CN105289336A - Method for preparing nanofiltration membrane by collectively coating pyrocatechol and polyethyleneimine - Google Patents
Method for preparing nanofiltration membrane by collectively coating pyrocatechol and polyethyleneimine Download PDFInfo
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- CN105289336A CN105289336A CN201510811322.9A CN201510811322A CN105289336A CN 105289336 A CN105289336 A CN 105289336A CN 201510811322 A CN201510811322 A CN 201510811322A CN 105289336 A CN105289336 A CN 105289336A
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Abstract
The present invention relates to a method for preparing a nanofiltration membrane by collectively coating pyrocatechol and polyethyleneimine. The method provided by the present invention aims to solve the problem that the existing preparation nanofiltration membrane industry is complex and unstable in performance and structure. The method comprises the steps of: preparing a polymeric solution, adding a pore-foaming agent, then forming a membrane by using an immersion precipitation phase conversion method and washing the membrane by deionized water to obtain a polymeric initial membrane; preparing a buffer solution and then adding pyrocatechol to obtain a pyrocatechol solution; then adding polytheneimine to obtain a mixed solution B; and and putting the polymer initial membrane into the mixed solution B to leave the membrane to stand so as to obtain the nanofiltration membrane. The nanofiltration membrane prepared by the method provided by the present invention has the advantages that the hydrophilicity is enhanced significantly, the permeation flux is great, and the retention rate of small molecules and inorganic salt is high and the like. Meanwhile, the method is simple in operation and low in cost. The method provided by the present invention is applied to the field of nanofiltration membrane preparation.
Description
Technical field
The present invention relates to a kind of catechol and PEI applies the method preparing NF membrane altogether.
Background technology
NF membrane separation engineering is used widely in each industrial circle and scientific research.The maximum NF membrane of current use is that polyamide composite nanofiltration membrane is prepared by the method for interfacial polymerization.There are some shortcomings in this kind of NF membrane preparation and use procedure, the chemical time be such as designed into is short, is difficult to control; Preparation is complicated, is affected by the external environment large, causes film properties unstable; Layer and basement membrane is selected easily to depart from.Therefore further simple, the performance of research and development preparation and constitutionally stable NF membrane, for the development and application of NF membrane and important.
Nanofiltration separation will produce significant environmental benefit and cost benefit to the removing of inorganic salts in concentrated and purified and industrial wastewater antibiotic in the recovery of the Wastewater Dyes that dyeing produces or removing, pharmaceuticals industry.For processes such as distillation, evaporation, chromatographic isolation, crystallization, absorption, extractions, no matter nanofiltration is the supplementary function alternatively or in a mixed process, all has huge potentiality.Because nanofiltration separation does not relate to phase transformation, do not need heating, avoid the defects such as Small molecular decomposes, while target substance concentration and recovery, the water obtained is recycling again.Therefore development has the solvent resistant NF membrane of good separation performance, substitute huge, the with serious pollution traditional handicraft engineering of some energy consumption with it, and it also there is important meaning to reducing costs, saving energy and reduce the cost, alleviate the aspect such as environmental pollution, raising enterprise competitiveness.
Summary of the invention
The present invention will solve existing preparation NF membrane industry complexity, performance and structural unstable problem, provides a kind of catechol and PEI to apply the method preparing NF membrane altogether.
A kind of catechol of the present invention and PEI apply the method preparing NF membrane altogether, comprise the following steps:
One, take polymer and solvent, be made into the polymer solution that mass fraction is 15% ~ 22%;
Two, in polymer solution, add pore-foaming agent, and be uniformly mixed to dissolving completely, obtain mixed solution A, wherein pore-foaming agent accounts for 0.1% ~ 3% of polymer solution quality;
Three, mixed solution A utilized immersion precipitation phase conversion method to carry out the preparation of film, the film made spends deionized water, obtains the former film of polymer;
Four, secure ph is the cushioning liquid of 8.5, then in cushioning liquid, adds catechol, and being made into concentration is 0.1 ~ 5mgml
-1catechol solution;
Five, in catechol solution, add PEI, obtain mixed solution B; Wherein the mass ratio of catechol and PEI is (0.1 ~ 1): (1 ~ 3);
Six, the former film of polymer step 3 obtained is placed in mixed solution B and leaves standstill 0.5 ~ 24h, obtains NF membrane; Wherein said polymer is polyacrylonitrile, polyimides, polysulfones or polyether sulfone.
The present invention adopts common painting method process to control well, and the coating obtained is relatively more even, the stable performance of gained NF membrane, and the bionical thing coating of the present invention in addition, between the coating obtained and substrate, adhesion is strong, therefore NF membrane Stability Analysis of Structures.Catechol and PEI apply altogether and the aperture of membrane surface are diminished gradually, reach NF membrane pore diameter range; Meanwhile, a large amount of amido not participating in polymerisation in coat makes film surface zeta potential current potential increase, and gives NF membrane and selects layer electropositive, be conducive to retaining of charged ion.The NF membrane that the method obtains not only to Small molecular such as dyestuffs, and all shows good cutoff performance to inorganic salts, has great application prospect.
Accompanying drawing explanation
The infrared spectrum that Fig. 1 is the former film of polyacrylonitrile in embodiment 1, catechol/PEI-600 applies polyacrylonitrile NF membrane altogether; Wherein a is that catechol/PEI-600 applies polyacrylonitrile NF membrane altogether, and b is the former film of polyacrylonitrile;
Fig. 2 is that the NF membrane contact angle of embodiment 1 ~ 3 is with PEI the change of molecular weight figure;
Fig. 3 is the NF membrane performance of embodiment 1 ~ 3 is pure water flux with PEI the change of molecular weight figure, a, and b is MgCl
2rejection, c is OG rejection, and d is CV rejection, and e is BTB rejection.
Detailed description of the invention
Detailed description of the invention one: a kind of catechol of present embodiment and PEI apply the method preparing NF membrane altogether, comprise the following steps:
One, take polymer and solvent, be made into the polymer solution that mass fraction is 15% ~ 22%;
Two, in polymer solution, add pore-foaming agent, and be uniformly mixed to dissolving completely, obtain mixed solution A, wherein pore-foaming agent accounts for 0.1% ~ 3% of polymer solution quality;
Three, mixed solution A utilized immersion precipitation phase conversion method to carry out the preparation of film, the film made spends deionized water, obtains the former film of polymer;
Four, secure ph is the cushioning liquid of 8.5, then in cushioning liquid, adds catechol, and being made into concentration is 0.1 ~ 5mgml
-1catechol solution;
Five, in catechol solution, add PEI, obtain mixed solution B; Wherein the mass ratio of catechol and PEI is (0.1 ~ 1): (1 ~ 3);
Six, the former film of polymer step 3 obtained is placed in mixed solution B and leaves standstill 0.5 ~ 24h, obtains NF membrane; Wherein said polymer is polyacrylonitrile, polyimides, polysulfones or polyether sulfone.
Present embodiment adopts painting method process altogether to control well, and the coating obtained is relatively more even, the stable performance of gained NF membrane, and the bionical thing coating of the present invention in addition, between the coating obtained and substrate, adhesion is strong, therefore NF membrane Stability Analysis of Structures.Catechol and PEI apply altogether and the aperture of membrane surface are diminished gradually, reach NF membrane pore diameter range; Meanwhile, a large amount of amido not participating in polymerisation in coat makes film surface zeta potential current potential increase, and gives NF membrane and selects layer electropositive, be conducive to retaining of charged ion.The NF membrane that the method obtains not only to Small molecular such as dyestuffs, and all shows good cutoff performance to inorganic salts, has great application prospect.
Detailed description of the invention two: present embodiment and detailed description of the invention one unlike: solvent described in step one is N-pyrrolidones, dimethyl sulfoxide (DMSO), DMF or DMA.Other is identical with detailed description of the invention one.
Detailed description of the invention three: present embodiment and detailed description of the invention one or two unlike: the pore-foaming agent described in step 2 is polypyrrole alkane ketone, PEG400 or polyethylene glycol-800.Other is identical with detailed description of the invention one or two.
Detailed description of the invention four: one of present embodiment and detailed description of the invention one to three unlike: in step 3, the film made is spent deionized water 3 ~ 6 times.Other is identical with one of detailed description of the invention one to three.
Detailed description of the invention five: the cushioning liquid that one of present embodiment and detailed description of the invention one to four are 8.5 unlike: the pH value described in step 4 is three (methylol) aminomethane-hydrochloric acid buffer solution.Other is identical with one of detailed description of the invention one to four.
Detailed description of the invention six: one of present embodiment and detailed description of the invention one to five unlike: the molecular weight of the PEI described in step 5 is 600,1800,10000 or 20000.Other is identical with one of detailed description of the invention one to five.
Detailed description of the invention seven: one of present embodiment and detailed description of the invention one to six unlike: be made into the polymer solution that mass fraction is 20% in step one.Other is identical with one of detailed description of the invention one to six.
Detailed description of the invention eight: one of present embodiment and detailed description of the invention one to seven unlike: being made into concentration in step 4 is 3mgml
-1catechol solution.Other is identical with one of detailed description of the invention one to seven.
Detailed description of the invention nine: one of present embodiment and detailed description of the invention one to eight unlike: in step 5, the mass ratio of catechol and PEI is 1:1.Other is identical with one of detailed description of the invention one to eight.
Detailed description of the invention ten: one of present embodiment and detailed description of the invention one to nine are placed in mixed solution B unlike: the former film of polymer step 3 obtained in step 6 and leave standstill 6h.Other is identical with one of detailed description of the invention one to nine.
Beneficial effect of the present invention is verified by following examples:
Embodiment one: a kind of catechol of the present embodiment and PEI apply the method preparing NF membrane altogether, comprise the following steps:
One, take polyacrylonitrile and N-pyrrolidones (NMP), be made into the polyacrylonitrile solution that mass fraction is 20%;
Two, in polyacrylonitrile solution, add polyethylene glycol-800 (PEG-800), and be uniformly mixed to dissolving completely, obtain mixed solution A, wherein PEG-800 accounts for 1% of polyacrylonitrile solution quality;
Three, mixed solution A utilized immersion precipitation phase conversion method to carry out the preparation of film, the film made is spent deionized water 5 times, obtain the former film of polyacrylonitrile;
Four, secure ph is three (methylol) aminomethane-hydrochloric acid buffer solution of 8.5, then in three (methylol) aminomethane-hydrochloric acid buffer solution, adds catechol, and being made into concentration is 3mgml
-1catechol solution;
Five, in catechol solution, add the PEI that molecular weight is 600, obtain mixed solution B; Wherein the mass ratio of catechol and PEI is 1:1;
Six, the former film of polyacrylonitrile step 3 obtained is placed in mixed solution B and leaves standstill 6h, obtains catechol and PEI-600 applies modified polyacrylonitrile NF membrane altogether.
The former film of polyacrylonitrile obtain the present embodiment step 3 and catechol and PEI-600 apply modified polyacrylonitrile NF membrane altogether and carry out infrared figure test.
As shown in Figure 1, from Fig. 1 infrared spectrum test result: compared with the former film of polyacrylonitrile, catechol and PEI-600 apply modified polyacrylonitrile NF membrane at 3400 ~ 3500cm to result altogether
-1the absorption intensity at place strengthens, and this is owing to introducing-OH and-NH functional group in coat; 1655cm simultaneously
-1and 1538cm
-1having there is the characteristic absorption peak of-C=N and-NH in place, shows to there occurs schiff base reaction between catechol and PEI ,-NH simultaneously
2be incorporated in coat.
Embodiment two: a kind of catechol of the present embodiment and PEI apply the method preparing NF membrane altogether, comprise the following steps:
One, take polyacrylonitrile and N-pyrrolidones (NMP), be made into the polyacrylonitrile solution that mass fraction is 20%;
Two, in polyacrylonitrile solution, add polyethylene glycol-800 (PEG-800), and be uniformly mixed to dissolving completely, obtain mixed solution A, wherein PEG-800 accounts for 1% of polyacrylonitrile solution quality;
Three, mixed solution A utilized immersion precipitation phase conversion method to carry out the preparation of film, the film made is spent deionized water 5 times, obtain the former film of polyacrylonitrile;
Four, secure ph is three (methylol) aminomethane-hydrochloric acid buffer solution of 8.5, then in three (methylol) aminomethane-hydrochloric acid buffer solution, adds catechol, and being made into concentration is 3mgml
-1catechol solution;
Five, in catechol solution, add the PEI that molecular weight is 1800, obtain mixed solution B; Wherein the mass ratio of catechol and PEI is 1:1;
Six, the former film of polyacrylonitrile step 3 obtained is placed in mixed solution B and leaves standstill 6h, obtains NF membrane.
Embodiment three: a kind of catechol of the present embodiment and PEI apply the method preparing NF membrane altogether, comprise the following steps:
One, take polyacrylonitrile and N-pyrrolidones (NMP), be made into the polyacrylonitrile solution that mass fraction is 20%;
Two, in polyacrylonitrile solution, add polyethylene glycol-800 (PEG-800), and be uniformly mixed to dissolving completely, obtain mixed solution A, wherein PEG-800 accounts for 1% of polyacrylonitrile solution quality;
Three, mixed solution A utilized immersion precipitation phase conversion method to carry out the preparation of film, the film made is spent deionized water 5 times, obtain the former film of polyacrylonitrile;
Four, secure ph is three (methylol) aminomethane-hydrochloric acid buffer solution of 8.5, then in three (methylol) aminomethane-hydrochloric acid buffer solution, adds catechol, and being made into concentration is 3mgml
-1catechol solution;
Five, in catechol solution, add the PEI that molecular weight is 10000, obtain mixed solution B; Wherein the mass ratio of catechol and PEI is 1:1;
Six, the former film of polyacrylonitrile step 3 obtained is placed in mixed solution B and leaves standstill 6h, obtains NF membrane.
The NF membrane prepare embodiment 1 ~ 3 and the contact angle of the former film of polyacrylonitrile are tested, and test result as shown in Figure 2.
Contact angle determination method is: adopt JC-2000C1 type contact angle instrument to measure the static contact angle of the water on film surface, the film dried is laid on article carrying platform, flatten, then (5.0 μ L) deionized water is dripped on the surface of the film with the wriggling microsyringe that instrument carries, obtain the wetting and spreading state of water on film surface by the image taking instrument of instrument, regulate baseline to make the surface of itself and film in alignment.According to YoungShi wetting theory, adopt equal altitude method to measure contact angle numerical value, each sample at least measures 10 times, and the mean value getting test result is to reduce systematic error.
From Fig. 2 contact angle test result: catechol and PEI apply modified, and the contact angle of film obviously diminishes, and this causes contact angle to diminish owing to introducing hydrophilic amine groups in coat; Meanwhile, film contact angle increases along with the increase of PEI molecular weight, and the PEI of surperficial small-molecular-weight is more conducive to the carrying out applied.
The NF membrane prepare embodiment 1 ~ 3 and the performance of the former film of polyacrylonitrile are tested, and test result as shown in Figure 3.
The assay method of pure water flux is:
The NF membrane sample getting certain area is fixing in nanofiltration stainless steel cup, at room temperature and 0.5MPa (N
2) under with pure water by NF membrane compacting, calculate the permeation flux PWP of NF membrane through pure water after 45min, the calculating formula of PWP is:
PWP＝V/(AtΔP)
In formula, V is infiltration capacity; A is the effective area of film; T is filtration time; Δ P is osmotic pressure.
The rejection assay method of film is:
With NF membrane to magnesium chloride (MgCl
2), the rejection of bromthymol blue (BTB), crystal violet (CV) and acid orange (OG) carrys out the rejection of characterization of membrane.Under the pressure of room temperature and 0.5MPa, filter the MgCl of appropriate concentration
2or dye solution, the rejection R (%) of film is calculated as follows:
R＝1-Cp/Cf
In formula, Cp and Cf represents MgCl in permeate, stoste respectively
2or the concentration of dyestuff.
From Fig. 3 film properties test result: catechol and PEI apply modified, the rejection of film obviously increases, pure water flux reduces simultaneously, this is because coating makes polyacrylonitrile surface fenestra reduce, the introducing of amido simultaneously makes film surface band positive electricity, steric effect and charge effect act on simultaneously, produce effectively retain dye molecule and inorganic ion.NF membrane increases along with the reduction of PEI molecular weight the rejection of dye well inorganic salts, and this is because the polyethylene of small-molecular-weight is more conducive to applying the carrying out reacted.
From the above results, the NF membrane prepared by the present invention has that hydrophily strengthens obviously, permeation flux is large and rejection advantages of higher to Small molecular and inorganic salts.Simultaneously the method is simple to operate, with low cost, in the recovery of the Wastewater Dyes produced at dyeing or removing, pharmaceuticals industry in antibiotic concentrated and purified and industrial wastewater inorganic salts removing etc. in there is important using value.
Although done detailed description to invention above in conjunction with the embodiments, person of ordinary skill in the field can understand, and under the prerequisite not departing from total value of the present invention, in claims, can also change or change etc. to above-described embodiment.
Claims (10)
1. catechol and PEI apply the method preparing NF membrane altogether, it is characterized in that comprising the following steps:
One, take polymer and solvent, be made into the polymer solution that mass fraction is 15% ~ 22%;
Two, in polymer solution, add pore-foaming agent, and be uniformly mixed to dissolving completely, obtain mixed solution A, wherein pore-foaming agent accounts for 0.1% ~ 3% of polymer solution quality;
Three, mixed solution A utilized immersion precipitation phase conversion method to carry out the preparation of film, the film made spends deionized water, obtains the former film of polymer;
Four, secure ph is the cushioning liquid of 8.5, then in cushioning liquid, adds catechol, and being made into concentration is 0.1 ~ 5mgml
-1catechol solution;
Five, in catechol solution, add PEI, obtain mixed solution B; Wherein the mass ratio of catechol and PEI is (0.1 ~ 1): (1 ~ 3);
Six, the former film of polymer step 3 obtained is placed in mixed solution B and leaves standstill 0.5 ~ 24h, obtains NF membrane; Wherein said polymer is polyacrylonitrile, polyimides, polysulfones or polyether sulfone.
2. a kind of catechol according to claim 1 and PEI apply the method preparing NF membrane altogether, it is characterized in that solvent described in step one is N-pyrrolidones, dimethyl sulfoxide (DMSO), DMF or DMA.
3. a kind of catechol according to claim 1 and PEI apply the method preparing NF membrane altogether, it is characterized in that the pore-foaming agent described in step 2 is polypyrrole alkane ketone, PEG400 or polyethylene glycol-800.
4. a kind of catechol according to claim 1 and PEI apply the method preparing NF membrane altogether, it is characterized in that, in step 3, the film made is spent deionized water 3 ~ 6 times.
5. a kind of catechol according to claim 1 and PEI apply the method preparing NF membrane altogether, it is characterized in that the pH value described in step 4 be 8.5 cushioning liquid be three (methylol) aminomethane-hydrochloric acid buffer solution.
6. a kind of catechol according to claim 1 and PEI apply the method preparing NF membrane altogether, it is characterized in that the molecular weight of the PEI described in step 5 is 600,1800,10000 or 20000.
7. a kind of catechol according to claim 1 and PEI apply the method preparing NF membrane altogether, it is characterized in that being made into the polymer solution that mass fraction is 20% in step one.
8. a kind of catechol according to claim 1 and PEI apply the method preparing NF membrane altogether, it is characterized in that being made into concentration in step 4 is 3mgml
-1catechol solution.
9. a kind of catechol according to claim 1 and PEI apply the method preparing NF membrane altogether, it is characterized in that the mass ratio of catechol and PEI in step 5 is 1:1.
10. a kind of catechol according to claim 1 and PEI apply the method preparing NF membrane altogether, it is characterized in that the former film of polymer step 3 obtained in step 6 is placed in mixed solution B and leaves standstill 6h.
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| CN106040011A (en) * | 2016-07-01 | 2016-10-26 | 哈尔滨工业大学宜兴环保研究院 | Method for preparing solvent-resistant nanofiltration membrane by coating catechol and terminal amino polyhedral oligomeric silsesquioxane |
| CN106310977A (en) * | 2016-10-10 | 2017-01-11 | 哈尔滨工业大学宜兴环保研究院 | Method for preparing composite nanofiltration membrane by tannic acid/Fe<3+> cocoating |
| CN107875868A (en) * | 2017-09-26 | 2018-04-06 | 浙江大学 | A kind of alternatively stacked composite nanometer filtering film of phenol amine and preparation method thereof |
| CN108201790A (en) * | 2018-01-05 | 2018-06-26 | 中国科学院宁波材料技术与工程研究所 | A kind of electrostatic spraying prepares the method and its product of NF membrane |
| CN113244786A (en) * | 2021-05-26 | 2021-08-13 | 福建农林大学 | Preparation method of antibacterial nanofiltration membrane based on carbon-loaded cadmium sulfide nano material |
| CN115069099A (en) * | 2022-07-04 | 2022-09-20 | 东华大学 | Preparation method and application of polymer affinity membrane with efficient nucleic acid separation and purification function |
| CN115160639A (en) * | 2022-07-04 | 2022-10-11 | 东华大学 | Preparation method and application of pH-responsive affinity membrane for nucleic acid separation and purification |
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| CN106040011A (en) * | 2016-07-01 | 2016-10-26 | 哈尔滨工业大学宜兴环保研究院 | Method for preparing solvent-resistant nanofiltration membrane by coating catechol and terminal amino polyhedral oligomeric silsesquioxane |
| CN106040011B (en) * | 2016-07-01 | 2018-09-14 | 哈尔滨工业大学宜兴环保研究院 | A kind of catechol and the end amido caged silsesquioxane method that coating prepares solvent resistant NF membrane altogether |
| CN106310977A (en) * | 2016-10-10 | 2017-01-11 | 哈尔滨工业大学宜兴环保研究院 | Method for preparing composite nanofiltration membrane by tannic acid/Fe<3+> cocoating |
| CN107875868A (en) * | 2017-09-26 | 2018-04-06 | 浙江大学 | A kind of alternatively stacked composite nanometer filtering film of phenol amine and preparation method thereof |
| CN108201790A (en) * | 2018-01-05 | 2018-06-26 | 中国科学院宁波材料技术与工程研究所 | A kind of electrostatic spraying prepares the method and its product of NF membrane |
| CN108201790B (en) * | 2018-01-05 | 2019-12-03 | 中国科学院宁波材料技术与工程研究所 | A kind of method and its product of electrostatic spraying preparation nanofiltration membrane |
| CN113244786A (en) * | 2021-05-26 | 2021-08-13 | 福建农林大学 | Preparation method of antibacterial nanofiltration membrane based on carbon-loaded cadmium sulfide nano material |
| CN115069099A (en) * | 2022-07-04 | 2022-09-20 | 东华大学 | Preparation method and application of polymer affinity membrane with efficient nucleic acid separation and purification function |
| CN115160639A (en) * | 2022-07-04 | 2022-10-11 | 东华大学 | Preparation method and application of pH-responsive affinity membrane for nucleic acid separation and purification |
| CN115160639B (en) * | 2022-07-04 | 2023-06-06 | 东华大学 | Preparation method and application of pH responsive affinity membrane for nucleic acid separation and purification |
| CN115069099B (en) * | 2022-07-04 | 2023-09-26 | 东华大学 | Preparation method and application of polymer affinity membrane with efficient nucleic acid separation and purification functions |
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