Preparation method of polymer-based nano composite ultrafiltration membrane

Abstract

The invention discloses a preparation method of a polymer-based nano composite ultrafiltration membrane, and belongs to the field of membrane material preparation. The preparation method mainly comprises the steps: a hydrophobic polyvinylidene fluoride ultrafiltration membrane is prepared by a traditional phase transformation method, then the polyvinylidene fluoride ultrafiltration membrane is activated and modified by using potassium permanganate and sodium bisulfite, and the polyvinylidene fluoride ultrafiltration membrane is grafted with hydrophilic groups; and then a metal oxide precursor is introduced, the surface of the polyvinylidene fluoride ultrafiltration membrane is loaded with nano metal oxide by an in-situ deposition method, and thus the polymer-based nano composite ultrafiltration membrane is prepared. The synthesis method disclosed by the invention is simple in process, the problems that the utilization efficiency is low and nano materials are easy to agglomerate because the interior of a membrane piece is easily encapsulated with nanoparticles are solved, and the prepared polymer-based nano composite ultrafiltration membrane has the advantages of high utilization efficiency of nanomaterials, large membrane flux, strong anti-pollution ability, stable separation performance and the like.

Description

technical field

[0001] The invention belongs to the field of membrane material preparation, and in particular relates to a preparation method of a polymer-based nanocomposite ultrafiltration membrane. Background technique

[0002] The organic-inorganic composite membrane has the characteristics of good flexibility and good film-forming performance of the organic membrane, and also has the high mechanical strength of the inorganic membrane, good stability, chemical and biological erosion resistance, and the anti-pollution performance is far better than the organic membrane. Diaphragm. Therefore, since it was synthesized for the first time in 1996, it has rapidly become an important research direction and hotspot in this field.

[0003] At present, the traditional organic-inorganic composite film synthesis process is to synthesize inorganic nanomaterials first, and then blend them with organic substances to form a film. However, in this method, nanoparticles are easy to aggl...

Examples

Embodiment 1

[0034] (1) Based on 100 parts of casting solution, take 20 parts of polyvinylidene fluoride powder and dissolve in 70 parts of dimethylacetamide solvent, add 10 parts of polyvinylpyrrolidone porogen, stir evenly, and defoam and mature Finally, the traditional phase transformation method is used to allow the casting solution to stand, gel, and scrape the membrane to synthesize polyvinylidene fluoride ultrafiltration membranes;

[0035] (2) The polyvinylidene fluoride ultrafiltration membrane that step (1) obtains is added to the KMnO containing the NaOH of mass fraction 10% and mass fraction 5%. 4 The activation reaction is carried out in the mixed solution, and the activation reaction time is 48h;

[0036] (3) the activated polyvinylidene fluoride ultrafiltration membrane obtained in step (2) is placed in a mass fraction of 30% NaHSO 3 Soak in the solution for 6 hours, and then wash with deionized water until the effluent is clear to obtain a modified polyvinylidene fluoride ...

Embodiment 2

[0040] Other conditions of this instance are the same as embodiment 1, and the difference is:

[0041] In step (1), the polyvinylidene fluoride is 35 parts, the solvent is 60 parts of dimethylformamide, and the porogen is 5 parts of polyethylene glycol;

[0042] In step (2), the mass fraction of NaOH in the mixed solution is 30%, KMnO 4 The mass fraction is 20%, and the activation reaction time is 29h;

[0043] The bisulfite solution adopted in the step (3) is that the mass fraction is 10% NaHSO 3 solution, soaking time is 1h;

[0044] The metal oxide precursor solution adopted in step (4) is a zirconium oxychloride solution with a mass fraction of 2%;

[0045] In step (5), the mass fraction of NaOH solution is 5%, and the polymer-based nanocomposite ultrafiltration membrane is prepared after in-situ deposition, washing and drying.

Embodiment 3

[0047] Other conditions of this instance are the same as embodiment 1, and the difference is:

[0048] In step (1), the polyvinylidene fluoride is 35 parts, the solvent is 40 parts of dimethyl sulfoxide, and the porogen is 25 parts of polyvinyl alcohol;

[0049] In step (2), the mass fraction of NaOH in the mixed solution is 5%, KMnO 4 The mass fraction of is 10%, and the activation reaction time is 6h;

[0050] The bisulfite solution that adopts in step (3) is the KHSO of 15% that massfraction is 3 Solution, soaking time is 3h;

[0051] The metal oxide precursor solution adopted in step (4) is a manganese nitrate solution with a mass fraction of 40%;

[0052] In step (5), the mass fraction of NaOH solution is 5%, and the polymer-based nanocomposite ultrafiltration membrane is prepared after in-situ deposition, washing and drying.

technical field

[0001] The invention belongs to the field of membrane material preparation, and in particular relates to a preparation method of a polymer-based nanocomposite ultrafiltration membrane. Background technique

[0002] The organic-inorganic composite membrane has the characteristics of good flexibility and good film-forming performance of the organic membrane, and also has the high mechanical strength of the inorganic membrane, good stability, chemical and biological erosion resistance, and the anti-pollution performance is far better than the organic membrane. Diaphragm. Therefore, since it was synthesized for the first time in 1996, it has rapidly become an important research direction and hotspot in this field.

[0003] At present, the traditional organic-inorganic composite film synthesis process is to synthesize inorganic nanomaterials first, and then blend them with organic substances to form a film. However, in this method, nanoparticles are easy to aggl...

Examples

Embodiment 1

[0034] (1) Based on 100 parts of casting solution, take 20 parts of polyvinylidene fluoride powder and dissolve in 70 parts of dimethylacetamide solvent, add 10 parts of polyvinylpyrrolidone porogen, stir evenly, and defoam and mature Finally, the traditional phase transformation method is used to allow the casting solution to stand, gel, and scrape the membrane to synthesize polyvinylidene fluoride ultrafiltration membranes;

[0035] (2) The polyvinylidene fluoride ultrafiltration membrane that step (1) obtains is added to the KMnO containing the NaOH of mass fraction 10% and mass fraction 5%. 4 The activation reaction is carried out in the mixed solution, and the activation reaction time is 48h;

[0036] (3) the activated polyvinylidene fluoride ultrafiltration membrane obtained in step (2) is placed in a mass fraction of 30% NaHSO 3 Soak in the solution for 6 hours, and then wash with deionized water until the effluent is clear to obtain a modified polyvinylidene fluoride ...

Embodiment 2

[0040] Other conditions of this instance are the same as embodiment 1, and the difference is:

[0041] In step (1), the polyvinylidene fluoride is 35 parts, the solvent is 60 parts of dimethylformamide, and the porogen is 5 parts of polyethylene glycol;

[0042] In step (2), the mass fraction of NaOH in the mixed solution is 30%, KMnO 4 The mass fraction is 20%, and the activation reaction time is 29h;

[0043] The bisulfite solution adopted in the step (3) is that the mass fraction is 10% NaHSO 3 solution, soaking time is 1h;

[0044] The metal oxide precursor solution adopted in step (4) is a zirconium oxychloride solution with a mass fraction of 2%;

[0045] In step (5), the mass fraction of NaOH solution is 5%, and the polymer-based nanocomposite ultrafiltration membrane is prepared after in-situ deposition, washing and drying.

Embodiment 3

[0047] Other conditions of this instance are the same as embodiment 1, and the difference is:

[0048] In step (1), the polyvinylidene fluoride is 35 parts, the solvent is 40 parts of dimethyl sulfoxide, and the porogen is 25 parts of polyvinyl alcohol;

[0049] In step (2), the mass fraction of NaOH in the mixed solution is 5%, KMnO 4 The mass fraction of is 10%, and the activation reaction time is 6h;

[0050] The bisulfite solution that adopts in step (3) is the KHSO of 15% that massfraction is 3 Solution, soaking time is 3h;

[0051] The metal oxide precursor solution adopted in step (4) is a manganese nitrate solution with a mass fraction of 40%;

[0052] In step (5), the mass fraction of NaOH solution is 5%, and the polymer-based nanocomposite ultrafiltration membrane is prepared after in-situ deposition, washing and drying.

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