CN108771979A - A kind of preparation method of chlorine-resistant composite ceramics NF membrane - Google Patents
A kind of preparation method of chlorine-resistant composite ceramics NF membrane Download PDFInfo
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- CN108771979A CN108771979A CN201810548417.XA CN201810548417A CN108771979A CN 108771979 A CN108771979 A CN 108771979A CN 201810548417 A CN201810548417 A CN 201810548417A CN 108771979 A CN108771979 A CN 108771979A
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- 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
- B01D69/12—Composite membranes; Ultra-thin membranes
- B01D69/125—In situ manufacturing by polymerisation, polycondensation, cross-linking or chemical reaction
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- 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
- B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
- B01D61/027—Nanofiltration
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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
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- 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
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/442—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by nanofiltration
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/30—Chemical resistance
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- 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
- C02F2101/10—Inorganic compounds
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- Chemical Kinetics & Catalysis (AREA)
- Nanotechnology (AREA)
- Water Supply & Treatment (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Organic Chemistry (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The present invention provides a kind of preparation method of chlorine-resistant composite ceramics NF membrane, it selects traditional piperazine/pyromellitic trimethylsilyl chloride interfacial polymerization to prepare the excellent nanofiltration membrane of chlorine resistance, and with the excellent macromolecule member material of the chlorine resistance of hydroxyl react using interfacial activity group and form the equally ester group with excellent chlorine-resistant property；Due to the introducing of the excellent macromolecule member material of chlorine resistance, while ensuring that NF membrane is resistant to performance to sodium hypochlorite, the high cutoff performance to inorganic ion is obtained.
Description
Technical field
The present invention relates to technical field of water purification, and in particular to a kind of preparation method of chlorine-resistant composite ceramics NF membrane.
Background technology
Nanofiltration be a kind of performance between ultrafiltration and it is reverse osmosis between pressure-driven membrane separation technique, research starts from 20
Century 70 end.From ultrafiltration and it is reverse osmosis unlike, the separating mechanism of nanofiltration other than nanometer level microporous sieve effect, also
Based on electric charging effect, this is mainly due to nanofiltration film surfaces to carry abundant charge, and it is molten can to act on repulsion by electrostatic repulsion
In liquid with the electrically charged identical ion of institute on film, to have higher selection separation property.The preparation method of NF membrane includes phase
Conversion method, interfacial polymerization, layer assembly method, chemical crosslink technique etc., the NF membrane of mainstream is substantially by interface currently on the market
Polymerization prepares, including polypiperazine-amide nanofiltration membrane and poly aromatic amide NF membrane, wherein polypiperazine-amide nanofiltration membrane
With higher selection separation property, multivalent ion and organic molecule can be retained through most monovalention, be suitable for spy
The fields such as kind separation；And poly aromatic amide NF membrane to comprising including monovalention inorganic salts and organic molecule have it is higher
Removal efficiency, the field having higher requirements to production water inorganic salt content suitable for Treated sewage reusing, wastewater treatment and drink water purifying etc..
In actual use, for achieve the effect that clean water source and reduce membrane biological pollution, membrane separation device front end
Sodium hypochlorite can be used to carry out sterilizing to water inlet, the Active Chlorine thus introduced can generate poly aromatic amide nanofiltration membrane structure
Irreversible destruction, makes film properties decline rapidly and can not be continuing with.Therefore, it to extend the service life of NF membrane, intakes
It also needs to carry out dechlorination processing after sterilization, the requirement of 0.1ppm is less than with contents of residual chlorine in reaching into water, this generic operation is apparent
Increase operating cost, and makes the excessively high risk for destroying NF membrane of residual activity chlorine there are still careless manipulation.If can make
It is standby to obtain the equipment with high desalinization NF membrane with chlorine-resistant property, then Operating Complexity can be effectively reduced, operating cost is reduced；Together
When due to chlorine residue in water inlet presence, can effectively inhibit the quick breeding of bacterium, avoid the biological pollution in film operational process,
Not only it is conducive to the stable operation of system, chemical cleaning number can also be reduced, further decrease system maintenance expense.
Therefore, a kind of chlorine-resistant composite nanometer filtering film is prepared, in Treated sewage reusing, wastewater treatment and is drunk to expanding nanofiltration
Application in the fields such as Water warfare has a very important significance.
Invention content
In order to solve the above technical problems, the present invention provides a kind of preparation method of chlorine-resistant composite ceramics NF membrane, selection is received
Based on filtering ceramic membrane, and the active group at its interface is utilized, further the macromolecule excellent with the chlorine-resistant property containing hydroxyl
Membrane material reacts, and more fine and close separating layer is introduced in a manner of chemical bond, to and meanwhile realize high inorganic salts removal efficiency and excellent
Free chlorine is resistant to performance.
A kind of preparation method of chlorine-resistant composite ceramics NF membrane, is combined by ceramic film and chlorine-resistant separating layer, described
Chlorine-resistant separating layer be by ceramic membrane successively with the aqueous phase solution containing piperazine, the organic phase solution containing pyromellitic trimethylsilyl chloride, contain hydroxyl
The water-soluble polymers that the chlorine resistance of base is excellent contact, and are heat-treated and are prepared.
The macromolecule member material that the chlorine-resistant property of the hydroxyl is excellent is polyvinyl alcohol, sodium alginate, carboxymethyl fibre
It ties up one or more in element, hydroxypropyl cellulose, hydroxyethyl cellulose, sodium lignin sulfonate etc..The hydroxyl it is resistance to
The water-soluble polymers mass concentration of chlorine function admirable is 0.01%~5.0%.
The ceramic membrane is made of the raw material of following parts by weight：120~150 parts of alumina powder, silicon carbide 30~40
Part, 30~40 parts of boron nitride, 70~100 parts of silica, 10~20 parts of antioxidant, 10~30 parts of additive.
The preparation method of the ceramic membrane includes the following steps：
1) each raw material is weighed by the composition of following parts by weight：Alumina powder 120~150,30~40 parts of silicon carbide, nitrogen
Change 30~40 parts of boron, 70~100 parts of silica, 10~20 parts of antioxidant, 10~30 parts of additive；
2) alumina powder, silicon carbide, boron nitride and silica are added in ball mill, through dry mixed ball milling 10-
15 hours, obtain mixed material；
3) by antioxidant, additive mixed grinding to 100-200 mesh, being added, the mixing that step 2) obtains is boring, mixing
It after uniformly, is put into high temperature furnace, in vacuum, tows and be heated to 700-1500 DEG C in atmosphere and be sintered 2-4 hours, near room temperature is
It can.
Further, the additive is any one or more in nano-titanium oxide, nano zine oxide.
Beneficial effects of the present invention are compared with prior art：The present invention selects traditional piperazine/pyromellitic trimethylsilyl chloride circle
Face polymerization prepares the excellent nanofiltration membrane of chlorine resistance, and utilizes the excellent high score of the chlorine resistance of interfacial activity group and hydroxyl
Sub- membrane material carries out reaction and forms the equally ester group with excellent chlorine-resistant property；Due to the excellent macromolecule member material of chlorine resistance
It introduces, while ensuring that NF membrane is resistant to performance to sodium hypochlorite, obtains the high cutoff performance to inorganic ion.
Specific implementation mode
The following is a clear and complete description of the technical scheme in the embodiments of the invention, it is clear that described embodiment
Only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field
The every other embodiment that art personnel are obtained without making creative work belongs to the model that the present invention protects
It encloses.
【Embodiment 1】
The preparation of S1, ceramic membrane：
1) each raw material is weighed by the composition of following parts by weight：120 parts of alumina powder, 40 parts of silicon carbide, boron nitride 300
Part, 70 parts of silica, 10 parts of antioxidant, 30 parts of nano oxidized titanium additives；
2) alumina powder, silicon carbide, boron nitride and silica are added in ball mill, it is small through dry mixed ball milling 15
When, obtain mixed material；
3) by antioxidant, additive mixed grinding to 200 mesh, being added, the mixing that step 2) obtains is boring, is uniformly mixed
Afterwards, it is put into high temperature furnace, in vacuum, tows and be heated to 1500 DEG C in atmosphere and be sintered 4 hours, near room temperature.
S2, chlorine-resistant composite ceramics NF membrane：
The ceramic membrane first prepared by step S1 immerses in the aqueous phase solution of the piperazine containing 0.5wt%, and table is removed with rubber rollers
It is contacted 40 seconds with the organic phase solution of the pyromellitic trimethylsilyl chloride containing 0.2wt% after the extra solution in face, surface is removed with rubber rollers
It contacts 1 minute with the aqueous solution of the polyvinyl alcohol containing 0.5wt% after extra solution, is finally heat-treated in 80 DEG C of baking oven again
5 minutes, obtain chlorine-resistant composite ceramics NF membrane.
【Embodiment 2】
The preparation of S1, ceramic membrane：
1) each raw material is weighed by the composition of following parts by weight：Alumina powder 130,30 parts of silicon carbide, 30 parts of boron nitride,
80 parts of silica, 20 parts of antioxidant, 10 parts of nano oxidized zinc additive；
2) alumina powder, silicon carbide, boron nitride and silica are added in ball mill, it is small through dry mixed ball milling 15
When, obtain mixed material；
3) by antioxidant, additive mixed grinding to 100 mesh, being added, the mixing that step 2) obtains is boring, is uniformly mixed
Afterwards, it is put into high temperature furnace, in vacuum, tows and be heated to 1500 DEG C in atmosphere and be sintered 4 hours, near room temperature.
S2, chlorine-resistant composite ceramics nanofiltration film preparation：
The ceramic membrane first prepared by step S1 immerses in the aqueous phase solution of the piperazine containing 0.5wt%, and table is removed with rubber rollers
It is contacted 40 seconds with the organic phase solution of the pyromellitic trimethylsilyl chloride containing 0.2wt% after the extra solution in face, surface is removed with rubber rollers
It is contacted 1 minute with the aqueous solution of the sodium carboxymethylcellulose containing 1.0wt% again after extra solution, finally in 80 DEG C of baking oven
Heat treatment 5 minutes obtains chlorine-resistant composite ceramics NF membrane.
【Embodiment 3】
The preparation of S1, ceramic membrane：
1) each raw material is weighed by the composition of following parts by weight：Alumina powder 150,35 parts of silicon carbide, 33 parts of boron nitride,
77 parts of silica, 13 parts of antioxidant, 10 parts of nano oxidized titanium additives, 10 parts of nano oxidized zinc additive；
2) alumina powder, silicon carbide, boron nitride and silica are added in ball mill, through dry mixed ball milling 10-
15 hours, obtain mixed material；
3) by antioxidant, additive mixed grinding to 100-200 mesh, being added, the mixing that step 2) obtains is boring, mixing
It after uniformly, is put into high temperature furnace, in vacuum, tows and be heated to 700-1500 DEG C in atmosphere and be sintered 2-4 hours, near room temperature is
It can.
S2, chlorine-resistant composite ceramics nanofiltration film preparation：
The ceramic membrane first prepared by step S1 immerses in the aqueous phase solution of the piperazine containing 0.5wt%, and table is removed with rubber rollers
It is contacted 40 seconds with the organic phase solution of the pyromellitic trimethylsilyl chloride containing 0.2wt% after the extra solution in face, surface is removed with rubber rollers
It is contacted again with the aqueous solution of the sodium lignin sulfonate containing 1.0wt% after extra solution 1 minute, it is finally hot in 80 DEG C of baking oven
Processing 5 minutes obtains chlorine-resistant composite ceramics NF membrane.
【Embodiment 4】
It is resistance to prepared by embodiment 1-3 under conditions of pressure is 0.5MPa, temperature is 25 DEG C, pH value is 7.0~8.0
The chlorine-resistant property of chlorine composite ceramics NF membrane is impregnated centainly by testing the aqueous sodium hypochlorite solution through a concentration of 2000mg/l
Separating property after time is evaluated.
Salt rejection rate (unit after 1 each chlorine-resistant composite ceramics nanofiltration membrane treatment different time of table：%)
Above description has fully disclosed the specific implementation mode of the present invention.It should be pointed out that being familiar with the field
Technical staff is to any change for being done of specific implementation mode of the present invention all without departing from the range of claims of the present invention.
Correspondingly, the scope of the claims of the invention is also not limited only to previous embodiment.
Claims (5)
1. a kind of preparation method of chlorine-resistant composite ceramics NF membrane, is combined by ceramic film and chlorine-resistant separating layer, described
Chlorine-resistant separating layer is by ceramic membrane priority and the aqueous phase solution containing piperazine, the organic phase solution containing pyromellitic trimethylsilyl chloride, hydroxyl
The excellent water-soluble polymers contact of chlorine resistance, and be heat-treated and be prepared；The ceramic membrane is by following weight
The raw material of part is made：120~150 parts of alumina powder, 30~40 parts of silicon carbide, 30~40 parts of boron nitride, silica 70~
100 parts, 10~20 parts of antioxidant, 10~30 parts of additive.
2. the preparation method of chlorine-resistant composite ceramics NF membrane according to claim 1, which is characterized in that the hydroxyl
The excellent macromolecule member material of chlorine-resistant property be polyvinyl alcohol, sodium alginate, carboxymethyl cellulose, hydroxypropyl cellulose, hydroxyl
It is one or more in ethyl cellulose, sodium lignin sulfonate etc..
3. the preparation method of chlorine-resistant composite ceramics NF membrane according to claim 1, which is characterized in that the hydroxyl
The excellent water-soluble polymers mass concentration of chlorine-resistant property be 0.01%~5.0%.
4. the preparation method of chlorine-resistant composite ceramics NF membrane according to claim 1, which is characterized in that the ceramic membrane
Preparation method include the following steps：
1) each raw material is weighed by the composition of following parts by weight：Alumina powder 120~150,30~40 parts of silicon carbide, boron nitride
30~40 parts, 70~100 parts of silica, 10~20 parts of antioxidant, 10~30 parts of additive；
2) alumina powder, silicon carbide, boron nitride and silica are added in ball mill, it is small through dry mixed ball milling 10-15
When, obtain mixed material；
3) by antioxidant, additive mixed grinding to 100-200 mesh, being added, the mixing that step 2) obtains is boring, is uniformly mixed
Afterwards, it is put into high temperature furnace, in vacuum, tows and be heated to 700-1500 DEG C in atmosphere and be sintered 2-4 hours, near room temperature.
5. the preparation method of chlorine-resistant composite ceramics NF membrane according to claim 1, which is characterized in that the additive
For any one or more in nano-titanium oxide, nano zine oxide.
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| CN201810548417.XA CN108771979A (en) | 2018-05-31 | 2018-05-31 | A kind of preparation method of chlorine-resistant composite ceramics NF membrane |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109925892A (en) * | 2019-04-01 | 2019-06-25 | 东华大学 | A kind of small molecule-modified nanofiber-based composite nanometer filtering film and preparation method thereof |
| CN110624276A (en) * | 2019-09-30 | 2019-12-31 | 陈圆圆 | Preparation method of flat composite ceramic membrane for treating oily wastewater |
| CN112058093A (en) * | 2020-09-02 | 2020-12-11 | 蓝星（杭州）膜工业有限公司 | Preparation method of anti-pollution composite nanofiltration membrane with network structure |
| CN117358066A (en) * | 2023-12-07 | 2024-01-09 | 湖南沁森高科新材料有限公司 | Nanofiltration membrane and preparation method thereof |
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| CN107126850A (en) * | 2017-05-23 | 2017-09-05 | 中国石油大学(华东) | A kind of polysulfonamide nanofiltration or reverse osmosis composite membrane and preparation method thereof |
| CN107899434A (en) * | 2017-09-25 | 2018-04-13 | 浙江理工大学 | A kind of preparation method of tight type chlorine-resistant composite nanometer filtering film |
| CN108043236A (en) * | 2017-12-20 | 2018-05-18 | 哈尔滨工业大学 | A kind of new ceramics-polyamide composite nanofiltration membrane and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109925892A (en) * | 2019-04-01 | 2019-06-25 | 东华大学 | A kind of small molecule-modified nanofiber-based composite nanometer filtering film and preparation method thereof |
| CN110624276A (en) * | 2019-09-30 | 2019-12-31 | 陈圆圆 | Preparation method of flat composite ceramic membrane for treating oily wastewater |
| CN112058093A (en) * | 2020-09-02 | 2020-12-11 | 蓝星（杭州）膜工业有限公司 | Preparation method of anti-pollution composite nanofiltration membrane with network structure |
| CN117358066A (en) * | 2023-12-07 | 2024-01-09 | 湖南沁森高科新材料有限公司 | Nanofiltration membrane and preparation method thereof |
| CN117358066B (en) * | 2023-12-07 | 2024-03-19 | 湖南沁森高科新材料有限公司 | Nanofiltration membrane and preparation method thereof |
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