CN108192129A - A kind of ultra-hydrophobic polyvinylidene fluoride aerogel material and preparation method thereof - Google Patents

A kind of ultra-hydrophobic polyvinylidene fluoride aerogel material and preparation method thereof Download PDF

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CN108192129A
CN108192129A CN201711234604.2A CN201711234604A CN108192129A CN 108192129 A CN108192129 A CN 108192129A CN 201711234604 A CN201711234604 A CN 201711234604A CN 108192129 A CN108192129 A CN 108192129A
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pvdf
preparation
hydrophobic
aerogel materials
gels
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孔勇
张嘉月
沈晓冬
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Nanjing Tech University
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2201/00—Foams characterised by the foaming process
    • C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
    • C08J2201/048—Elimination of a frozen liquid phase
    • C08J2201/0484—Elimination of a frozen liquid phase the liquid phase being aqueous
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2205/00—Foams characterised by their properties
    • C08J2205/02—Foams characterised by their properties the finished foam itself being a gel or a gel being temporarily formed when processing the foamable composition
    • C08J2205/026—Aerogel, i.e. a supercritically dried gel
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2205/00—Foams characterised by their properties
    • C08J2205/04—Foams characterised by their properties characterised by the foam pores
    • C08J2205/044—Micropores, i.e. average diameter being between 0,1 micrometer and 0,1 millimeter
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2205/00—Foams characterised by their properties
    • C08J2205/04—Foams characterised by their properties characterised by the foam pores
    • C08J2205/05—Open cells, i.e. more than 50% of the pores are open
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
    • C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
    • C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • C08J2327/16—Homopolymers or copolymers of vinylidene fluoride

Abstract

The present invention relates to a kind of ultra-hydrophobic polyvinylidene fluoride PVDF aerogel materials, it is characterised in that form be White-opalescent bulk material, 0.075~0.198g/cm of density3, porosity 89~95.8%, 256~343m of specific surface area2/ g, 153~158 ° of water contact angle, 0.03531~0.04463W/ of thermal conductivity (mK) have hierarchical pore structure, and nano-pore is distributed in 3~100nm, 0.5~5 μm of micron pore size distribution.PVDF aeroges are made by the physics sol gel process based on phase inversion, PVDF powder and additive are dissolved addition deionized water after mixing in organic solvent under certain temperature makes PVDF that inversion of phases formation PVDF gels occur, and PVDF gels replace and be dried to obtain PVDF aeroges through solvent.The present invention is prepared for novel super-hydrophobic PVDF aerogel materials using a kind of new preparation method, this method is simple for process, it is easy to industrialized production, prepared PVDF aerogel materials have relatively low thermal conductivity, are a kind of thermal insulation materials available in low temperature and moisture environment.

Description

A kind of ultra-hydrophobic polyvinylidene fluoride aerogel material and preparation method thereof
Technical field
The invention belongs to the preparation field of new material, be related to a kind of ultra-hydrophobic polyvinylidene fluoride PVDF aerogel materials and its Preparation method.
Background technology
As a kind of nano-porous materials, aeroge has three-D nano-porous network structure, assigns its low-density, high ratio The characteristics such as surface area, macroporosity can effectively limit heat transmission, be a kind of ideal High Performance Adiabatic material, room temperature Thermal conductivity under normal pressure is the minimum solid of thermal conductivity hereinafter, be significantly better than traditional insulation materials generally in 0.02W/ (mK) Material, available for fields such as industrial production, building energy conservation, aerospaces.Most study and commercialization at present is SiO2 Aerogel insulating material, but SiO2Aeroge intensity is low, brittleness is big, leads to SiO2" picking falls aerogel insulating material generally existing The problem of slag ", this not only limits SiO2The use of aerogel insulating material, is less useful for environmental protection and production and construction personnel are good for Health.SiO can be improved by surface hydrophobicity modification to a certain extent2The scaling-off problem of picking of aeroge, but can not be from basic Upper this problem of change, and surface modification can destroy SiO2The pore structure of aerogel insulating material.Crosslinked polymer modification can To solve SiO2The scaling-off problem of picking of aerogel material, but obtained crosslinked polymer SiO2Aerogel material is from basic On lose the architectural characteristic of aerogel material, performance is closer to traditional plastics.
Invention content
In order to improve the deficiencies in the prior art, the present invention provides a kind of PVDF aerogel materials, another mesh of the invention The preparation method for being to provide material.Prepared PVDF aerogel materials have good flexible, hydrophobicity and thermal insulation, solution Determined traditional hydrophobic SiO2The shortcomings that aerogel material picking is scaling-off.Moreover, prepared by the phase inversion of PVDF aerogel materials It is not chemically reacted in technical process, is physics sol-gel process, relative to traditional SiO2The hydrolysis of aerogel material- Polymerization processes for preparing is simpler, safe and environment-friendly.
The object of the invention technical solution：
A kind of ultra-hydrophobic polyvinylidene fluoride PVDF aerogel materials, it is characterised in that form is White-opalescent block-shaped material Material, 0.075~0.198g/cm of density3, porosity 89~95.8%, 256~343m of specific surface area2/ g, water contact angle 153~ 158 °, 0.03531~0.04463W/ of thermal conductivity (mK), there is hierarchical pore structure, nano-pore is distributed in 3~100nm, 0.5~5 μm of pore size distribution of micron.
The present invention also provides the preparation methods of above-mentioned ultra-hydrophobic polyvinylidene fluoride PVDF aerogel materials, specific to walk It is rapid as follows：
At (1) 70~90 DEG C, add in additive that mass fraction is 1~3% in organic solvent and mass fraction be 5~ 15% PVDF powder obtains clear PVDF solution after stirring；
(2) mass fraction is added to by step as 10~20% deionized water using the speed of 1~5mL/min under lasting stirring Suddenly PVDF colloidal sols are obtained in the PVDF solution obtained in (1)；
(3) the PVDF colloidal sols obtained in step (2) are placed at 10~30 DEG C and carry out sol gel reaction and obtain PVDF and coagulate Glue；
(4) by the PVDF gels obtained in step (3) be placed in 20~30 DEG C alcohol or deionized water in carry out solvent displacement；
(5) alcogel obtained after solvent displacement in step (4) or hydrogel are subjected to CO2Supercritical drying or freezing are dry It is dry to obtain super-hydrophobic PVDF aerogel materials.
Organic solvent described in preferred steps (1) is N-N dimethylformamides, N-N dimethylacetylamides or dimethyl One kind in sulfoxide.
Additive described in preferred steps (1) is one kind in lithium chloride, sodium chloride or polyvinylpyrrolidone.
Mixing time in preferred steps (1) is 20~60 minutes.
Displacement number in preferred steps (4) is 4~8 times, and each time swap is 6~12 hours.
Alcohol described in preferred steps (4) is one kind in methanol, ethyl alcohol or isopropanol.
PVDF aerogel materials prepared by the present invention can be used for the fields such as heat-insulation and heat-preservation, water process, gas absorption.
Advantageous effect：
PVDF aerogel materials according to the present invention are prepared by phase inversion, present invention process method and use PVDF aerogel materials prepared by this method have the characteristics that：
(1) the physics sol-gel technology based on phase inversion is used, avoids traditional Si O2Aerogel material prepares institute Acid/base catalyzing hydrolysis-polymerization technique of use does not need to add in any catalyst in sol-gel process, without chemical reaction, Preparation process is safe and environment-friendly.
(2) the PVDF aerogel materials prepared by not only have good hydrophobic performance and heat-proof quality, but also with good Good flexibility, it is bent, do not lose powder scaling-off, protected available for oil and fuel transport storage facilities thermal insulation material, feature clothes Adiabator etc..
Description of the drawings
Fig. 1 is PVDF aerogel materials material object photo made from example 2.
Fig. 2 is PVDF aerogel materials SEM photograph made from example 2.
Specific embodiment
Example 1
At 70 DEG C, the PVDF powder that sodium chloride and mass fraction that mass fraction is 1% are 5% is added to N-N diformazans In base formamide, stirring obtains clear PVDF solution after twenty minutes, and quality is added in PVDF solution with the speed of 5mL/min The deionized water that score is 20% obtains PVDF colloidal sols；PVDF colloidal sols are placed in progress sol gel reaction at 10 DEG C to obtain PVDF gels；PVDF gels are immersed in solvent displacement 8 times (each time swap is 6 hours) in 20 DEG C of deionized water and obtain water Gel, hydrogel are freeze-dried to obtain super-hydrophobic PVDF aerogel materials.PVDF aeroge sample rates 0.075/g/ cm3, porosity 95.8%, specific surface area 306m2/ g, 153 ° of water contact angle, thermal conductivity 0.04463W/ (mK), nanometer pore size distribution In 3~100nm, micron openings is distributed in 0.5~5 μm.
Example 2
At 80 DEG C, the PVDF powder that lithium chloride and mass fraction that mass fraction is 2% are 10% is added to N-N diformazans In yl acetamide, stirring obtains clear PVDF solution after forty minutes, and quality is added in PVDF solution with the speed of 3mL/min The deionized water of score 15% obtains PVDF colloidal sols；PVDF colloidal sols are placed in progress sol gel reaction at 20 DEG C and obtain PVDF Gel；PVDF gels are immersed in solvent displacement 6 times (each time swap is 8 hours) in 25 DEG C of ethyl alcohol and obtain alcogel, alcohol Gel carries out CO2Supercritical drying obtains super-hydrophobic PVDF aerogel materials.PVDF aeroge sample rates 0.143g/cm3, hole Gap rate 92%, specific surface area 343m2/ g, 158 ° of water contact angle, thermal conductivity 0.03531W/ (mK), nano-pore is distributed in 5~ 80nm, micron openings are distributed in 0.5~3 μm.
Referring to attached drawing, Fig. 1 is PVDF aeroges material object photo made from example 2.It can be seen that prepared PVDF airsettings Glue is the complete bulk material of flawless, and appearance is White-opalescent.
Referring to attached drawing, Fig. 2 is the SEM photograph of PVDF aeroges made from example 2.SEM tests are using German karr Zeiss Company's LEO-1530VP field emission scanning electron microscopes.It can be seen that the PVDF airsettings prepared by the present invention from SEM photograph Glue has hierarchical pore structure：The nanometer skeleton of threadiness is mutually wound in porous ball, and nano-pore is flooded in porous ball；It is micro- Meter level porous ball is interconnected to form PVDF aeroge network structures, and micrometer grade hole is flooded between micron order ball.
Example 3
At 90 DEG C, the PVDF powder that polyvinylpyrrolidone and mass fraction that mass fraction is 3% are 15% is added in Into dimethyl sulfoxide (DMSO), stirring obtains clear PVDF solution after sixty minutes, is added in PVDF solution with the speed of 1mL/min 10% deionized water obtains PVDF colloidal sols；PVDF colloidal sols are placed in progress sol gel reaction at 10 DEG C and obtain PVDF gels； PVDF gels are immersed in solvent displacement 4 times (each time swap is 12 hours) in 30 DEG C of methanol and obtain alcogel, alcogel Carry out CO2Supercritical drying obtains super-hydrophobic PVDF aerogel materials.PVDF aeroge sample rates 0.198g/cm3, porosity 89%, specific surface area 256m2/ g, 154 ° of water contact angle, thermal conductivity 0.04152W/ (mK), nano-pore is distributed in 3~100nm, Micron openings is distributed in 0.8~5 μm.
Example 4
At 80 DEG C, the PVDF powder that lithium chloride and mass fraction that mass fraction is 3% are 10% is added to dimethyl In sulfoxide, stirring obtains clear PVDF solution after forty minutes, and 10% is added in PVDF solution with the speed of 1mL/min and is gone Ionized water obtains PVDF colloidal sols；PVDF colloidal sols are placed in progress sol gel reaction at 30 DEG C and obtain PVDF gels；PVDF gels It is immersed in solvent displacement 6 times (each time swap is 12 hours) in 25 DEG C of isopropanol and obtains alcogel, alcogel carries out CO2 Supercritical drying obtains super-hydrophobic PVDF aerogel materials.PVDF aeroge sample rates 0.147g/cm3, porosity 91.8%, Specific surface area 312m2/ g, 153 ° of water contact angle, thermal conductivity 0.03894W/ (mK), nano-pore are distributed in 5~70nm, micron openings It is distributed in 0.5~2.6 μm.
Example 5
At 90 DEG C, the PVDF powder that polyvinylpyrrolidone and mass fraction that mass fraction is 1% are 15% is added in Into N-N dimethylacetylamides, stirring obtains clear PVDF solution after sixty minutes, with the speed of 3mL/min in PVDF solution The deionized water of middle addition 10% obtains PVDF colloidal sols；PVDF colloidal sols are placed in progress sol gel reaction at 10 DEG C to obtain PVDF gels；PVDF gels, which are immersed in 30 DEG C of ethyl alcohol solvent and replace 8 times (each time swap is 12 hours) and obtain alcohol, to coagulate Glue, alcogel carry out CO2Supercritical drying obtains super-hydrophobic PVDF aerogel materials.PVDF aeroge sample rates 0.186g/ cm3, porosity 89.7%, specific surface area 298m2/ g, 157 ° of water contact angle, thermal conductivity 0.04057W/ (mK), nanometer pore size distribution In 3~100nm, micron openings is distributed in 0.5~5 μm.
Example 6
At 90 DEG C, the PVDF powder that lithium chloride and mass fraction that mass fraction is 3% are 5% is added to N-N diformazans In base formamide, stirring obtains clear PVDF solution after 30 minutes, and 20% is added in PVDF solution with the speed of 5mL/min Deionized water obtain PVDF colloidal sols；PVDF colloidal sols are placed in progress sol gel reaction at 10 DEG C and obtain PVDF gels；PVDF Gel is immersed in solvent displacement 8 times (each time swap is 8 hours) in 20 DEG C of methanol and obtains alcogel, and alcogel carries out CO2Supercritical drying obtains super-hydrophobic PVDF aerogel materials.PVDF aeroge sample rates 0.078g/cm3, porosity 95.7%, specific surface area 264m2/ g, 153 ° of water contact angle, thermal conductivity 0.03998W/ (mK), nano-pore is distributed in 3~ 100nm, micron openings are distributed in 0.5~5 μm.

Claims (7)

1. a kind of ultra-hydrophobic polyvinylidene fluoride PVDF aerogel materials, it is characterised in that form is White-opalescent bulk material, 0.075~0.198g/cm of density3, porosity 89~95.8%, 256~343m of specific surface area2/ g, 153~158 ° of water contact angle, 0.03531~0.04463W/ of thermal conductivity (mK), has hierarchical pore structure, and nano-pore is distributed in 3~100nm, micron openings 0.5~5 μm of distribution.
2. a kind of method for preparing ultra-hydrophobic polyvinylidene fluoride PVDF aerogel materials as described in claim 1, specific to walk It is rapid as follows：
At (1) 70~90 DEG C, addition mass fraction is 1~3% in organic solvent additive and mass fraction are 5~15% PVDF powder, clear PVDF solution is obtained after stirring；
(2) mass fraction is added to by step as 10~20% deionized water using the speed of 1~5mL/min under lasting stirring (1) PVDF colloidal sols are obtained in the PVDF solution obtained in；
(3) the PVDF colloidal sols obtained in step (2) are placed in progress sol gel reaction at 10~30 DEG C and obtain PVDF gels；
(4) by the PVDF gels obtained in step (3) be placed in 20~30 DEG C alcohol or deionized water in carry out solvent displacement；
(5) alcogel obtained after solvent displacement in step (4) or hydrogel are subjected to CO2Supercritical drying is freeze-dried To super-hydrophobic PVDF aerogel materials.
3. preparation method according to claim 2, it is characterised in that the organic solvent described in step (1) is N-N diformazans One kind in base formamide, N-N dimethylacetylamides or dimethyl sulfoxide (DMSO).
4. preparation method according to claim 2, it is characterised in that the additive described in step (1) is lithium chloride, chlorine Change one kind in sodium or polyvinylpyrrolidone.
5. preparation method according to claim 2, it is characterised in that the mixing time in step (1) is 20~60 minutes.
6. preparation method according to claim 2, it is characterised in that the displacement number in step (4) is 4~8 times, every time Time swap is 6~12 hours.
7. preparation method according to claim 2, it is characterised in that the alcohol described in step (4) is methanol, ethyl alcohol or different One kind in propyl alcohol.
CN201711234604.2A 2017-11-30 2017-11-30 A kind of ultra-hydrophobic polyvinylidene fluoride aerogel material and preparation method thereof Pending CN108192129A (en)

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CN108976673A (en) * 2018-07-25 2018-12-11 南京工业大学 A kind of preparation method of 3D fiber support polymer aerogel composite material
CN109499496A (en) * 2018-12-29 2019-03-22 电子科技大学 A kind of flexibility PZT/PVDF composite piezoelectric aerogel material and preparation method thereof
CN109821484A (en) * 2019-03-27 2019-05-31 中国科学院化学研究所 A kind of dipeptides aeroge and the preparation method and application thereof
CN109852165A (en) * 2019-01-29 2019-06-07 长沙理工大学 Super-hydrophobic mud stone modifying agent and preparation method thereof and mud stone modification method
CN110452480A (en) * 2019-09-21 2019-11-15 青岛科技大学 A kind of preparation method of ultra-light heat insulation flexibility aeroge
CN112553914A (en) * 2020-12-01 2021-03-26 苏州大学 Preparation method and application of waterproof heat-insulation coating agent
CN113941299A (en) * 2021-11-15 2022-01-18 常熟理工学院 ZIF-8 modified natural cellulose-polyvinylidene fluoride composite aerogel material for oil-water separation and preparation method thereof
CN115785593A (en) * 2022-12-08 2023-03-14 电子科技大学长三角研究院(衢州) Simple preparation method of high-plasticity super-hydrophobic low-thermal conductivity PVDF aerogel
CN116371218A (en) * 2023-03-07 2023-07-04 嘉兴中芯纳米材料有限责任公司 Preparation method of anti-fouling hydrophobic oleophylic PVDF filter membrane and product thereof
CN116426030A (en) * 2023-04-24 2023-07-14 新疆大学 Preparation method and application of PVC aerogel for separating water-in-oil emulsion

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CN108976673A (en) * 2018-07-25 2018-12-11 南京工业大学 A kind of preparation method of 3D fiber support polymer aerogel composite material
CN109499496A (en) * 2018-12-29 2019-03-22 电子科技大学 A kind of flexibility PZT/PVDF composite piezoelectric aerogel material and preparation method thereof
CN109499496B (en) * 2018-12-29 2021-07-02 电子科技大学 Flexible PZT/PVDF composite piezoelectric aerogel material and preparation method thereof
CN109852165A (en) * 2019-01-29 2019-06-07 长沙理工大学 Super-hydrophobic mud stone modifying agent and preparation method thereof and mud stone modification method
CN109852165B (en) * 2019-01-29 2020-11-13 长沙理工大学 Super-hydrophobic mudstone modifier, preparation method thereof and mudstone improvement method
CN109821484A (en) * 2019-03-27 2019-05-31 中国科学院化学研究所 A kind of dipeptides aeroge and the preparation method and application thereof
CN110452480B (en) * 2019-09-21 2023-04-28 青岛科技大学 Preparation method of ultra-light heat-insulating flexible aerogel
CN110452480A (en) * 2019-09-21 2019-11-15 青岛科技大学 A kind of preparation method of ultra-light heat insulation flexibility aeroge
CN112553914A (en) * 2020-12-01 2021-03-26 苏州大学 Preparation method and application of waterproof heat-insulation coating agent
CN112553914B (en) * 2020-12-01 2022-03-11 苏州大学 Preparation method and application of waterproof heat-insulation coating agent
CN113941299A (en) * 2021-11-15 2022-01-18 常熟理工学院 ZIF-8 modified natural cellulose-polyvinylidene fluoride composite aerogel material for oil-water separation and preparation method thereof
CN113941299B (en) * 2021-11-15 2023-08-22 常熟理工学院 ZIF-8 modified natural cellulose-polyvinylidene fluoride composite aerogel material for oil-water separation and preparation method thereof
CN115785593A (en) * 2022-12-08 2023-03-14 电子科技大学长三角研究院(衢州) Simple preparation method of high-plasticity super-hydrophobic low-thermal conductivity PVDF aerogel
CN116371218A (en) * 2023-03-07 2023-07-04 嘉兴中芯纳米材料有限责任公司 Preparation method of anti-fouling hydrophobic oleophylic PVDF filter membrane and product thereof
CN116371218B (en) * 2023-03-07 2023-09-05 嘉兴中芯纳米材料有限责任公司 Preparation method of anti-fouling hydrophobic oleophylic PVDF filter membrane and product thereof
CN116426030A (en) * 2023-04-24 2023-07-14 新疆大学 Preparation method and application of PVC aerogel for separating water-in-oil emulsion
CN116426030B (en) * 2023-04-24 2024-01-26 新疆大学 Preparation method and application of PVC aerogel for separating water-in-oil emulsion

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Application publication date: 20180622