CN110025985A - It is a kind of to prepare oil-water separation filter paper super hydrophilic oleophobic treatment agent and its application method - Google Patents
It is a kind of to prepare oil-water separation filter paper super hydrophilic oleophobic treatment agent and its application method Download PDFInfo
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- CN110025985A CN110025985A CN201910338280.XA CN201910338280A CN110025985A CN 110025985 A CN110025985 A CN 110025985A CN 201910338280 A CN201910338280 A CN 201910338280A CN 110025985 A CN110025985 A CN 110025985A
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- filter paper
- oil
- super hydrophilic
- water separation
- treatment agent
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- 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
- B01D17/02—Separation of non-miscible liquids
Abstract
The present invention relates to a kind of super hydrophilic oleophobic treatment agent for preparing oil-water separation filter paper and its application method, which is made of nanometer and micron organosilicon filler, active film forming matter, bleeding agent and solvent；The nanometer and micron organosilicon filler is the hydrolysate of amino-silane terminated dose and alkoxy silane；The active film forming matter is the reaction product of epoxy resin, chain extender, fluorochemical, bisphenol compound.The invention also discloses the application methods of the inorganic agent.For inorganic agent of the present invention using simply, the filter paper of acquisition has super hydrophilic fuel shedding quality, can be used for the fields such as oil water mixture separation and oily waste water treatment, is with a wide range of applications.
Description
Technical field
The present invention relates to water-oil separating field, in particular to a kind of oil-water separation filter paper for preparing is with super hydrophilic oleophobic treatment agent
And its application method.
Background technique
A small amount of oil dispersed is a problem in wastewater treatment, oil droplet in the system in the oil-in-water emulsified waste water that water is formed
Partial size is most of at 0.1~2 μm less than 10 μm, therefore has high stability, common oily water separation technique such as gravity point
It is difficult to realize efficiently separate from, ultrasonic separation, dissolved air flotation, centrifugal separation technology；And adsorbent is difficult to weight in absorption method
It is multiple to utilize；Electrochemical process energy consumption is high, need special installation and usually requires additional addition chemical reagent can just higher come out
Effect；Therefore developing the new technology for being suitable for handling oil-in-water emulsified waste water has high market value.
Water-oil separating membrane material is there are two types of implementation method, and one of which is by constructing oleophylic, hydrophobic property, i.e. oil can lead to
It crosses and water cannot pass through, as patent CN105964014A, CN107050928A, CN106868948A, CN108411707A are
Divide material using such method building grease；Another kind is building oleophobic, water-wet behavior, i.e. water can cannot be passed through by oil,
Such patent is very more, if patent CN201310575190.5 is using red copper net as substrate, is first constructed with solution infusion method micro-nano
Acicular texture is surface modified acquisition with polydimethyl diallyl ammonium chloride-Sodium perfluorooctanoate/silica composite again
The material of the performance；Patent CN201810754081.2 discloses one kind and quickly prepares super hydrophilic/underwater superoleophobic stainless (steel) wire
Method, method are that the concentrated sulfuric acid for being 98% by mass fraction is mixed with 2mol/L chromium trioxide solution according to volume ratio 1:4, are stirred
It mixes uniformly, obtains mixed solution；It is dried after 350 mesh stainless (steel) wires are cleaned by ultrasonic in dehydrated alcohol, deionized water respectively, so
Clean stainless (steel) wire is immersed into 3min in mixed solution at room temperature afterwards；Stainless (steel) wire drying after immersion is obtained super close
Water/underwater superoleophobic stainless (steel) wire.Filter paper is a kind of common separation material, is usually used in separating the molecule in liquid, lead to
It crosses and is modified the material and can be used for water-oil separating.It is simple etc. with high efficiency, low energy consumption, equipment that water-oil separating is carried out using filter paper
Advantage, therefore have a good application prospect.It is retrieved, it is found that patent document disclosure relevant to the application is as follows:
Patent CN201610548449.0 provides a kind of copolymer with pH responsiveness, by the copolymer and titanium dioxide
Silicon nano formed a mixed solution, be then prepared for by way of dip-coating pH responsiveness two-dimensional film material (cotton,
Filter paper) and three-dimensional sponge material (polyurethane sponge).Patent CN201710723713.4 discloses a kind of high-intensitive self-supporting
Water-oil separationg film and preparation method thereof comprising following steps: by monomer, clay and thermal initiator is soluble in water is configured to pre-polymerization
Liquid；Resulting pre-polymerization liquid is poured into the filter equipped with water system filter membrane and is filtered, the performed polymer being concentrated；Then with pre-
Columnar arrays template is covered above the filter paper of aggressiveness, is put into hot press, is polymerize under the action of certain pressure and temperature and is generated
With the aquagel membrane for running through array pore structure.Patent CN201811542523.3 provides one metal ion species/Arabic gum
The preparation method and its usage of the modified composite membrane of gel, using graphene oxide, Arabic gum and metal salt as raw material, by molten
Sol-gel constructs coarse hydrophilic-structure in substrate surfaces such as stainless (steel) wire, copper mesh, pvdf membrane, ordinary filter papers, prepares super close
Water/modified the composite membrane of underwater superoleophobic graphene oxide/Arabic gum gel.Patent CN201810603729.6 discloses one
It plants and the preparation method that oil hydrosol separates the functional membrane removed with dyestuff can be achieved at the same time, including (1) prepared polymer matrix is molten
Liquid, (2) by the substrate of hydroxyl in conjunction with polymer matrix liquid solution, a step, which is realized, accelerates gelation and introducing charged functional groups,
Obtain can be achieved at the same time the functional membrane of oil hydrosol separation and dyestuff removal.The invention is assigned by polymer matrix liquid solution contains hydroxyl
The substrate high-ratio surface energy of base and obtain super hydrophilic, underwater superoleophobic property, and then can realize efficiently separating for grease.
Summary of the invention
The present invention be directed to super hydrophilic oleophobic water-oil separating material preparation process complexity problem, provide it is a kind of prepare grease divide
From the super hydrophilic oleophobic treatment agent of filter paper, the inorganic agent effect is obvious, uses simplicity.
The technical solution adopted by the invention is as follows: a kind of prepare the super hydrophilic oleophobic treatment agent of oil-water separation filter paper, spy
Sign is:
Nano-organosilicon filler and micron organosilicon filler 0.5~5%；
Active film forming matter 1~8%；
Bleeding agent 0.1~2；
Balance of solvent；
The nano-organosilicon filler and micron organosilicon filler are the hydrolysis of amino-silane terminated dose and alkoxy silane
Product, surface carry a large amount of amino group；
The activity film forming matter is the reaction product of epoxy resin, chain extender, fluorochemical, bisphenol compound；
The bleeding agent is fatty alcohol polyethenoxy ether class surfactant；
The solvent is water, ethyl alcohol, propyl alcohol, isopropanol, ethylene glycol, methanol ethylene glycol, ethylene glycol monoethanol, 1,3 2
At least one of oxygen Polymorphs Anhui, dioxane can make nanometer and micron organosilicon filler, active film forming matter, bleeding agent
Dispersion well.
Wherein amino-silane terminated dose of structure is as follows；
Wherein R1For linking group-CH2CH2-S-CH2CH2Or-CH2CH2CH2-；Alkoxy silane be tetramethoxy-silicane,
Tetraethoxysilane or their mixture.
Wherein chain extender is ethamine, propylamine, butylamine, ethanol amine, amino acid or their mixture；Fluorochemical is
CF3(CF2CF2)n-(CH2CH2O)m-R2-NH2, it is 2~9, R that wherein n, which is 2~9, m,2For linking group-CH2,-CH2CH2Or-
COCH2CH2-；The structure of bisphenol compound is as follows
Wherein R3For linking group such as-CH2,-CH2CH2Or-CH2CH2CH2-；On the one hand chain extender improves point of resin
Son amount, on the other hand adjusts hydrophilicity；Fluorochemical assigns material oleophobic performance；Bisphenol compound can occur even with amino
Connection reaction, makes active film forming matter crosslink raising intensity, and be capable of fixing nanometer and micron organosilicon filler forms stabilization
Micro nano structure.
Further, the nano-organosilicon packing material size is 10~50nm, and micron organosilicon packing material size is 0.5~3 μ
M calculates by weight 0.3~1 that nanofiller dosage is micron filler.
Further, in the active film forming matter, chain extender, fluorochemical, bisphenol compound are calculated by molar amount,
Ratio is (0.5~0.7): (0.2~0.3): (0.2~0.3).
The oil-water separation filter paper application method of super hydrophilic oleophobic treatment agent is prepared the present invention also provides a kind of, comprising:
(1) inorganic agent is diluted to solid part is 1%；
(2) filter paper is placed in Bush's funnel, by inorganic agent into Bush's funnel,
(3) it is filtered using vacuum pump；
(4) filter paper that will be handled well, as dry at 50~90 DEG C.
Compared with the existing technology, the beneficial effects of the present invention are embodied in: (1) inorganic agent is easy to use, does not need complexity and sets
It is standby, it is easy to operate；(2) super hydrophilic oleophobic effects are significant, and prepared grease can be used for water-oil separating from filter paper, effectively remove
Greasy dirt in oily waste water is all with a wide range of applications in chemical separating and field of water pollution control.
Detailed description of the invention
Fig. 1 is untreated filter paper shape appearance figure of the invention；
Fig. 2 is filter paper shape appearance figure in the embodiment of the present invention 1.
Specific embodiment
Present invention is further described in detail with reference to embodiments, it should be pointed out that embodiment described below purport
It is being convenient for the understanding of the present invention, and is not playing any restriction effect to it.The experiment of actual conditions is not specified in the following example
Method, usually according to normal condition.Unless otherwise stated, otherwise all score is parts by weight, and all percentage is weight
Percentage.
Active film forming matter A
Epoxy resin E44 51g is dissolved in 105ml ethylene glycol monoethanol, ethanol amine 4g, fluorochemical is then added
8.5g(CF3(CF2CF2)2(CH2CH2O)2CH2CH2NH2) and 4- (2- ethylamino-) benzene -1,2- diphenol 6.5g, mechanical stirring,
80 DEG C are heated under nitrogen protection to react 1 hour.
Active film forming matter B
Epoxy resin E44 51g is dissolved in 101ml ethylene glycol monoethanol, ethanol amine 2g, butylamine 3.2g is then added, contains
Fluorine compounds 4.4g (CF3(CF2CF2)2(CH2CH2O)2CH2CH2NH2) and 4- (2- ethylamino-) benzene -1,2- diphenol 6.7g, it is mechanical
Stirring is heated to 80 DEG C under nitrogen protection and reacts 1 hour.
Embodiment 1
Take above-mentioned active film forming matter solution A 175g, nano-organosilicon filler (average diameter 30nm) 10g, micron organic
Silicon filler (2 μm of average diameter) 20g, bleeding agent 3g adds 970g ethylene glycol monoethanol to dilute, admittedly contain 10%.
It takes above-mentioned inorganic agent that ethylene glycol monoethanol is added further to be diluted to 1%, the Medium speed filter paper that diameter is 20cm is placed in
In Bush's funnel, takes 1% concentration inorganic agent of 50ml into Bush's funnel, filtered using vacuum cycle water pump, by filter paper,
It is placed at 60 DEG C one hour dry.
The contact angle of the filter paper water is 3 ° after measured, 89 ° of the contact angle of petroleum ether.Folded filter paper funnel was placed in
It filters in funnel.By oil field ether (60~90 DEG C of boiling point) and deionized water by volume 1:50 ratio mix, high speed disperser
Oil water mixture is stirred into, is poured into filter paper, oil water mixture efficiently separates, and separative efficiency can reach 99.7% or more.The filter
Paper stability is good, reusable.
Embodiment 2
It is other same as Example 1, only change the Medium speed filter paper that diameter is 20cm into fast grade filter paper.
The contact angle of the filter paper water is 15 ° after measured, 78 ° of folded filter paper funnel merging filterings of contact angle of petroleum ether
In funnel.The ratio of oil field ether (60~90 DEG C of boiling point) and deionized water 1:50 by volume are mixed, high speed disperser stirs
Oil water mixture is mixed, is poured into filter paper, oil water mixture efficiently separates, and separative efficiency can reach 95.7% or more.The filter paper
Stability is good, reusable.
Embodiment 3
Above-mentioned active film forming matter solution A 175g, bleeding agent 3g are taken, 657g ethylene glycol monoethanol is added to dilute, admittedly contain 10%.
It takes above-mentioned inorganic agent that ethylene glycol monoethanol is added further to be diluted to 1%, the Medium speed filter paper that diameter is 20cm is placed in
In Bush's funnel, takes 1% concentration inorganic agent of 50ml into Bush's funnel, filtered using vacuum cycle water pump, by filter paper,
It is placed at 60 DEG C one hour dry.
The contact angle of the filter paper water is 40 ° after measured, 65 ° of the contact angle of petroleum ether.Folded filter paper funnel was placed in
It filters in funnel.By oil field ether (60~90 DEG C of boiling point) and deionized water by volume 1:50 ratio mix, high speed disperser
Oil water mixture is stirred into, is poured into filter paper, oil water mixture efficiently separates, and separative efficiency can reach 50.1% or more.The filter
Paper stability is good, reusable.
Embodiment 4
Active film forming matter B solution 168g is taken, nano-organosilicon filler (average diameter 30nm) 15g, micron organosilicon are filled out
Expect (2 μm of average diameter) 35g, bleeding agent 3g, 650g ethylene glycol monoethanol is added to dilute, admittedly contain 15%.
It takes above-mentioned inorganic agent that ethylene glycol monoethanol is added further to be diluted to 1.5%, the Medium speed filter paper that diameter is 20cm is set
In Bush's funnel, takes 1% concentration inorganic agent of 50ml into Bush's funnel, filtered, will be filtered using vacuum cycle water pump
Paper is placed at 60 DEG C one hour dry.
The contact angle of the filter paper water is 20 ° after measured, 75 ° of the contact angle of petroleum ether.Folded filter paper funnel was placed in
It filters in funnel.By oil field ether (60~90 DEG C of boiling point) and deionized water by volume 1:50 ratio mix, high speed disperser
Oil water mixture is stirred into, is poured into filter paper, oil water mixture efficiently separates, and separative efficiency can reach 70.7% or more.
Comparative example 1
The contact angle of Medium speed filter paper water is 1 °, 0 ° of the contact angle of petroleum ether.Folded filter paper funnel is placed in filter tunnel
In.The ratio of oil field ether (60~90 DEG C of boiling point) and deionized water 1:50 by volume are mixed, high speed disperser stirs into
Oil water mixture pours into filter paper, and grease cannot separate.
Technical solution of the present invention is described in detail in embodiment described above, it should be understood that the above is only
For specific embodiments of the present invention, it is not intended to restrict the invention, all any modifications made in spirit of the invention,
Supplement or equivalent replacement etc., should all be included in the protection scope of the present invention.
Claims (6)
1. a kind of oil-water separation filter paper for preparing is with super hydrophilic oleophobic treatment agent, it is characterised in that:
Nano-organosilicon filler and micron organosilicon filler 0.5~5%；
Active film forming matter 1~8%；
Bleeding agent 0.1~2；
Balance of solvent；
The nano-organosilicon filler and micron organosilicon filler are the hydrolysate of amino-silane terminated dose and alkoxy silane,
Surface carries a large amount of amino group；
The activity film forming matter is the reaction product of epoxy resin, chain extender, fluorochemical, bisphenol compound；
The bleeding agent is fatty alcohol polyethenoxy ether class surfactant；
The solvent is water, ethyl alcohol, propyl alcohol, isopropanol, ethylene glycol, methanol ethylene glycol, ethylene glycol monoethanol, 1,3 dioxas
At least one of penta Anhui of ring, dioxane.
2. a kind of oil-water separation filter paper for preparing according to claim 1 is with super hydrophilic oleophobic treatment agent, it is characterised in that: its
In amino-silane terminated dose structure it is as follows；
Wherein R1For linking group-CH2CH2-S-CH2CH2Or-CH2CH2CH2-；Alkoxy silane is tetramethoxy-silicane, tetrem
Oxysilane or their mixture.
3. a kind of oil-water separation filter paper for preparing according to claim 1 is with super hydrophilic oleophobic treatment agent, it is characterised in that: its
Middle chain extender is ethamine, propylamine, butylamine, ethanol amine, amino acid or their mixture；Fluorochemical is CF3(CF2CF2)n-
(CH2CH2O)m-R2-NH2, it is 2~9, R that wherein n, which is 2~9, m,2For linking group-CH2,-CH2CH2Or-COCH2CH2-；Bis-phenol
The structure of compound is as follows
Wherein R3For linking group such as-CH2,-CH2CH2Or-CH2CH2CH2-。
4. a kind of oil-water separation filter paper for preparing according to claim 1 is with super hydrophilic oleophobic treatment agent, it is characterised in that: institute
Stating nano-organosilicon packing material size is 10~50nm, and micron organosilicon packing material size is 0.5~3 μm, calculates by weight nanometer and fills out
Expect that dosage is the 0.3~1 of micron filler.
5. a kind of oil-water separation filter paper for preparing according to claim 1 is with super hydrophilic oleophobic treatment agent, it is characterised in that: institute
It states in active film forming matter, chain extender, fluorochemical, bisphenol compound are calculated by molar amount, and ratio is (0.5~0.7):
(0.2~0.3): (0.2~0.3).
6. one kind is according to claim 1 to prepare the oil-water separation filter paper application method of super hydrophilic oleophobic treatment agent, packet
It includes:
(1) inorganic agent is diluted to solid part is 1%；
(2) filter paper is placed in Bush's funnel, by inorganic agent into Bush's funnel；
(3) it is filtered using vacuum pump；
(4) filter paper that will be handled well, as dry at 50~90 DEG C.
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| CN201910338280.XA CN110025985B (en) | 2019-04-25 | 2019-04-25 | Super-hydrophilic oil-repellent treatment agent for preparing oil-water separation filter paper and using method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112982030A (en) * | 2021-02-04 | 2021-06-18 | 西安理工大学 | Preparation method of super-hydrophilic/underwater super-oleophobic filter paper |
| CN113772667A (en) * | 2021-07-23 | 2021-12-10 | 西北民族大学 | Graphene oxide-based porous photothermal material capable of efficiently generating solar steam, and preparation method and application thereof |
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| CN1580397A (en) * | 2003-08-11 | 2005-02-16 | 王剑光 | Chemical Modifying method of filter paper core for oil-water separating filter |
| CN105771322A (en) * | 2016-05-19 | 2016-07-20 | 山东交通学院 | Super hydrophilic oil-water separation filter paper and preparation method thereof |
| CN109603302A (en) * | 2018-12-20 | 2019-04-12 | 东南大学 | Antifouling modified walnut shell filtering material of one kind and its preparation method and application |
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2019
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1580397A (en) * | 2003-08-11 | 2005-02-16 | 王剑光 | Chemical Modifying method of filter paper core for oil-water separating filter |
| CN105771322A (en) * | 2016-05-19 | 2016-07-20 | 山东交通学院 | Super hydrophilic oil-water separation filter paper and preparation method thereof |
| CN109603302A (en) * | 2018-12-20 | 2019-04-12 | 东南大学 | Antifouling modified walnut shell filtering material of one kind and its preparation method and application |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112982030A (en) * | 2021-02-04 | 2021-06-18 | 西安理工大学 | Preparation method of super-hydrophilic/underwater super-oleophobic filter paper |
| CN112982030B (en) * | 2021-02-04 | 2023-06-23 | 陕西鸿鑫耐斯环保科技有限公司 | Preparation method of super-hydrophilic/underwater super-oleophobic filter paper |
| CN113772667A (en) * | 2021-07-23 | 2021-12-10 | 西北民族大学 | Graphene oxide-based porous photothermal material capable of efficiently generating solar steam, and preparation method and application thereof |
| CN113772667B (en) * | 2021-07-23 | 2023-11-10 | 西北民族大学 | Graphene oxide-based porous photo-thermal material capable of efficiently generating solar steam and preparation method and application thereof |
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