CN108993175A - A kind of preparation method of the super-hydrophobic filter membrane of nonwoven fabric base - Google Patents

A kind of preparation method of the super-hydrophobic filter membrane of nonwoven fabric base Download PDF

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Publication number
CN108993175A
CN108993175A CN201810861512.5A CN201810861512A CN108993175A CN 108993175 A CN108993175 A CN 108993175A CN 201810861512 A CN201810861512 A CN 201810861512A CN 108993175 A CN108993175 A CN 108993175A
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China
Prior art keywords
super
filter membrane
nonwoven fabric
hydrophobic
fabric base
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CN201810861512.5A
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Chinese (zh)
Inventor
张勇
陈艳霞
徐素芹
姚菊明
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Zhejiang Sci Tech University ZSTU
Zhejiang University of Science and Technology ZUST
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Zhejiang Sci Tech University ZSTU
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/06—Organic material
    • B01D71/26—Polyalkenes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
    • B01D17/08—Thickening liquid suspensions by filtration
    • B01D17/085—Thickening liquid suspensions by filtration with membranes
    • 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
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/06—Organic material
    • B01D71/30—Polyalkenyl halides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/06—Organic material
    • B01D71/48—Polyesters
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2325/00—Details relating to properties of membranes
    • B01D2325/38—Hydrophobic membranes

Abstract

The invention discloses a kind of preparation methods of the super-hydrophobic filter membrane of nonwoven fabric base.Main points using method are to combine to prepare hydrophobic SiO with hydrophobically modified by sol-gal process2Particle, and nonwoven surface is grafted on, the super-hydrophobic filter membrane of nonwoven fabric base is obtained after heat cure.This method is quick, efficient, at low cost, the preparation suitable for the super-hydrophobic filter membrane of nonwoven fabric base.The super-hydrophobic filter membrane preparation process of nonwoven fabric base prepared by the present invention is simple, low energy consumption, production cost is low, hydrophobicity is good, propose a kind of preparation method of super-hydrophobic filter membrane that can be used for being mass produced, be conducive to accelerate to break through simultaneously to separate oil and this technical problem of organic solvent from oily waste water, there are important environmental and social benefits.

Description

A kind of preparation method of the super-hydrophobic filter membrane of nonwoven fabric base
Technical field
The present invention relates to a kind of preparation method of super-hydrophobic filter membrane, in particular to the system of a kind of super-hydrophobic filter membrane of nonwoven fabric base Preparation Method belongs to field of environment engineering technology.
Background technique
In recent years, with the sustainable development of petroleum related industries, oily wastewater increasingly increases.Meanwhile crude oil is in exploration, fortune Defeated and storage process leakage is also an important factor for causing environment and ecological disruption.Such as Gulf of Mexico oil spilling thing in 2010 Part releases more than 2.1 hundred million gallons crude oil, seriously polluted marine ecosystems, also produces to financial circles, tourist industry etc. negative Face is rung.Oil is separated from oily waste water and organic matter is energy saving and the global challenges of protection environment.Traditional purification Technology includes air bearing, absorption, flocculation, extraction etc..However, there are high operation costs, low separative efficiency, secondary pollution for these technologies And the problems such as high energy consumption, hinder its large-scale application in oily waste water treatment.Separative efficiency is high, low energy consumption, operation letter Just membrane separation technique is in urgent need in oil/water mixture large-scale application.Super-hydrophobicity water-oil separationg film can be realized from water Middle efficient absorption crosses oil strain without generating pollution, is a kind of effective water-oil separating material.
In general, precision process such as chemical method for etching, template and nanoimprint lithography etc. can be by constructing coarse table Face and the preparation that super-hydrophobic film is realized using low surface free energy material.However, in practical applications, more preferably at low cost, Technical method that is simple and effective and can be used for being mass produced.Based on this, by low cost and simple effective method, preparation is super Hydrophobicity water-oil separating filtering material simultaneously realizes its large-scale application in oiliness sewage treatment for alleviating oily waste water pair The pressure of society and environment is significant.
In hydrophobic separation filter membrane preparation field, a kind of Chinese patent (CN 107936377A) " hydrophobic nonwoven plastic film material Material and preparation method thereof " passes through polypropylene, allyl polyglycol, 8- hydroxyl beautiful jade, lanolin, melamine, borax, stabilization Agent, polyvinyl butyral ester, rilanit special, ethyl orthosilicate, blanc fixe, second phthalein acetone vanadium, oxidized polyethylene wax, The raw materials such as ten difluoro heptyl propyl trimethoxy silicanes prepare hydrophobic nonwoven plastic film material；Chinese patent (CN 106833253A) " a kind of hydrophobic material and preparation method thereof " hydrophobic material by substrate and it is hydrophobic surface coated constitute, wherein Surface covering is made of stearic acid modified magnesium hydroxide powder and phenolic resin, substrate be selected from stainless (steel) wire, glass, cotton, High-intensitive woven fabric, nylon filter, thin polymer film, aluminium net, nickel screen and copper mesh；Chinese patent (CN107096391A) is " a kind of The preparation method of underwater superoleophobic and oily lower super-hydrophobic film and its continuously method from light oil/water/heavy oil mixture " preparation is super thin Moisture film method includes: preparing Network substrates, prepares coating dispersion liquid, spraying, prepares underwater superoleophobic and oily lower super-hydrophobic film； Chinese patent (CN 105779943A) " a kind of method of physical vapour deposition (PVD) silicon fluoride preparation hydrophobic membrane " to substrate implement etc. from Sub- aura processing, then medium frequency magnetron sputtering transparent Indium silicon fiml, sputtering target material are pure silicon target, and last vacuum evaporation silicon fluoride is dredged Moisture film obtains transparent silicon fluoride hydrophobic film layer.So far, it yet there are no and combined by sol-gal process with hydrophobically modified Prepare hydrophobic SiO2Particle is grafted on nonwoven surface, is carried out heat cure and is prepared the super-hydrophobic filter membrane of nonwoven fabric base Related process technologies occur.
Summary of the invention
Prepare that preparation process existing for super-hydrophobic water-oil separationg film is complicated, operating cost is high, energy consumption is high at present to overcome The problems such as, the object of the present invention is to provide a kind of preparation methods of simple and effective super-hydrophobic filter membrane of nonwoven fabric base.
To achieve the above object, the technical scheme is that using following steps:
A kind of preparation method of the super-hydrophobic filter membrane of nonwoven fabric base, which comprises the following steps:
1) by non-woven fabrics ultraviolet lamp under irradiate 2min, obtain the non-woven fabrics through ultraviolet light irradiation；
2) sodium metasilicate is dissolved in 30mL deionized water, keeps its evenly dispersed under mechanical agitation, obtains silicic acid Sodium solution；
3) silane is added into sodium silicate solution obtained in step 2), keeps its evenly dispersed under mechanical agitation, Obtain the sodium silicate solution of silane-containing；
4) ethyl alcohol is slowly added dropwise into the sodium silicate solution of silane-containing obtained in step 3), stands 6h and is placed on 70-90 180-240min is reacted in DEG C water-bath, obtains hydrophobic SiO2Colloidal sol；
5) non-woven fabrics through ultraviolet light irradiation obtained in step 1) is horizontally placed at hydrophobic obtained in step 4) SiO2It takes out, is washed with deionized 3 times after 30min in colloidal sol, be put into 80 DEG C of baking ovens and taken out after 2h, has been grafted hydrophobic SiO2The non-woven fabrics of particle；
6) step 5) is repeated 3 times, hydrophobic SiO will be grafted2Thermosetting under the conditions of 120 DEG C of the non-woven fabrics of particle Change, obtains the super-hydrophobic filter membrane of nonwoven fabric base.
The non-woven fabrics is one of PP non-woven fabrics, PET non-woven fabrics, PVC non-woven fabrics.
The ultraviolet lamp illumination wavelength is one of 172nm, 222nm, 308nm.
The concentration of the sodium silicate solution is 20-50wt%.
The silane is 3- aminopropyl three (trimethylsiloxy group) silane, octadecyl trimethoxysilane, double three One of methyl siloxy methyl-monosilane, the mass ratio of sodium metasilicate and silane are 1-4:1.
The ethyl alcohol is dehydrated alcohol, dosage 12-20mL.
Compared with the background art, the invention has the advantages that:
The super-hydrophobic filter membrane preparation process of nonwoven fabric base prepared by the present invention is simple, energy consumption is lower, production cost is low, hydrophobicity Well, it can be achieved that large-scale production, is conducive to accelerate to break through to separate oily and this technical problem of organic solvent from oily waste water, With important environmental and social benefits.
Detailed description of the invention
Fig. 1 is the water contact angle picture for the super-hydrophobic filter membrane product (b) of nonwoven fabric base being prepared by embodiment 2.
Specific embodiment
The present invention is further explained in the light of specific embodiments.
Embodiment 1:
1) PP non-woven fabrics is irradiated into 2min in the case where wavelength is the ultraviolet lamp of 172nm, obtains the non-woven fabrics through ultraviolet light irradiation；
2) sodium metasilicate is dissolved in 30mL deionized water, keeps its evenly dispersed under mechanical agitation, obtains concentration For the sodium silicate solution of 20wt%；
3) three (trimethyl silicane of 3- aminopropyl is added into the sodium silicate solution that concentration obtained in step 2) is 20wt% Oxygroup) silane, the mass ratio of sodium metasilicate and silane is 1:1, keeps its evenly dispersed under mechanical agitation, obtains silane-containing Sodium silicate solution；
4) 12mL dehydrated alcohol is slowly added dropwise into the sodium silicate solution of silane-containing obtained in step 3), stands 6h postposition 180min is reacted in 70 DEG C of water-baths, obtains hydrophobic SiO2Colloidal sol；
5) non-woven fabrics through ultraviolet light irradiation obtained in step 1) is horizontally placed at hydrophobic obtained in step 4) SiO2It takes out, is washed with deionized 3 times after 30min in colloidal sol, be put into 80 DEG C of baking ovens and taken out after 2h, has been grafted hydrophobic SiO2The non-woven fabrics of particle；
6) step 5) is repeated 3 times, hydrophobic SiO will be grafted2Thermosetting under the conditions of 120 DEG C of the non-woven fabrics of particle Change, obtains the super-hydrophobic filter membrane (a) of nonwoven fabric base.
Embodiment 2:
1) PET non-woven fabrics is irradiated into 2min in the case where wavelength is the ultraviolet lamp of 222nm, obtains the nonwoven through ultraviolet light irradiation Cloth；
2) sodium metasilicate is dissolved in 30mL deionized water, keeps its evenly dispersed under mechanical agitation, obtains concentration For the sodium silicate solution of 30wt%；
3) octadecyl trimethoxysilane is added into the sodium silicate solution that concentration obtained in step 2) is 30wt%, The mass ratio of sodium metasilicate and silane is 2:1, keeps its evenly dispersed under mechanical agitation, the sodium metasilicate for obtaining silane-containing is molten Liquid；
4) 16mL dehydrated alcohol is slowly added dropwise into the sodium silicate solution of silane-containing obtained in step 3), stands 6h postposition 210min is reacted in 80 DEG C of water-baths, obtains hydrophobic SiO2Colloidal sol；
5) non-woven fabrics through ultraviolet light irradiation obtained in step 1) is horizontally placed at hydrophobic obtained in step 4) SiO2It takes out, is washed with deionized 3 times after 30min in colloidal sol, be put into 80 DEG C of baking ovens and taken out after 2h, has been grafted hydrophobic SiO2The non-woven fabrics of particle；
6) step 5) is repeated 3 times, hydrophobic SiO will be grafted2Thermosetting under the conditions of 120 DEG C of the non-woven fabrics of particle Change, obtains the super-hydrophobic filter membrane (b) of nonwoven fabric base.
Embodiment 3:
1) PVA non-woven fabrics is irradiated into 2min in the case where wavelength is the ultraviolet lamp of 308nm, obtains the nonwoven through ultraviolet light irradiation Cloth；
2) sodium metasilicate is dissolved in 30mL deionized water, keeps its evenly dispersed under mechanical agitation, obtains concentration For the sodium silicate solution of 40wt%；
3) octadecyl trimethoxysilane is added into the sodium silicate solution that concentration obtained in step 2) is 40wt%, The mass ratio of sodium metasilicate and silane is 3:1, keeps its evenly dispersed under mechanical agitation, the sodium metasilicate for obtaining silane-containing is molten Liquid；
4) 18mL dehydrated alcohol is slowly added dropwise into the sodium silicate solution of silane-containing obtained in step 3), stands 6h postposition 240min is reacted in 80 DEG C of water-baths, obtains hydrophobic SiO2Colloidal sol；
5) non-woven fabrics through ultraviolet light irradiation obtained in step 1) is horizontally placed at hydrophobic obtained in step 4) SiO2It takes out, is washed with deionized 3 times after 30min in colloidal sol, be put into 80 DEG C of baking ovens and taken out after 2h, has been grafted hydrophobic SiO2The non-woven fabrics of particle；
6) step 5) is repeated 3 times, hydrophobic SiO will be grafted2Thermosetting under the conditions of 120 DEG C of the non-woven fabrics of particle Change, obtains the super-hydrophobic filter membrane (c) of nonwoven fabric base.
Embodiment 4:
1) PVA non-woven fabrics is irradiated into 2min in the case where wavelength is the ultraviolet lamp of 308nm, obtains the nonwoven through ultraviolet light irradiation Cloth；
2) sodium metasilicate is dissolved in 30mL deionized water, keeps its evenly dispersed under mechanical agitation, obtains concentration For the sodium silicate solution of 50wt%；
3) double trimethylsiloxy group methyl silicon are added into the sodium silicate solution that concentration obtained in step 2) is 50wt% The mass ratio of alkane, sodium metasilicate and silane is 4:1, keeps its evenly dispersed under mechanical agitation, obtains the sodium metasilicate of silane-containing Solution；
4) 20mL dehydrated alcohol is slowly added dropwise into the sodium silicate solution of silane-containing obtained in step 3), stands 6h postposition 240min is reacted in 90 DEG C of water-baths, obtains hydrophobic SiO2Colloidal sol；
5) non-woven fabrics through ultraviolet light irradiation obtained in step 1) is horizontally placed at hydrophobic obtained in step 4) SiO2It takes out, is washed with deionized 3 times after 30min in colloidal sol, be put into 80 DEG C of baking ovens and taken out after 2h, has been grafted hydrophobic SiO2The non-woven fabrics of particle；
6) step 5) is repeated 3 times, hydrophobic SiO will be grafted2Thermosetting under the conditions of 120 DEG C of the non-woven fabrics of particle Change, obtains the super-hydrophobic filter membrane (d) of nonwoven fabric base.
Measure the water contact angle of the super-hydrophobic filter membrane of nonwoven fabric base prepared by embodiment 1,2,3,4, table 1 be embodiment 1,2,3, The measurement result of the super-hydrophobic filter membrane water contact angle of nonwoven fabric base of 4 preparations.It can be seen that by 1 data of table, the super-hydrophobic filter membrane of preparation (a), (b), (c), (d) water contact angle be respectively 170 °, 174 °, 168 °, 172 ° up to 160 ° or more show the nonwoven fabric base Super-hydrophobic filter membrane has preferable hydrophobic effect, and preparation process is simple, energy consumption is lower, production cost is low, it can be achieved that extensive Production is conducive to accelerate to break through to separate oil and this technical problem of organic solvent from oily waste water, with important environment and Social benefit.
Table 1
The above enumerated are only specific embodiments of the present invention.Present invention is not limited to the above embodiments, can also there are many Deformation.All deformations that those skilled in the art directly can export or associate from present disclosure, should all It is considered protection scope of the present invention.

Claims (6)

1. a kind of preparation method of the super-hydrophobic filter membrane of nonwoven fabric base, which comprises the following steps:
1) by non-woven fabrics ultraviolet lamp under irradiate 2min, obtain the non-woven fabrics through ultraviolet light irradiation；
2) sodium metasilicate is dissolved in 30mL deionized water, keeps its evenly dispersed under mechanical agitation, it is molten obtains sodium metasilicate Liquid；
3) silane is added into sodium silicate solution obtained in step 2), keeps its evenly dispersed under mechanical agitation, obtains The sodium silicate solution of silane-containing；
4) ethyl alcohol is slowly added dropwise into the sodium silicate solution of silane-containing obtained in step 3), stands 6h and is placed on 70-90 DEG C of water 180-240min is reacted in bath, obtains hydrophobic SiO2Colloidal sol；
5) non-woven fabrics through ultraviolet light irradiation obtained in step 1) is horizontally placed at hydrophobic SiO obtained in step 4)2It is molten It takes out, is washed with deionized 3 times after 30min in glue, be put into 80 DEG C of baking ovens and taken out after 2h, be grafted hydrophobic SiO2? The non-woven fabrics of grain；
6) step 5) is repeated 3 times, hydrophobic SiO will be grafted2Heat cure under the conditions of 120 DEG C of the non-woven fabrics of particle, obtains The super-hydrophobic filter membrane of nonwoven fabric base.
2. a kind of preparation method of the super-hydrophobic filter membrane of nonwoven fabric base according to claim 1, it is characterised in that: the nothing Woven fabric is one of PP non-woven fabrics, PET non-woven fabrics, PVC non-woven fabrics.
3. a kind of preparation method of the super-hydrophobic filter membrane of nonwoven fabric base according to claim 1, it is characterised in that: the purple Outer light irradiation wavelength is one of 172nm, 222nm, 308nm.
4. a kind of preparation method of the super-hydrophobic filter membrane of nonwoven fabric base according to claim 1, it is characterised in that: the silicon The concentration of acid sodium solution is 20-50wt%.
5. a kind of preparation method of the super-hydrophobic filter membrane of nonwoven fabric base according to claim 1, it is characterised in that: the silicon Alkane is 3- aminopropyl three (trimethylsiloxy group) silane, octadecyl trimethoxysilane, double trimethylsiloxy group methyl silicon The mass ratio of one of alkane, sodium metasilicate and silane is 1-4:1.
6. a kind of preparation method of the super-hydrophobic filter membrane of nonwoven fabric base according to claim 1, it is characterised in that: the second Alcohol is dehydrated alcohol, dosage 12-20mL.
CN201810861512.5A 2018-07-29 2018-07-29 A kind of preparation method of the super-hydrophobic filter membrane of nonwoven fabric base Pending CN108993175A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110026093A (en) * 2019-04-27 2019-07-19 浙江理工大学 A kind of PET-SiO2The preparation method of super-hydrophobic film

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101090923A (en) * 2004-12-27 2007-12-19 小西化学工业株式会社 Organic-solvent dispersion of fine polysilsesquioxane particle, process for producing the same, aqueous dispersion polysilsesquioxane particle, and process
CN104492286A (en) * 2014-12-19 2015-04-08 天津工业大学 Preparation and application of support layer functionalized adsorption-enhanced type composite ultrafiltration membrane
CN105002656A (en) * 2014-12-29 2015-10-28 中国科学院烟台海岸带研究所 Hydrophobic film with self-cleaning function, preparation method thereof and application thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101090923A (en) * 2004-12-27 2007-12-19 小西化学工业株式会社 Organic-solvent dispersion of fine polysilsesquioxane particle, process for producing the same, aqueous dispersion polysilsesquioxane particle, and process
CN104492286A (en) * 2014-12-19 2015-04-08 天津工业大学 Preparation and application of support layer functionalized adsorption-enhanced type composite ultrafiltration membrane
CN105002656A (en) * 2014-12-29 2015-10-28 中国科学院烟台海岸带研究所 Hydrophobic film with self-cleaning function, preparation method thereof and application thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110026093A (en) * 2019-04-27 2019-07-19 浙江理工大学 A kind of PET-SiO2The preparation method of super-hydrophobic film

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Application publication date: 20181214