are not contradictory, and further description is omitted here in view of brevity of the text.
The above description is only an example of the present invention, and is not intended to limit the present invention. Various modifications and alterations to this invention will become apparent to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the scope of the claims of the present invention.
Claims (10)
1. A filter structure, comprising an inorganic filter substrate and an organic coupling layer, wherein the filter structure comprises an inorganic filter substrate and an organic coupling layerThe inorganic filter substrate is provided with a plurality of first filter holes, the pore diameters of the first filter holes are less than or equal to 60nm, the inorganic filter substrate comprises a support body and a membrane layer, and the support body is made of α -Al2O3The material of the film layer is ZrO2The organic coupling layer comprises sulfonated polysulfone and dimethylacetamide, the organic coupling layer is arranged on the wall of each first filtering hole to form a plurality of second filtering holes, and the aperture value of each second filtering hole is 0.8-0.95 times that of each first filtering hole.
2. The filter structure of claim 1, wherein the sulfonated polysulfone has a degree of sulfonation of 35%.
3. The filter structure according to claim 1, wherein the inorganic filter matrix is a tubular inorganic ceramic membrane.
4. The filter structure according to claim 1, wherein the ratio of the sulfonated polysulfone to the dimethylacetamide is 20: 80.
5. a method of making a filter structure according to any one of claims 1 to 4, comprising:
obtaining an inorganic filtering substrate, wherein the inorganic filtering substrate is provided with a plurality of first filtering holes, the pore diameters of the first filtering holes are less than or equal to 60nm, the inorganic filtering substrate comprises a support body and a membrane layer, and the support body is made of α -Al2O3The material of the film layer is ZrO2；
Obtaining organic coupling sol, wherein the organic coupling sol comprises sulfonated polysulfone and dimethylacetamide;
immersing the inorganic filtering matrix into the organic coupling sol by adopting an immersion method, keeping the inorganic filtering matrix for a preset time, and taking out the inorganic filtering matrix to obtain a first intermediate product;
and drying the first intermediate product to obtain the filtering structural member, wherein the filtering structural member is provided with a plurality of second filtering holes, and the aperture value of the second filtering holes is 0.8-0.95 times that of the first filtering holes.
6. The method according to claim 5, wherein the obtaining the organically coupled sol comprises:
under the heating condition, obtaining an organic coupling sol, wherein the organic coupling sol comprises sulfonated polysulfone and dimethylacetamide.
7. The method according to claim 6, wherein the obtaining of the organic coupling sol under heating comprises obtaining an organic coupling sol, wherein the organic coupling sol comprises sulfonated polysulfone and dimethylacetamide, and comprises:
under the heating condition of heat conducting oil at the temperature of 80-110 ℃, organic coupling sol is obtained, wherein the organic coupling sol comprises sulfonated polysulfone and dimethylacetamide.
8. The preparation method according to claim 7, wherein the organic coupling sol is obtained under the heating condition of heat conducting oil with the temperature of 80-110 ℃, wherein the organic coupling sol comprises sulfonated polysulfone and dimethylacetamide, and the step of immersing the inorganic filtering substrate into the organic coupling sol by using an immersion method, keeping the immersion method for a preset time and then taking out the inorganic filtering substrate to obtain the first intermediate product further comprises the following steps:
reducing the temperature of the organic coupling sol to 50 ℃.
9. The preparation method according to claim 5, wherein the obtaining of the organic coupling sol, wherein the organic coupling sol comprises sulfonated polysulfone and dimethylacetamide, and the immersing of the inorganic filter substrate into the organic coupling sol by the dipping method, the holding for a predetermined time and the removing, and the obtaining of the first intermediate product further comprises:
and carrying out vacuum defoaming operation on the organic coupling sol.
10. The method of claim 5, wherein the drying the first intermediate product to obtain the filter structure having a plurality of second filter pores having a pore size 0.8 to 0.95 times a pore size of the first filter pores comprises:
drying the first intermediate product to solidify the organic coupling sol into organic coupling gel to form a second intermediate product;
and roasting the second intermediate product to obtain the filtering structural member, wherein the filtering structural member is provided with a plurality of second filtering holes, and the aperture value of the second filtering holes is 0.8-0.95 times of the aperture value of the first filtering holes.
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| US4925566A (en) * | 1986-06-20 | 1990-05-15 | Commissariat A L'energie Atomique | Ultrafiltration, hyperfiltration or demineralization element, its production process and its use for the treatment of liquid radioactive effluents |
| JPH06238140A (en) * | 1993-02-18 | 1994-08-30 | Toto Ltd | Filter membrane |
| US5342521A (en) * | 1990-10-22 | 1994-08-30 | Commissariat A L'energie Atomique | Reverse osmosis or nanofiltration membrane and its production process |
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| CN109304098A (en) * | 2018-10-22 | 2019-02-05 | 南京工业大学 | A kind of preparation method of the compound inner membrance of polymer-ceramic |
| CN212881904U (en) * | 2020-07-17 | 2021-04-06 | 中关村至臻环保股份有限公司 | Filtering structure |
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| US4925566A (en) * | 1986-06-20 | 1990-05-15 | Commissariat A L'energie Atomique | Ultrafiltration, hyperfiltration or demineralization element, its production process and its use for the treatment of liquid radioactive effluents |
| US5342521A (en) * | 1990-10-22 | 1994-08-30 | Commissariat A L'energie Atomique | Reverse osmosis or nanofiltration membrane and its production process |
| JPH06238140A (en) * | 1993-02-18 | 1994-08-30 | Toto Ltd | Filter membrane |
| CN108380064A (en) * | 2018-03-10 | 2018-08-10 | 王金桢 | A kind of preparation method of composite hyperfiltration membrane |
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