CN110038438A - A kind of preparation method of organo-mineral complexing nanofiltration membrane - Google Patents
A kind of preparation method of organo-mineral complexing nanofiltration membrane Download PDFInfo
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- CN110038438A CN110038438A CN201910274063.9A CN201910274063A CN110038438A CN 110038438 A CN110038438 A CN 110038438A CN 201910274063 A CN201910274063 A CN 201910274063A CN 110038438 A CN110038438 A CN 110038438A
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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
- B01D65/00—Accessories or auxiliary operations, in general, for separation processes or apparatus using semi-permeable membranes
- B01D65/10—Testing of membranes or membrane apparatus; Detecting or repairing leaks
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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
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0083—Thermal after-treatment
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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
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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
- B01D2321/00—Details relating to membrane cleaning, regeneration, sterilization or to the prevention of fouling
- B01D2321/20—By influencing the flow
- B01D2321/2066—Pulsated flow
- B01D2321/2075—Ultrasonic treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2321/00—Details relating to membrane cleaning, regeneration, sterilization or to the prevention of fouling
- B01D2321/28—Details relating to membrane cleaning, regeneration, sterilization or to the prevention of fouling by soaking or impregnating
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Abstract
The invention discloses a kind of preparation methods of organo-mineral complexing nanofiltration membrane, 3- aminopropyl triethoxysilane is grafted on through highly basic activation ceramic membrane, then using piperazine as aqueous phase monomers, using pyromellitic trimethylsilyl chloride as organic phase monomer, it is sour accepting agent with sodium phosphate or organic diamine, organic function layer is formed on the surface of above-mentioned ceramic membrane to get the organo-mineral complexing nanofiltration membrane by interface polymerization reaction in conjunction with additive.The present invention uses inorganic ceramic membrane film to provide enough chemical and thermal stability as the stabilized baseplate of organic nanofiltration membrane, being capable of solvent resistant and high temperature.
Description
Technical field
The invention belongs to nanofiltration membrane preparation technical fields, and in particular to a kind of preparation of organo-mineral complexing nanofiltration membrane
Method.
Background technique
Nanofiltration be a kind of performance between ultrafiltration and it is reverse osmosis between membrane separation technique, can be used in divalent salts and monovalent salt
Separation, research start from late 1970s, be to be grown up by reverse osmosis membrane.Nanofiltration membrane currently on the market is main
It is organic nanofiltration membrane, is cut by electrostatic repulsion effect with steric effect collective effect since film surface is with charge abundant
The ion in solution is stayed, thus selection separation property with higher.Preparation method mainly have phase inversion, interfacial polymerization,
Layer assembly method, chemical crosslink technique etc. obtain nanofiltration membrane currently on the market and are substantially prepared by interfacial polymerization.Currently, organic
Nanofiltration membrane is widely used in concentration and separation, Treated sewage reusing, wastewater treatment and drink water purifying of drug etc., but at present
Organic film some problems existing for liquid in industrial application, such as solvent resistant are poor, are easy to happen swelling and degradation, non-refractory and
It is required that operating condition is high, and main research direction is that using crosslinking agent and the anti-of polymer blended raising nanofiltration membrane is added at present
The stability of solvent borne and film.
Summary of the invention
It is an object of the invention to overcome prior art defect, a kind of preparation of organo-mineral complexing nanofiltration membrane is provided
Method.
Technical scheme is as follows:
A kind of preparation method of organo-mineral complexing nanofiltration membrane, grafted silane is coupled on through highly basic activation ceramic membrane
Agent, using pyromellitic trimethylsilyl chloride as organic phase monomer, connects then using piperazine as aqueous phase monomers using sodium phosphate or organic diamine as acid
By agent, organic function layer is formed on the surface of above-mentioned ceramic membrane to get described organic by interface polymerization reaction in conjunction with additive
Inorganic compound ceramic nanofiltration membrane, the Kong Jingwei 5-50nm of the inorganic functional layer of above-mentioned ceramic membrane, above-mentioned additive are glycerol, second two
At least one of alcohol, polyethylene glycol and Sodium Polyacrylate, the material of above-mentioned ceramic membrane are aluminium oxide or titanium oxide, above-mentioned silane
Coupling agent is 3- aminopropyl triethoxysilane.
In a preferred embodiment of the invention, include the following steps:
(1) by the ceramic membrane it is sonicated after, be soaked in the strong base solution of 0.1-10mol/L and carry out at activation
Reason, is then dried, the ceramic membrane after being activated；
(2) ceramic membrane after activation is soaked in the silane coupler solution that concentration is 1-20mmol/L and reacts 1-10h,
Then it dries, the ceramic membrane after being grafted；
(3) ceramic membrane after grafting is soaked in the organic phase monomer solution that concentration is 0.1-5wt%, at room temperature instead
It answers, removes unreacted organic phase monomer solution, be then soaked in aqueous phase solution, react at room temperature, remove unreacted
Aqueous phase solution, the sour accepting agent and appropriate additive of the aqueous phase monomers containing 1-10wt%, 0.5-5wt% in the aqueous phase solution,
Solvent is water；
(5) it after air-drying step (3) resulting material, is heat-treated in 30-80 DEG C, to get described organic after natural cooling
Inorganic compound ceramic nanofiltration membrane.
It is further preferred that the time of the ultrasonic treatment in the step (1) is 1-10h.
It is further preferred that the time of the activation processing in the step (1) is 1-10h.
It is further preferred that the temperature of the drying in the step (1) is 100-150 DEG C, time 5-15h.
It is further preferred that the temperature of the drying in the step (2) is 100-150 DEG C, time 5-15h.
It is further preferred that the reaction time at room temperature in the step (3) is 1-15min.
In a preferred embodiment of the invention, the highly basic is sodium hydroxide or potassium hydroxide.
The beneficial effects of the present invention are:
1, the present invention uses inorganic ceramic membrane film as the stabilized baseplate of organic nanofiltration membrane, provides enough chemically and thermally steady
It is qualitative, it being capable of solvent resistant and high temperature.
2, the present invention is by preparing organic/inorganic ceramic on being grafted upper 3- aminopropyl triethoxysilane inorganic ceramic membrane
Nanofiltration membrane, under room temperature and the test condition of 0.6MPa, rejection (95- with higher to the Adlerika of 0.2wt%
97%), pure water flux 40-43LHM impregnates at the pH nitric acid solution for being 2 and pH be 12 85 DEG C of sodium hydroxide solution
168h, it is 39-43LHM that its pure water flux is then tested under room temperature and the test condition of 0.6MPa, to the magnesium sulfate of 0.2wt%
Solution retains 93-95.3%, is held essentially constant, and flux of the GE commercialization film DK at 0.76MPa is 27LHM, and acid and alkali-resistance is
PH is 3-9.
Detailed description of the invention
Fig. 1 is the stereoscan photograph of organo-mineral complexing nanofiltration membrane prepared by the embodiment of the present invention 1.
Specific embodiment
Technical solution of the present invention is further explained and described below by way of specific embodiment.
Embodiment 1:
1, membrane tube is handled
It is molten with 1mol/L sodium hydroxide after the 10nm aluminium oxide ceramics membrane tube ultrasound 2h for being 50cm or so by length after cutting
Liquid impregnates 5h, is dried for 24 hours at 100 DEG C, it is molten for the 3- aminopropyl triethoxysilane ethyl alcohol of 2mmol/L that concentration is immersed in after cooling
In liquid, 12h is reacted at room temperature, is then successively rinsed for several times, is put into baking oven with desired temperature with ethyl alcohol and deionized water
Furnace cooling after 150 DEG C of dry 12h
2, nanofiltration film preparation
Step 1, by treated, membrane tube is soaked in the TMC hexane solution that mass fraction is 5wt%, is reacted at room temperature
It is taken out after 3min, carries out the drying of soaked and air gun；
Membrane tube is soaked in the piperazine, 1wt% glycerol and the 1wt% sodium phosphate that are 10wt% containing mass fraction by step 2 again
Aqueous phase solution in, taken out after reacting 3min at room temperature, carry out the drying of soaked and air gun；
Step 3 repeats step 1 and 2
Step 4, membrane tube placed at room temperature air-dry in the cool after be put into 30 DEG C of baking ovens and be heat-treated 15min, Zhi Housui
Furnace is cooling, prepares complete organo-mineral complexing nanofiltration membrane as shown in Figure 1
Membrane tube performance test: under the test condition of room temperature and the pressure of 0.6MPa, pure water flux 43LHM, to 0.2wt%
Adlerika rejection 97%.
Resistance to acid and alkali test: at 85 DEG C, by organo-mineral complexing nanofiltration membrane made from the present embodiment respectively pH be 2
Nitric acid solution and pH be 12 sodium hydroxide solution impregnate 168h after, then in the test condition of room temperature and the pressure of 0.6MPa
Lower its pure water flux of test is that 42.5LHM is held essentially constant the Adlerika rejection 95.3% of 0.2wt%.And GE
Flux of the commercial film DK at 0.76MPa is 27LHM, and the pH of acid and alkali-resistance range is 3-9.
Embodiment 2:
1, membrane tube is handled
After the 50nm titanium oxide ceramics membrane tube ultrasound 2h for being 50cm or so by length after cutting, soaked with 1mol/L potassium hydroxide
10h is steeped, the 3- aminopropyl triethoxysilane ethanol solution for being immersed in that concentration is 5mmol/L after cooling for 24 hours is dried at 100 DEG C
In, 12h is reacted at room temperature, is then successively rinsed for several times, is put into baking oven with desired temperature 150 with ethyl alcohol and deionized water
Furnace cooling after DEG C dry 12h
2, nanofiltration film preparation
Step 1, by treated, membrane tube is soaked in the TMC hexane solution that mass fraction is 1wt%, is reacted at room temperature
It is taken out after 10min, carries out the drying of soaked and air gun；
Membrane tube is soaked in the piperazine, 1wt% ethylene glycol and the 1wt% poly- third that are 5wt% containing mass fraction by step 2 again
It in the aqueous phase solution of olefin(e) acid sodium, is taken out after reacting 10min at room temperature, carries out the drying of soaked and air gun；
Step 3 repeats step 1 and 2
Step 4, membrane tube placed at room temperature air-dry in the cool after be put into 60 DEG C of baking ovens and be heat-treated 15min, Zhi Housui
Furnace is cooling, prepares complete organo-mineral complexing nanofiltration membrane.
Membrane tube performance test: under the test condition of room temperature and the pressure of 0.6MPa, pure water flux 40LHM, to 0.2wt%
Adlerika rejection 95wt%.
Resistance to acid and alkali test: at 85 DEG C, by organo-mineral complexing nanofiltration membrane made from the present embodiment respectively pH be 2
Nitric acid solution and pH be 12 sodium hydroxide solution impregnate 168h after, then in the test condition of room temperature and the pressure of 0.6MPa
Lower its pure water flux of test is that 39.4LHM is held essentially constant the Adlerika rejection 93.2% of 0.2wt%.And GE
Flux of the commercial film DK at 0.76MPa is 27LHM, and the pH of acid and alkali-resistance range is 3-9.
Embodiment 3:
1, membrane tube is handled
After the 5nm titanium oxide ceramics membrane tube ultrasound 5h for being 50cm or so by length after cutting, soaked with 1mol/L sodium hydroxid
10h is steeped, the 3- aminopropyl triethoxysilane ethanol solution for being immersed in that concentration is 10mmol/L after cooling for 24 hours is dried at 100 DEG C
In, 12h is reacted at room temperature, is then successively rinsed for several times, is put into baking oven with desired temperature 150 with ethyl alcohol and deionized water
Furnace cooling after DEG C dry 12h
2, nanofiltration film preparation
Step 1, by treated, membrane tube is soaked in the TMC hexane solution that mass fraction is 0.5wt%, at room temperature instead
It is taken out after answering 15min, carries out the drying of soaked and air gun；
Membrane tube is soaked in gathers containing piperazine, 1wt% polyethylene glycol and the 1wt% that mass fraction is 1wt% again by step 2
It in the aqueous phase solution of sodium acrylate, is taken out after reacting 15min at room temperature, carries out the drying of soaked and air gun；
Step 3 repeats step 1 and 2
Step 4, membrane tube placed at room temperature air-dry in the cool after be put into 80 DEG C of baking ovens and be heat-treated 15min, Zhi Housui
Furnace is cooling, prepares complete organo-mineral complexing nanofiltration membrane.
Membrane tube performance test: under the test condition of room temperature and the pressure of 0.6MPa, pure water flux 42LHM, to 0.2wt%
Adlerika rejection 96.5wt%.
Resistance to acid and alkali test: at 85 DEG C, by organo-mineral complexing nanofiltration membrane made from the present embodiment respectively pH be 2
Nitric acid solution and pH be 12 sodium hydroxide solution impregnate 168h after, then in the test condition of room temperature and the pressure of 0.6MPa
Lower its pure water flux of test is that 41LHM is held essentially constant the Adlerika rejection 94% of 0.2wt%.And GE is commercial
Flux of the film DK at 0.76MPa is 27LHM, and the pH of acid and alkali-resistance range is 3-9.
The foregoing is only a preferred embodiment of the present invention, the range that the present invention that therefore, it cannot be limited according to is implemented, i.e.,
Equivalent changes and modifications made in accordance with the scope of the invention and the contents of the specification should still be within the scope of the present invention.
Claims (8)
1. a kind of preparation method of organo-mineral complexing nanofiltration membrane, it is characterised in that: connect on through highly basic activation ceramic membrane
Branch silane coupling agent, then using piperazine as aqueous phase monomers, using pyromellitic trimethylsilyl chloride as organic phase monomer, with sodium phosphate or organic two
First amine is sour accepting agent, forms organic function layer on the surface of above-mentioned ceramic membrane by interface polymerization reaction in conjunction with additive, i.e.,
Obtain the organo-mineral complexing nanofiltration membrane, the Kong Jingwei 5-50nm of the inorganic functional layer of above-mentioned ceramic membrane, above-mentioned additive
For at least one of glycerol, ethylene glycol, polyethylene glycol and Sodium Polyacrylate, the material of above-mentioned ceramic membrane is aluminium oxide or oxidation
Titanium, above-mentioned silane coupling agent are 3- aminopropyl triethoxysilane.
2. preparation method as described in claim 1, characterized by the following steps:
(1) by the ceramic membrane it is sonicated after, be soaked in the strong base solution of 0.1-10mol/L and be activated, so
After dry, the ceramic membrane after being activated；
(2) ceramic membrane after activation is soaked in the silane coupler solution that concentration is 1-20mmol/L and reacts 1-10h, then
Drying, the ceramic membrane after being grafted；
(3) ceramic membrane after grafting is soaked in the organic phase monomer solution that concentration is 0.1-5wt%, is reacted at room temperature,
Unreacted organic phase monomer solution is removed, is then soaked in aqueous phase solution, reacts at room temperature, removes unreacted water phase
Solution, the sour accepting agent and appropriate additive of the aqueous phase monomers containing 1-10wt%, 0.5-5wt%, solvent in the aqueous phase solution
For water；
(5) it after air-drying step (3) resulting material, is heat-treated in 30-80 DEG C, to get the organic-inorganic after natural cooling
Composite ceramics nanofiltration membrane.
3. preparation method as claimed in claim 2, it is characterised in that: the time of the ultrasonic treatment in the step (1) is 1-
10h。
4. preparation method as claimed in claim 2, it is characterised in that: the time of the activation processing in the step (1) is 1-
10h。
5. preparation method as claimed in claim 2, it is characterised in that: the temperature of the drying in the step (1) is 100-150
DEG C, time 5-15h.
6. preparation method as claimed in claim 2, it is characterised in that: the temperature of the drying in the step (2) is 100-150
DEG C, time 5-15h.
7. preparation method as claimed in claim 2, it is characterised in that: the reaction time at room temperature in the step (3) is
1-15min。
8. the preparation method as described in any claim in claim 1 to 7, it is characterised in that: the highly basic is hydroxide
Sodium or potassium hydroxide.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020200289A1 (en) * | 2019-04-04 | 2020-10-08 | 三达膜科技（厦门）有限公司 | Preparation method for organic-inorganic piperazine polyamide composite ceramic nanofiltration membrane |
| CN111974222A (en) * | 2020-08-25 | 2020-11-24 | 达拉特旗永胜污水处理有限公司 | Regeneration and restoration integration method for industrial waste reverse osmosis membrane |
| CN113797770A (en) * | 2020-06-12 | 2021-12-17 | 三达膜科技（厦门）有限公司 | Dopamine-modified molybdenum oxide-molybdenum disulfide-doped piperazine polyamide composite ceramic nanofiltration membrane and preparation method thereof |
| CN113797766A (en) * | 2020-06-12 | 2021-12-17 | 三达膜科技（厦门）有限公司 | High-flux modified titanium oxide composite ultrafiltration membrane and application thereof |
| CN113797768A (en) * | 2020-06-12 | 2021-12-17 | 三达膜科技（厦门）有限公司 | Molybdenum oxide disulfide doped piperazine polyamide composite ceramic nanofiltration membrane and preparation method thereof |
| CN114130219A (en) * | 2020-09-04 | 2022-03-04 | 三达膜科技（厦门）有限公司 | Titanium dioxide loaded molybdenum disulfide oxide doped piperazine polyamide composite ceramic nanofiltration membrane and preparation method thereof |
| CN115364689A (en) * | 2021-05-21 | 2022-11-22 | 三达膜科技（厦门）有限公司 | Preparation method of ultrathin zirconium oxide-titanium oxide ceramic composite nanofiltration membrane |
| CN115779705A (en) * | 2022-12-27 | 2023-03-14 | 威海智洁环保技术有限公司 | Preparation method and application of polyamide/ceramic composite solvent-resistant nanofiltration membrane |
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| CN113797770A (en) * | 2020-06-12 | 2021-12-17 | 三达膜科技（厦门）有限公司 | Dopamine-modified molybdenum oxide-molybdenum disulfide-doped piperazine polyamide composite ceramic nanofiltration membrane and preparation method thereof |
| CN113797766A (en) * | 2020-06-12 | 2021-12-17 | 三达膜科技（厦门）有限公司 | High-flux modified titanium oxide composite ultrafiltration membrane and application thereof |
| CN113797768A (en) * | 2020-06-12 | 2021-12-17 | 三达膜科技（厦门）有限公司 | Molybdenum oxide disulfide doped piperazine polyamide composite ceramic nanofiltration membrane and preparation method thereof |
| CN113797768B (en) * | 2020-06-12 | 2023-04-14 | 三达膜科技（厦门）有限公司 | Molybdenum disulfide oxide doped piperazine polyamide composite ceramic nanofiltration membrane and preparation method thereof |
| CN111974222A (en) * | 2020-08-25 | 2020-11-24 | 达拉特旗永胜污水处理有限公司 | Regeneration and restoration integration method for industrial waste reverse osmosis membrane |
| CN114130219A (en) * | 2020-09-04 | 2022-03-04 | 三达膜科技（厦门）有限公司 | Titanium dioxide loaded molybdenum disulfide oxide doped piperazine polyamide composite ceramic nanofiltration membrane and preparation method thereof |
| CN114130219B (en) * | 2020-09-04 | 2023-04-14 | 三达膜科技（厦门）有限公司 | Titanium dioxide-loaded molybdenum oxide disulfide-doped piperazine polyamide composite ceramic nanofiltration membrane and preparation method thereof |
| CN115364689A (en) * | 2021-05-21 | 2022-11-22 | 三达膜科技（厦门）有限公司 | Preparation method of ultrathin zirconium oxide-titanium oxide ceramic composite nanofiltration membrane |
| CN115364689B (en) * | 2021-05-21 | 2024-07-19 | 三达膜科技（厦门）有限公司 | Preparation method of ultrathin zirconia-titania ceramic composite nanofiltration membrane |
| CN115779705A (en) * | 2022-12-27 | 2023-03-14 | 威海智洁环保技术有限公司 | Preparation method and application of polyamide/ceramic composite solvent-resistant nanofiltration membrane |
| CN115779705B (en) * | 2022-12-27 | 2024-03-26 | 威海智洁环保技术有限公司 | Preparation method and application of polyamide/ceramic composite solvent-resistant nanofiltration membrane |
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