CN110026093A - A kind of PET-SiO2The preparation method of super-hydrophobic film - Google Patents

A kind of PET-SiO2The preparation method of super-hydrophobic film Download PDF

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Publication number
CN110026093A
CN110026093A CN201910348026.8A CN201910348026A CN110026093A CN 110026093 A CN110026093 A CN 110026093A CN 201910348026 A CN201910348026 A CN 201910348026A CN 110026093 A CN110026093 A CN 110026093A
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China
Prior art keywords
sio
pet
super
film
hydrophobic film
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Inventor
张勇
陈艳霞
黄玉
朱海东
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
    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • 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
    • B01D71/02—Inorganic material
    • B01D71/024—Oxides
    • B01D71/027—Silicium oxide
    • 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 PET-SiO2The preparation method of super-hydrophobic film.Main points using method are by growing SiO in modified PET film surface in situ2Particle, and carry out low-surface-energy modification to it, obtains that hydrophobicity is good, PET-SiO of high mechanical strength, easily biological-degradable2Super-hydrophobic film.This method is easy to operate, energy-efficient, cost is relatively low, the preparation suitable for PET based super hydrophobic film.The preparation method of super-hydrophobic film proposed by the present invention grows SiO in situ2PET film in introduce poly-dopamine, improve PET film and SiO2Bond strength, SiO can be substantially reduced2The usage amount of Gel Precursor, reduces the production cost of hydrophobic membrane, while being conducive to accelerate to break through stable water-in-oil emulsion this technical problem of separation surfactant, has important environmental and social benefits.

Description

A kind of PET-SiO2The preparation method of super-hydrophobic film
Technical field
The present invention relates to a kind of preparation method of super-hydrophobic film, in particular to a kind of PET-SiO2The preparation side of super-hydrophobic film Method belongs to high-molecular organic material technical field.
Background technique
The oily waste water generated in industrial processes and oil spill accident causes significant damage to ecological environment and human health, special Be not in oily phase containing largely less than 20 μm dispersion water droplet water-in-oil emulsion it is highly stable, make it be difficult to separate, effectively point The water-in-oil emulsion stable from surfactant has become global challenges.Various conventional methods include electrostatic separation, biology Demulsification, chemical demulsification and floatation etc., however these methods are difficult to efficiently separate oil emulsion/aqueous mixtures, and operating cost it is high, Easily cause secondary pollution, equipment energy consumption high.Therefore, it needs to develop new and effective oil hydrosol separation material.
In recent years, oil emulsion/aqueous mixtures are separated by the extensive of water-oil separating field by super hydrophobic porous membrane material Concern.In general, can realize the preparation of super-hydrophobic film by building rough surface and using low surface free energy material.Currently, The common method for preparing super hydrophobic surface is to tie membrane material mutually with inorganic particle by the methods of spraying, etching, chemical deposition It closes, establishes multilayered structure abundant and realize surface super-hydrophobic.But nano particle, which is excessively added, can cause interface mutually to separate simultaneously And coating adherence energy and preparation process complexity, energy consumption height are reduced due to particle aggregation.Based on this, by simple and effective and The method of low energy consumption reduces the quantity of nanoparticle, improves the interface binding power between membrane material and inorganic particulate, prepares super thin Water porous film material is significant to realize its large-scale application in separation oil emulsion/aqueous mixtures.
In super-hydrophobic separation filter membrane preparation field, " preparation of one-step shaping method is multistage for Chinese patent (109338597 A of CN) The super-hydrophobic electrostatic spinning film of the polycaprolactone of structure " prepares electrostatic spinning polycaprolactone/methyl-silicone oil precursor liquid, in precursor liquid Middle addition hydrophobic silica nano particle is simultaneously stirred by ultrasonic, and prepares polycaprolactone/methyl-silicone oil/nanometer by method of electrostatic spinning The film of silica bead structure, water contact angle is up to 151 °；Chinese patent (109012199 A of CN) be " a kind of resist wet Super-hydrophobic film and preparation method thereof " carries out organosilicon material coating in film surface, in conjunction with sol-gal process, forms one in film surface Kind is similar to the coat of " sandwich ", and the low-surface-energy of organosilicon material and the coarse structure of nano particle can be such that film is surpassed Hydrophobicity；Chinese patent (109126205 A of CN) " a kind of preparation method of water-oil separating PS/PMMA bionic super-hydrophobic film " By the way that the tetrahydrofuran solution of PS, PMMA are mixed with carbon nano tube dispersion liquid, then be added solvent mutually separated, make PS, The strand of PMMA curls into a ball of string, obtains the porous composite film of the mastoid process structure with similar lotus leaf, further with 1H, 1H, 2H, 2H- perfluoro decyl mercaptan are surface modified, and PS/PMMA bionic super-hydrophobic film is made；United States Patent (USP) (US 2017165612A1)“Robust carbon nanotube membranes and methods of making the Same " grows carbon nanotube on metallic substrates, is prepared for super-hydrophobic film, and performance is stablized in moist or corrosive environment.It cuts PET film is modified by poly-dopamine to currently, yet there are no, growth in situ SiO2Prepare PET-SiO2The correlation of super-hydrophobic film Technology occurs.
A kind of PET-SiO provided by the invention2The preparation method of super-hydrophobic film, it is good using high mechanical strength, chemical resistance Good, easily biological-degradable PET film is substrate, passes through poly-dopamine modified lithium, growth in situ SiO2Particle, and low surface is carried out to it Can modification, prepare that hydrophobicity is good, cost is relatively low, the PET-SiO of easily biological-degradable2Super-hydrophobic film.The PET-SiO prepared2 Super-hydrophobic film can be applied to the stable water-in-oil emulsion process of separation surfactant, have great market prospects and society's effect Benefit.
Summary of the invention
Super hydrophobic surface existing membrane material in the process is prepared in order to overcome to combine by membrane material with inorganic particle at present The problems such as material and inorganic particle poor adhesion, preparation process are complicated, energy consumption is high passes through simple and effective and low energy consumption method and improves Interface binding power between membrane material and inorganic particulate.The object of the present invention is to provide a kind of preparations of super hydrophobic porous membrane material Method.
To achieve the above object, the technical scheme is that using following steps:
1) 0.1-0.3g dopamine hydrochloride is dissolved in 100mL deionized water, it is made under mechanical agitation uniformly Dispersion adjusts pH to 8.5, obtains the poly-dopamine solution that concentration is 1-3g/L；
2) PET film is placed in the poly-dopamine solution that concentration obtained in step 1) is 1-3g/L after 2h and is taken out, spent It ion water washing 3 times, is put into 60 DEG C of baking ovens and is taken out after 3h, obtain modified PET film；
3) 0.4mL tetraethyl orthosilicate is dissolved in dehydrated alcohol, keeps its evenly dispersed under mechanical agitation, obtains Tetraethyl orthosilicate solution；
4) ammonium chloride solution is slowly added dropwise into tetraethyl orthosilicate solution obtained in step 3), under mechanical agitation Keep its evenly dispersed, obtains SiO2Colloidal sol；
5) to SiO obtained in step 4)2Silane is added dropwise in colloidal sol, is placed under mechanical agitation in 25 DEG C of water-baths anti- 6h is answered, is obtained by the SiO after hydrophobically modified2Colloidal sol；
6) modified PET film obtained in step 2) is infiltrated on obtained in step 5) by the SiO after hydrophobically modified2 In colloidal sol, is taken out after standing 15min, be put into 60 DEG C of baking ovens and taken out after 6h, obtain PET-SiO2Super-hydrophobic film.
The dehydrated alcohol dosage is 5-10mL.
The ammonium chloride solution concentration is 18wt%, dosage 0.4-0.8mL.
The silane is Cyclohexyl Methyl Dimethoxysilane, hexadecyl trimethoxy silane, 1,1,3,3,5,5- The volume ratio of one of hexam ethylcyclotrisiloxane, silane and tetraethyl orthosilicate is 0.5-1.5:1.
Compared with the background art, the invention has the advantages that:
PET-SiO prepared by the present invention2Super-hydrophobic film preparation process is simple, energy-efficient, cost is relatively low, hydrophobicity is good Good, high mechanical strength, easily biological-degradable are conducive to accelerate to break through stable water-in-oil emulsion this technology of separation surfactant Problem has important environmental and social benefits.
Specific embodiment
The present invention is further explained in the light of specific embodiments.
Embodiment 1:
1) 0.1g dopamine hydrochloride is dissolved in 100mL deionized water, keeps its evenly dispersed under mechanical agitation, PH to 8.5 is adjusted, the poly-dopamine solution that concentration is 1g/L is obtained；
2) PET film is placed in the poly-dopamine solution that concentration obtained in step 1) is 1g/L and is taken out after 2h, spend from Sub- water washing 3 times is put into 60 DEG C of baking ovens and takes out after 3h, obtains modified PET film；
3) 0.4mL tetraethyl orthosilicate is dissolved in 5mL dehydrated alcohol, keeps its evenly dispersed under mechanical agitation, Obtain tetraethyl orthosilicate solution；
4) it is molten that the ammonium chloride that 0.4mL concentration is 18wt% is slowly added dropwise into tetraethyl orthosilicate solution obtained in step 3) Liquid keeps its evenly dispersed, obtains SiO under mechanical agitation2Colloidal sol；
5) to SiO obtained in step 4)2Cyclohexyl Methyl Dimethoxysilane is added dropwise in colloidal sol, with tetraethyl orthosilicate Volume ratio be 0.5:1, be placed under mechanical agitation in 25 DEG C of water-baths and react 6h, obtained by the SiO after hydrophobically modified2It is molten Glue；
6) modified PET film obtained in step 2) is infiltrated on obtained in step 5) by the SiO after hydrophobically modified2 In colloidal sol, is taken out after standing 15min, be put into 60 DEG C of baking ovens and taken out after 6h, obtain PET-SiO2Super-hydrophobic film (a).
Embodiment 2:
1) 0.2g dopamine hydrochloride is dissolved in 100mL deionized water, keeps its evenly dispersed under mechanical agitation, PH to 8.5 is adjusted, the poly-dopamine solution that concentration is 2g/L is obtained；
2) PET film is placed in the poly-dopamine solution that concentration obtained in step 1) is 2g/L and is taken out after 2h, spend from Sub- water washing 3 times is put into 60 DEG C of baking ovens and takes out after 3h, obtains modified PET film；
3) 0.4mL tetraethyl orthosilicate is dissolved in 7mL dehydrated alcohol, keeps its evenly dispersed under mechanical agitation, Obtain tetraethyl orthosilicate solution；
4) it is molten that the ammonium chloride that 0.5mL concentration is 18wt% is slowly added dropwise into tetraethyl orthosilicate solution obtained in step 3) Liquid keeps its evenly dispersed, obtains SiO under mechanical agitation2Colloidal sol；
5) to SiO obtained in step 4)2Hexadecyl trimethoxy silane is added dropwise in colloidal sol, with tetraethyl orthosilicate Volume ratio is 0.8:1, is placed in 25 DEG C of water-baths under mechanical agitation and reacts 6h, obtained by the SiO after hydrophobically modified2It is molten Glue；
6) modified PET film obtained in step 2) is infiltrated on obtained in step 5) by the SiO after hydrophobically modified2 In colloidal sol, is taken out after standing 15min, be put into 60 DEG C of baking ovens and taken out after 6h, obtain PET-SiO2Super-hydrophobic film (b).
Embodiment 3:
1) 0.25g dopamine hydrochloride is dissolved in 100mL deionized water, divides it uniformly It dissipates, adjusts pH to 8.5, obtain the poly-dopamine solution that concentration is 2.5g/L；
2) PET film is placed in the poly-dopamine solution that concentration obtained in step 1) is 2.5g/L after 2h and is taken out, spent It ion water washing 3 times, is put into 60 DEG C of baking ovens and is taken out after 3h, obtain modified PET film；
3) 0.4mL tetraethyl orthosilicate is dissolved in 8mL dehydrated alcohol, keeps its evenly dispersed under mechanical agitation, Obtain tetraethyl orthosilicate solution；
4) it is molten that the ammonium chloride that 0.6mL concentration is 18wt% is slowly added dropwise into tetraethyl orthosilicate solution obtained in step 3) Liquid keeps its evenly dispersed, obtains SiO under mechanical agitation2Colloidal sol；
5) to SiO obtained in step 4)2Hexadecyl trimethoxy silane is added dropwise in colloidal sol, with tetraethyl orthosilicate Volume ratio is 1:1, is placed in 25 DEG C of water-baths under mechanical agitation and reacts 6h, obtained by the SiO after hydrophobically modified2Colloidal sol；
6) modified PET film obtained in step 2) is infiltrated on obtained in step 5) by the SiO after hydrophobically modified2 In colloidal sol, is taken out after standing 15min, be put into 60 DEG C of baking ovens and taken out after 6h, obtain PET-SiO2Super-hydrophobic film (c).
Embodiment 4:
1) 0.3g dopamine hydrochloride is dissolved in 100mL deionized water, keeps its evenly dispersed under mechanical agitation, PH to 8.5 is adjusted, the poly-dopamine solution that concentration is 3g/L is obtained；
2) PET film is placed in the poly-dopamine solution that concentration obtained in step 1) is 3g/L and is taken out after 2h, spend from Sub- water washing 3 times is put into 60 DEG C of baking ovens and takes out after 3h, obtains modified PET film；
3) 0.4mL tetraethyl orthosilicate is dissolved in 10mL dehydrated alcohol, keeps its evenly dispersed under mechanical agitation, Obtain tetraethyl orthosilicate solution；
4) it is molten that the ammonium chloride that 0.8mL concentration is 18wt% is slowly added dropwise into tetraethyl orthosilicate solution obtained in step 3) Liquid keeps its evenly dispersed, obtains SiO under mechanical agitation2Colloidal sol；
5) to SiO obtained in step 4)21,1,3,3,5,5- hexam ethylcyclotrisiloxane is added dropwise in colloidal sol, with silicic acid four The volume ratio of ethyl ester is 1.5:1, is placed in 25 DEG C of water-baths under mechanical agitation and reacts 6h, obtained by after hydrophobically modified SiO2Colloidal sol；
6) modified PET film obtained in step 2) is infiltrated on obtained in step 5) by the SiO after hydrophobically modified2 In colloidal sol, is taken out after standing 15min, be put into 60 DEG C of baking ovens and taken out after 6h, obtain PET-SiO2Super-hydrophobic film (d).
Measure PET-SiO prepared by embodiment 1,2,3,42The water contact angle of super-hydrophobic film, table 1 are embodiment 1,2,3,4 The PET-SiO of preparation2The measurement result of super-hydrophobic film water contact angle.It can be seen that by 1 data of table, the PET-SiO of preparation2It is super-hydrophobic Film (a), (b), (c), (d) water contact angle be respectively 165 °, 166 °, 165 °, 167 ° up to 165 ° or more show the PET- SiO2Super-hydrophobic film has preferable hydrophobic effect, and the method is easy to operate, energy-efficient, cost is relatively low, it can be achieved that extensive Production is conducive to accelerate to break through stable water-in-oil emulsion this technical problem of separation surfactant, has 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 (4)

1. a kind of PET-SiO2The preparation method of super-hydrophobic film, which comprises the following steps:
1) 0.1-0.3g dopamine hydrochloride is dissolved in 100mL deionized water, keeps its evenly dispersed under mechanical agitation, PH to 8.5 is adjusted, the poly-dopamine solution that concentration is 1-3g/L is obtained；
2) PET film is placed in the poly-dopamine solution that concentration obtained in step 1) is 1-3g/L after 2h and is taken out, use deionization It water washing 3 times, is put into 60 DEG C of baking ovens and is taken out after 3h, obtain modified PET film；
3) 0.4mL tetraethyl orthosilicate is dissolved in dehydrated alcohol, keeps its evenly dispersed under mechanical agitation, obtains silicic acid Tetrem ester solution；
4) ammonium chloride solution is slowly added dropwise into tetraethyl orthosilicate solution obtained in step 3), makes it under mechanical agitation It is evenly dispersed, obtain SiO2Colloidal sol；
5) to SiO obtained in step 4)2Silane is added dropwise in colloidal sol, is placed under mechanical agitation in 25 DEG C of water-baths and reacts 6h, It obtains by the SiO after hydrophobically modified2Colloidal sol；
6) modified PET film obtained in step 2) is infiltrated on obtained in step 5) by the SiO after hydrophobically modified2Colloidal sol In, it is taken out after standing 15min, is put into 60 DEG C of baking ovens and is taken out after 6h, obtain PET-SiO2Super-hydrophobic film.
2. a kind of PET-SiO according to claim 12The preparation method of super-hydrophobic film, it is characterised in that: described is anhydrous Ethanol consumption is 5-10mL.
3. a kind of PET-SiO according to claim 12The preparation method of super-hydrophobic film, it is characterised in that: the chlorination Ammonium salt solution concentration is 18wt%, dosage 0.4-0.8mL.
4. a kind of PET-SiO according to claim 12The preparation method of super-hydrophobic film, it is characterised in that: the silane For in Cyclohexyl Methyl Dimethoxysilane, hexadecyl trimethoxy silane, 1,1,3,3,5,5- hexam ethylcyclotrisiloxane The volume ratio of one kind, silane and tetraethyl orthosilicate is 0.5-1.5:1.
CN201910348026.8A 2019-04-27 2019-04-27 A kind of PET-SiO2The preparation method of super-hydrophobic film Pending CN110026093A (en)

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Cited By (5)

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CN111764170A (en) * 2020-06-22 2020-10-13 武汉纺织大学 Waterproof moisture-permeable film and preparation method thereof
CN112647287A (en) * 2020-12-17 2021-04-13 中国科学院过程工程研究所 Super-hydrophobic material with hierarchical coarse structure and preparation method and application thereof
CN113731199A (en) * 2021-07-20 2021-12-03 东华大学 Super-amphiphobic membrane and preparation method and application thereof
CN114432742A (en) * 2020-10-19 2022-05-06 中国石油化工股份有限公司 Oil-water separation metal net film and preparation method and application thereof
CN114874592A (en) * 2022-03-30 2022-08-09 中原工学院 Flexible porous super-hydrophobic film and preparation method thereof

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CN107723687A (en) * 2017-09-25 2018-02-23 常州市瑞泰物资有限公司 A kind of preparation method of based superhydrophobic thin films
CN108993175A (en) * 2018-07-29 2018-12-14 浙江理工大学 A kind of preparation method of the super-hydrophobic filter membrane of nonwoven fabric base
CN109401373A (en) * 2018-09-30 2019-03-01 福建师范大学 A kind of preparation method of super-hydrophobic oleophobic silica solution

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CN106800885A (en) * 2016-12-21 2017-06-06 中国科学院兰州化学物理研究所 A kind of large-scale preparation method of transparent hydrophobic/super-amphiphobic coating
CN107446401A (en) * 2017-04-01 2017-12-08 华南理工大学 Using dopamine as high hydrophobicity anti-bacterial attachment surface of anchor molecule and preparation method thereof
CN107442064A (en) * 2017-08-08 2017-12-08 西安工程大学 The preparation method of novel hydrophobic zirconium dioxide silica composite adsorbing material
CN107723687A (en) * 2017-09-25 2018-02-23 常州市瑞泰物资有限公司 A kind of preparation method of based superhydrophobic thin films
CN108993175A (en) * 2018-07-29 2018-12-14 浙江理工大学 A kind of preparation method of the super-hydrophobic filter membrane of nonwoven fabric base
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111764170A (en) * 2020-06-22 2020-10-13 武汉纺织大学 Waterproof moisture-permeable film and preparation method thereof
CN114432742A (en) * 2020-10-19 2022-05-06 中国石油化工股份有限公司 Oil-water separation metal net film and preparation method and application thereof
CN112647287A (en) * 2020-12-17 2021-04-13 中国科学院过程工程研究所 Super-hydrophobic material with hierarchical coarse structure and preparation method and application thereof
CN112647287B (en) * 2020-12-17 2022-01-04 中国科学院过程工程研究所 Super-hydrophobic material with hierarchical coarse structure and preparation method and application thereof
CN113731199A (en) * 2021-07-20 2021-12-03 东华大学 Super-amphiphobic membrane and preparation method and application thereof
CN114874592A (en) * 2022-03-30 2022-08-09 中原工学院 Flexible porous super-hydrophobic film and preparation method thereof
CN114874592B (en) * 2022-03-30 2023-11-03 中原工学院 Flexible porous super-hydrophobic film and preparation method thereof

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Application publication date: 20190719