CN105032204B - A kind of preparation method of titania modified polypyrrole composite nanometer filtering film - Google Patents
A kind of preparation method of titania modified polypyrrole composite nanometer filtering film Download PDFInfo
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Abstract
A kind of preparation method of titania modified polypyrrole composite nanometer filtering film, the present invention relates to a kind of preparation method of NF membrane.The present invention is to solve low and cutoff performance difference the problem of nanofiltration membrane flux prepared by existing method, method is：Polyacrylonitrile solution is prepared, polyacrylonitrile basement membrane, the polyacrylonitrile basement membrane after preparation treatment is prepared, prepare the ultrafiltration membranes containing pyrroles's titanium dioxide, composite nanometer filtering film crude product is prepared, is immersed in ethanol water, obtain titania modified polypyrrole composite nanometer filtering film.The present invention uses titania modified polypyrrole composite nanometer filtering film, its hydrophily is set effectively to be regulated and controled, improve the stability of film, the permeation flux of film is greatly improved, the NF membrane for obtaining has good separating property, and the present invention is applied to separation, concentration of juices and the water desalination field of antibiotic.
Description
Technical field
The present invention relates to a kind of preparation method of NF membrane.
Background technology
Water as life on earth necessity, the also most basic key element of human survival.Water resource is not only relevant
The people's livelihood matter of fundamental importance, equally restricts the sustainable development of this global economy.Therefore, the control of water resources problems is that the earth seeks existence
Necessary condition, equally governs China and builds economizing type, friendly society.Well imagine, the reuse of water resource and purifying problem
It is urgently to be resolved hurrily.
Membrane separation technique be a physics without phase transition process, in terms of water process have many advantages.Therefore, in recent years,
Application of the membrane separation technique in water process is more and more extensive, is paid close attention to by universal.Milipore filter (ultrafiltration
Membranes), NF membrane (nanofiltration membranes), reverse osmosis membrane (reverse osmosis
) and the membrane technology such as membrane bioreactor is in large-scale reclaimed water recycling engineering, Seawater Desalination Project, drink membranes
More and more favored with engineering of water treatment.
In recent years, the NF membrane in organic solvent environment is applied just to be subject to the extensive concern in the fields such as medicine, catalysis.By
It is not related to phase transformation in nanofiltration separation process, it is possible to reduce traditional method of purification brings the damage of active ingredient due to temperature change
Lose, and recovered solvent can reach the level of recycling, reduce due to body eutrophication that solvent discharge brings etc.
Pollution.But used in the case where high concentration obtains organic solvent environment, the requirement to membrane material is also higher.Therefore, it is adaptable to this ring
The developmental research of the nanofiltration membrane material under border turns into wide concerned problem.
The content of the invention
The present invention is to solve low and cutoff performance difference the problem of nanofiltration membrane flux prepared by existing method, there is provided a kind of two
The preparation method of titanium oxide modified polypyrrole composite nanometer filtering film.
A kind of preparation method of titania modified polypyrrole composite nanometer filtering film of the present invention, it is characterised in that the method includes
Following steps：
First, solvent, pore former and polyacrylonitrile are mixed, polyacrylonitrile solution is obtained；
2nd, polyacrylonitrile solution is made ultrafiltration membranes, deionized water washing 3~5 using submergence-precipitation phase inversion
It is secondary, obtain polyacrylonitrile basement membrane；
3rd, polyacrylonitrile basement membrane is placed in sodium hydroxide solution, 20min~60min is reacted at 20 DEG C~50 DEG C, instead
After should terminating, polyacrylonitrile basement membrane is taken out, be put into 0.5~2h of soaking and washing in deionized water, then be placed in leaching in hydrochloric acid solution
1~5h of bubble, the polyacrylonitrile basement membrane after being processed；
4th, in the polyacrylonitrile basement membrane immersion pyrroles-titanium dioxide-ethanol solution after step 3 is processed, immersion 60~
180min, is then taken out, and the ultrafiltration membranes containing pyrroles-titanium dioxide are obtained after drying；Wherein pyrroles-titanium dioxide-ethanol
The mass concentration of pyrroles is 5% in solution, and the mass concentration of titanium dioxide is 0.025%~0.2%；
5th, the ultrafiltration membranes containing pyrroles-titanium dioxide are placed in strong oxidant solution, soak 110~130min, taken
Dried after going out, obtain composite nanometer filtering film crude product；
6th, in being 70%~100% ethanol water by composite nanometer filtering film crude product immersion mass fraction, immersion 0.5h~
100h, obtains titania modified polypyrrole composite nanometer filtering film after taking-up.
The present invention uses titania modified polypyrrole composite nanometer filtering film, its hydrophily is effectively regulated and controled, and improves
The stability of film, the permeation flux of film is greatly improved.The NF membrane for obtaining has good separating property, it is adaptable to
The separation of various dyestuffs, antibiotic, desalinization etc., there is great application prospect.
Brief description of the drawings
Fig. 1 is the SEM photograph of titania modified polypyrrole composite nanometer filtering film prepared by embodiment 1；
Fig. 2 is the SEM photograph of titania modified polypyrrole composite nanometer filtering film prepared by embodiment 2；
Fig. 3 is the infrared spectrum of titania modified polypyrrole composite nanometer filtering film prepared by embodiment 3；
Fig. 4 is titania modified polypyrrole composite nanometer filter membrane flux and rejection test result prepared by embodiment 1~5
Figure；Wherein a is the flux of isopropanol；B is the flux of ethanol；C is the flux of tetrahydrofuran；D is the flux of acetone；E is methyl alcohol
Flux；F is the rejection of light blue；G is the rejection of RB, and Mem-6 is embodiment 1, and Mem-7 is embodiment 2,
Mem-8 is embodiment 3, and Mem-9 is embodiment 4, and Mem-10 is embodiment 5.
Specific embodiment
Specific embodiment one：A kind of preparation method of titania modified polypyrrole composite nanometer filtering film of present embodiment,
It is characterized in that the method is comprised the following steps：
First, solvent, pore former and polyacrylonitrile are mixed, polyacrylonitrile solution is obtained；
2nd, polyacrylonitrile solution is made ultrafiltration membranes, deionized water washing 3~5 using submergence-precipitation phase inversion
It is secondary, obtain polyacrylonitrile basement membrane；
3rd, polyacrylonitrile basement membrane is placed in sodium hydroxide solution, 20min~60min is reacted at 20 DEG C~50 DEG C, instead
After should terminating, polyacrylonitrile basement membrane is taken out, be put into 0.5~2h of soaking and washing in deionized water, then be placed in leaching in hydrochloric acid solution
1~5h of bubble, the polyacrylonitrile basement membrane after being processed；
4th, in the polyacrylonitrile basement membrane immersion pyrroles-titanium dioxide-ethanol solution after step 3 is processed, immersion 60~
180min, is then taken out, and the ultrafiltration membranes containing pyrroles-titanium dioxide are obtained after drying；Wherein pyrroles-titanium dioxide-ethanol
The mass concentration of pyrroles is 5% in solution, and the mass concentration of titanium dioxide is 0.025%~0.2%；
5th, the ultrafiltration membranes containing pyrroles-titanium dioxide are placed in strong oxidant solution, soak 110~130min, taken
Dried after going out, obtain composite nanometer filtering film crude product；
6th, in being 70%~100% ethanol water by composite nanometer filtering film crude product immersion mass fraction, immersion 0.5h~
100h, obtains titania modified polypyrrole composite nanometer filtering film after taking-up.
Present embodiment uses titania modified polypyrrole composite nanometer filtering film, its hydrophily is effectively regulated and controled,
The stability of film is improved, the permeation flux of film is greatly improved.The NF membrane for obtaining has good separating property, fits
For various dyestuffs, the separation of antibiotic, desalinization etc., there is great application prospect.
Specific embodiment two：Present embodiment from unlike specific embodiment one：Solvent described in step one is
1-METHYLPYRROLIDONE.Other are identical with specific embodiment one.
Specific embodiment three：Present embodiment and the pore-forming described in step one unlike specific embodiment one or two
Agent is polyethylene glycol or polyvinylpyrrolidone.Other are identical with specific embodiment one or two.
Specific embodiment four：Unlike one of present embodiment and specific embodiment one to three：Gather in step one
The mass ratio of acrylonitrile, pore former and solvent is (15~25):1:(74~84).Other are one of with specific embodiment one to three
It is identical.
Specific embodiment five：Unlike one of present embodiment and specific embodiment one to four：Described in step 3
React 30min at 40 DEG C.Other are identical with one of specific embodiment one to four.
Specific embodiment six：Unlike one of present embodiment and specific embodiment one to five：Described in step 3
Sodium hydroxide solution mass concentration be 5%~20%.Other are identical with one of specific embodiment one to five.
Specific embodiment seven：Unlike one of present embodiment and specific embodiment one to six：Described in step 3
Hydrochloric acid solution concentration be 0.05mol/L~0.5mol/L.Walk other identical with one of specific embodiment one to six.
Specific embodiment eight：Unlike one of present embodiment and specific embodiment one to seven：Described in step 5
Strong oxidant solution for concentration 1.0mol/L ammonium persulfate solution.Other are identical with one of specific embodiment one to seven.
Specific embodiment nine：Unlike one of present embodiment and specific embodiment one to eight：Soaked in step 5
Bubble 120min.Other are identical with one of specific embodiment one to eight.
Specific embodiment ten：Unlike one of present embodiment and specific embodiment one to nine：Soaked in step 6
Bubble 4h.Other are identical with one of specific embodiment one to nine.
The following examples will be further described to the present invention, but not thereby limiting the invention.
Embodiment 1：The preparation method of the titania modified polypyrrole composite nanometer filtering film of the present embodiment, comprises the following steps：
First, by 79g N-methyls pyrrolidones and 1g polyethylene glycol, add in 20g polyacrylonitrile, polyacrylonitrile is obtained molten
Liquid；
2nd, polyacrylonitrile solution is made ultrafiltration membranes using submergence-precipitation phase inversion, deionized water is washed 5 times, obtained
To polyacrylonitrile basement membrane；
3rd, polyacrylonitrile basement membrane is placed in the sodium hydroxide solution that mass concentration is 10%, is reacted at 40 DEG C
30min, after reaction terminates, polyacrylonitrile basement membrane is taken out, and is put into soaking and washing 0.5h in deionized water, then be placed in 0.1mol/L
3h is soaked in hydrochloric acid solution, the polyacrylonitrile basement membrane after being processed；
4th, in the polyacrylonitrile basement membrane immersion pyrroles-titanium dioxide-ethanol solution after step 3 is processed, immersion
180min, is then taken out, and the ultrafiltration membranes containing pyrroles-titanium dioxide are obtained after drying；Wherein pyrroles-titanium dioxide-ethanol
The mass concentration of pyrroles is 5% in solution, and the mass concentration of titanium dioxide is 0.025%；
5th, the ultrafiltration membranes containing pyrroles-titanium dioxide are placed in the ammonium persulfate solution of concentration 1.0mol/L, are soaked
120min, dries after taking-up, obtains composite nanometer filtering film crude product；
6th, in being 70% ethanol water by composite nanometer filtering film crude product immersion mass fraction, 4h is soaked, is obtained after taking-up
Titania modified polypyrrole composite nanometer filtering film.
The SEM photograph of titania modified polypyrrole composite nanometer filtering film manufactured in the present embodiment is as shown in figure 1, can by Fig. 1
Know, modified titanium dioxide is good with the compatibility of basement membrane, thus tends to be laid in the surface of film, and in Surface Creation
Some short grained surfaces are mellow and full.
The preparation method of the titania modified polypyrrole composite nanometer filtering film of embodiment 2, the present embodiment, comprises the following steps：
First, by 79g N-methyls pyrrolidones and 1g polyethylene glycol, add in 20g polyacrylonitrile, polyacrylonitrile is obtained molten
Liquid；
2nd, polyacrylonitrile solution is made ultrafiltration membranes using submergence-precipitation phase inversion, deionized water is washed 5 times, obtained
To polyacrylonitrile basement membrane；
3rd, polyacrylonitrile basement membrane is placed in the sodium hydroxide solution that mass concentration is 10%, is reacted at 40 DEG C
30min, after reaction terminates, polyacrylonitrile basement membrane is taken out, and is put into soaking and washing 0.5h in deionized water, then be placed in 0.1mol/L
3h is soaked in hydrochloric acid solution, the polyacrylonitrile basement membrane after being processed；
4th, in the polyacrylonitrile basement membrane immersion pyrroles-titanium dioxide-ethanol solution after step 3 is processed, immersion
180min, is then taken out, and the ultrafiltration membranes containing pyrroles-titanium dioxide are obtained after drying；Wherein pyrroles-titanium dioxide-ethanol
The mass concentration of pyrroles is 5% in solution, and the mass concentration of titanium dioxide is 0.05%；
5th, the ultrafiltration membranes containing pyrroles-titanium dioxide are placed in the ammonium persulfate solution of concentration 1.0mol/L, are soaked
120min, dries after taking-up, obtains composite nanometer filtering film crude product；
6th, in being 70% ethanol water by composite nanometer filtering film crude product immersion mass fraction, 4h is soaked, is obtained after taking-up
Titania modified polypyrrole composite nanometer filtering film.
The SEM photograph of titania modified polypyrrole composite nanometer filtering film manufactured in the present embodiment is as shown in Fig. 2 can by Fig. 2
Know, modified titanium dioxide is good with the compatibility of basement membrane, thus tends to be laid in the surface of film, and in Surface Creation
Some short grained surfaces are mellow and full.
The preparation method of the titania modified polypyrrole composite nanometer filtering film of embodiment 3, the present embodiment, comprises the following steps：
First, by 79g N-methyls pyrrolidones and 1g polyethylene glycol, add in 20g polyacrylonitrile, polyacrylonitrile is obtained molten
Liquid；
2nd, polyacrylonitrile solution is made ultrafiltration membranes using submergence-precipitation phase inversion, deionized water is washed 5 times, obtained
To polyacrylonitrile basement membrane；
3rd, polyacrylonitrile basement membrane is placed in the sodium hydroxide solution that mass concentration is 10%, is reacted at 40 DEG C
30min, after reaction terminates, polyacrylonitrile basement membrane is taken out, and is put into soaking and washing 0.5h in deionized water, then be placed in 0.1mol/L
3h is soaked in hydrochloric acid solution, the polyacrylonitrile basement membrane after being processed；
4th, in the polyacrylonitrile basement membrane immersion pyrroles-titanium dioxide-ethanol solution after step 3 is processed, immersion
180min, is then taken out, and the ultrafiltration membranes containing pyrroles-titanium dioxide are obtained after drying；Wherein pyrroles-titanium dioxide-ethanol
The mass concentration of pyrroles is 5% in solution, and the mass concentration of titanium dioxide is 0.075%；
5th, the ultrafiltration membranes containing pyrroles-titanium dioxide are placed in the ammonium persulfate solution of concentration 1.0mol/L, are soaked
120min, dries after taking-up, obtains composite nanometer filtering film crude product；
6th, in being 70% ethanol water by composite nanometer filtering film crude product immersion mass fraction, 4h is soaked, is obtained after taking-up
Titania modified polypyrrole composite nanometer filtering film.
The infrared spectrum of titania modified polypyrrole composite nanometer filtering film manufactured in the present embodiment is as shown in figure 3, can by Fig. 3
Know, the stretching vibration peak of infrared spectrogram C=C and C-C in 1531cm-1 and 1440cm-1 are respectively pyrrole ring；1277cm-
1,1136cm-1, and 1016cm-1 is the=in-plane bending vibration peak of C-H ,=C-H out-of-plane bending vibrations peak is that 904cm-1 is attached
Closely.It is all the feature stretching vibration peak of pyrrole ring.Meanwhile, the characteristic absorption peak of carbonyl is also occurred in that at 1690cm-1.
The preparation method of the titania modified polypyrrole composite nanometer filtering film of embodiment 4, the present embodiment, comprises the following steps：
First, by 79g N-methyls pyrrolidones and 1g polyethylene glycol, add in 20g polyacrylonitrile, polyacrylonitrile is obtained molten
Liquid；
2nd, polyacrylonitrile solution is made ultrafiltration membranes using submergence-precipitation phase inversion, deionized water is washed 5 times, obtained
To polyacrylonitrile basement membrane；
3rd, polyacrylonitrile basement membrane is placed in the sodium hydroxide solution that mass concentration is 10%, is reacted at 40 DEG C
30min, after reaction terminates, polyacrylonitrile basement membrane is taken out, and is put into soaking and washing 0.5h in deionized water, then be placed in 0.1mol/L
3h is soaked in hydrochloric acid solution, the polyacrylonitrile basement membrane after being processed；
4th, in the polyacrylonitrile basement membrane immersion pyrroles-titanium dioxide-ethanol solution after step 3 is processed, immersion
180min, is then taken out, and the ultrafiltration membranes containing pyrroles-titanium dioxide are obtained after drying；Wherein pyrroles-titanium dioxide-ethanol
The mass concentration of pyrroles is 5% in solution, and the mass concentration of titanium dioxide is 0.1%；
5th, the ultrafiltration membranes containing pyrroles-titanium dioxide are placed in the ammonium persulfate solution of concentration 1.0mol/L, are soaked
120min, dries after taking-up, obtains composite nanometer filtering film crude product；
6th, in being 70% ethanol water by composite nanometer filtering film crude product immersion mass fraction, 4h is soaked, is obtained after taking-up
Titania modified polypyrrole composite nanometer filtering film.
The preparation method of the titania modified polypyrrole composite nanometer filtering film of embodiment 5, embodiment, comprises the following steps：
First, by 79g N-methyls pyrrolidones and 1g polyethylene glycol, add in 20g polyacrylonitrile, polyacrylonitrile is obtained molten
Liquid；
2nd, polyacrylonitrile solution is made ultrafiltration membranes using submergence-precipitation phase inversion, deionized water is washed 5 times, obtained
To polyacrylonitrile basement membrane；
3rd, polyacrylonitrile basement membrane is placed in the sodium hydroxide solution that mass concentration is 10%, is reacted at 40 DEG C
30min, after reaction terminates, polyacrylonitrile basement membrane is taken out, and is put into soaking and washing 0.5h in deionized water, then be placed in 0.1mol/L
3h is soaked in hydrochloric acid solution, the polyacrylonitrile basement membrane after being processed；
4th, in the polyacrylonitrile basement membrane immersion pyrroles-titanium dioxide-ethanol solution after step 3 is processed, immersion
180min, is then taken out, and the ultrafiltration membranes containing pyrroles-titanium dioxide are obtained after drying；Wherein pyrroles-titanium dioxide-ethanol
The mass concentration of pyrroles is 5% in solution, and the mass concentration of titanium dioxide is 0.2%；
5th, the ultrafiltration membranes containing pyrroles-titanium dioxide are placed in the ammonium persulfate solution of concentration 1.0mol/L, are soaked
120min, dries after taking-up, obtains composite nanometer filtering film crude product；
6th, in being 70% ethanol water by composite nanometer filtering film crude product immersion mass fraction, 4h is soaked, is obtained after taking-up
Titania modified polypyrrole composite nanometer filtering film.
Organic solvent permeation flux is tested：After the NF membrane that will be prepared is cut into the circle of suitable size, self-control is put into
Dead end nanofiltration cup in, nanofiltration cup effective infiltrating area be 21.2cm2.Organic solvent wherein used include isopropanol (IPA),
Ethanol (EtOH), methyl alcohol (MEK), acetone (DMK), tetrahydrofuran (THF).
Rejection is tested：Carry out the retention of characterization of membrane to the rejection of RB (RB), light blue (BB) with NF membrane
Property, the molecular weight of RB is~1018, molecular weight~793 of light blue.
Titania modified polypyrrole composite nanometer filter membrane flux prepared by embodiment 1~5 is with rejection test result figure such as
Shown in Fig. 4, wherein a is the flux of isopropanol；B is the flux of ethanol；C is the flux of tetrahydrofuran；D is the flux of acetone；E is
The flux of methyl alcohol；F is the rejection of light blue；G is the rejection of RB.As shown in Figure 4, titanium dioxide is added first
The order that the solvent resistant NF membrane of titanium is descending to the permeation flux of five kinds of organic solvents is methyl alcohol, acetone, tetrahydrofuran, second
Alcohol and isopropanol.The size for illustrating permeation flux is correct by the conclusion that molecule free volume and viscosity size are determined.However,
Permeation flux of the compound solvent resistant NF membrane to organic solvent and the rejection to two kinds of dyestuffs that with the addition of titanium dioxide exist
Content of titanium dioxide reaches maximum when being 0.075%, the flux of isopropanol is 3.57, and the flux of ethanol is 5.02, tetrahydrochysene furan
The flux muttered is 9.46, and the flux of acetone is 12.63, and the flux of methyl alcohol is 17.59, and the rejection of light blue is 89.67, Bangladesh
The rejection of rose-red is 97.89.The reason for producing this phenomenon is that after being modified to titanium dioxide, its dispersive property becomes
It is good and stronger with the active force of basement membrane and pyrrole monomer.This inhibits diffusion of the pyrrole monomer to solution on the one hand, reduces
The generation of oligomer, forms more small structures, so as to increased the permeation flux and rejection of organic solvent.When two
When titanium oxide content continues to increase, reunite more serious, but the chemical group existed due to its surface effect, to pyrrole monomer
It is still very strong with the sucking action of polypyrrole strand, but be affected with the electron transmission of polypyrrole, therefore simply reduce
Defect and to producing more apertures not promote, therefore flux generates decline with rejection.
Embodiment 1~5 uses titania modified polypyrrole composite nanometer filtering film, its hydrophily is effectively regulated and controled,
The stability of film is improved, the permeation flux of film is greatly improved, and the NF membrane for obtaining has good separating property, fitted
For various dyestuffs, the separation of antibiotic, desalinization etc., there is great application prospect.
Claims (8)
1. a kind of preparation method of titania modified polypyrrole composite nanometer filtering film, it is characterised in that the method includes following step
Suddenly：
First, solvent, pore former and polyacrylonitrile are mixed, polyacrylonitrile solution is obtained；
2nd, polyacrylonitrile solution is made ultrafiltration membranes using submergence-precipitation phase inversion, deionized water is washed 3~5 times, obtained
To polyacrylonitrile basement membrane；
3rd, polyacrylonitrile basement membrane is placed in sodium hydroxide solution, 20min~60min, reaction knot is reacted at 20 DEG C~50 DEG C
Shu Hou, polyacrylonitrile basement membrane is taken out, and is put into 0.5~2h of soaking and washing in deionized water, then be placed in immersion 1 in hydrochloric acid solution~
5h, the polyacrylonitrile basement membrane after being processed；
4th, in the polyacrylonitrile basement membrane immersion pyrroles-titanium dioxide-ethanol solution after step 3 is processed, immersion 60~
180min, is then taken out, and the ultrafiltration membranes containing pyrroles-titanium dioxide are obtained after drying；Wherein pyrroles-titanium dioxide-ethanol
The mass concentration of pyrroles is 5% in solution, and the mass concentration of titanium dioxide is 0.025%~0.2%；
5th, the ultrafiltration membranes containing pyrroles-titanium dioxide are placed in strong oxidant solution, 110~130min are soaked, after taking-up
Dry, obtain composite nanometer filtering film crude product；
6th, in being 70%~100% ethanol water by composite nanometer filtering film crude product immersion mass fraction, immersion 0.5h~
100h, obtains titania modified polypyrrole composite nanometer filtering film after taking-up；Solvent described in step one is 1-METHYLPYRROLIDONE；
Pore former described in step one is polyethylene glycol or polyvinylpyrrolidone.
2. a kind of preparation method of titania modified polypyrrole composite nanometer filtering film according to claim 1, its feature exists
The mass ratio of polyacrylonitrile, pore former and solvent is (15~25) in step one:1:(74~84).
3. a kind of preparation method of titania modified polypyrrole composite nanometer filtering film according to claim 1, its feature exists
In reacting 30min at 40 DEG C described in step 3.
4. a kind of preparation method of titania modified polypyrrole composite nanometer filtering film according to claim 1, its feature exists
In the sodium hydroxide solution described in step 3 mass concentration be 5%~20%.
5. a kind of preparation method of titania modified polypyrrole composite nanometer filtering film according to claim 1, its feature exists
In the hydrochloric acid solution described in step 3 concentration be 0.05mol/L~0.5mol/L.
6. a kind of preparation method of titania modified polypyrrole composite nanometer filtering film according to claim 1, its feature exists
In the ammonium persulfate solution that the strong oxidant solution described in step 5 is 0.5~1.2mol/L of concentration.
7. a kind of preparation method of titania modified polypyrrole composite nanometer filtering film according to claim 1, its feature exists
120min is soaked in step 5.
8. a kind of preparation method of titania modified polypyrrole composite nanometer filtering film according to claim 1, its feature exists
4h is soaked in step 6.
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| CN108704481B (en) * | 2018-05-29 | 2023-09-12 | 华北电力大学（保定） | Preparation method of polypyrrole/nano metal crystal/high polymer nanofiltration conductive film |
| CN108722203B (en) * | 2018-05-30 | 2021-04-16 | 哈尔滨工业大学（威海） | Preparation method of high-flux polyaniline composite nanofiltration membrane |
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| CN1903417A (en) * | 2006-07-14 | 2007-01-31 | 哈尔滨工业大学 | Titanium dioxide granule modified aromatic polyamide separation film and its prepn. method |
| CN103285741A (en) * | 2013-05-20 | 2013-09-11 | 哈尔滨工业大学 | Preparation method of solvent-resistant compound nanofiltration membrane |
| CN104316573A (en) * | 2014-10-24 | 2015-01-28 | 浙江大学 | Polypyrrole/titanium dioxide composite impedance film gas sensor and preparation method thereof |
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| CN1903417A (en) * | 2006-07-14 | 2007-01-31 | 哈尔滨工业大学 | Titanium dioxide granule modified aromatic polyamide separation film and its prepn. method |
| CN103285741A (en) * | 2013-05-20 | 2013-09-11 | 哈尔滨工业大学 | Preparation method of solvent-resistant compound nanofiltration membrane |
| CN104316573A (en) * | 2014-10-24 | 2015-01-28 | 浙江大学 | Polypyrrole/titanium dioxide composite impedance film gas sensor and preparation method thereof |
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