CN110404296A - A kind of super wetability water-oil separating material and the preparation method and application thereof - Google Patents
A kind of super wetability water-oil separating material and the preparation method and application thereof Download PDFInfo
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- CN110404296A CN110404296A CN201910711466.5A CN201910711466A CN110404296A CN 110404296 A CN110404296 A CN 110404296A CN 201910711466 A CN201910711466 A CN 201910711466A CN 110404296 A CN110404296 A CN 110404296A
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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
- B01D17/0202—Separation of non-miscible liquids by ab- or adsorption
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Abstract
The invention belongs to polyurethane material field, a kind of super wetability water-oil separating material and the preparation method and application thereof is disclosed.The super wetability water-oil separating material is prepared by the following steps to obtain: synthesis of polyurethane first, then polyurethane solutions are dried and polyurethane film is made, make polyurethane film water absorption and swelling that polyurethane hydrogel film be made again, finally polyurethane hydrogel film is punched, cellular polyurethane hydrogel water-oil separationg film is made.In the separation process that oil-water separation divides mixture, hydrophily and underwater oleophobic property due to cellular polyurethane hydrogel water-oil separationg film, oil cannot mutually be penetrated from seperation film and is trapped, and water phase can pass through mesh, to realize that grease efficiently separates.Processing (acidleach, the alkali leaching) under various harsh environments, cellular polyurethane hydrogel water-oil separationg film still keeps certain oil interception capacity, and the separative efficiency of cellular polyurethane hydrogel water-oil separationg film oil water mixture can still keep 99% or more.
Description
Technical field
The present invention relates to polyurethane material field, in particular to a kind of super wetability water-oil separating material and preparation method thereof
With application.
Background technique
The hydrogel material for being currently used for water-oil separating requires to rely on the bases such as stainless (steel) wire, copper mesh, textile substantially
Material.It is a complicated process that hydrogel material, which is coated on substrate, and improves hydrogel adhesive force on base material and be
A major challenge, carry out oil water separation process for a long time in use, coating material often deficient in stability, be easy to take off from substrate
It falls, this severely limits the practical applications that these surpass wet material.
Summary of the invention
In order to overcome the shortcomings and deficiencies of the prior art described above, primary and foremost purpose of the present invention is to provide a kind of super wetability oil
The preparation method of water separation material.
Another object of the present invention is to provide the super wetability water-oil separating material that the above method is prepared.
Still a further object of the present invention is to provide application of the above-mentioned super wetability water-oil separating material in water-oil separating field.
The purpose of the present invention is realized by following proposal:
A kind of preparation method of super wetability water-oil separating material, comprising the following steps:
(1) it synthesis of polyurethane: after polyethylene glycol and solvent A are mixed, dissolves by heating, two isocyanide of isophorone is then added
Acid esters and catalyst carry out temperature reaction, cool down after the reaction was completed, add the mixed solution of solvent B and water, are stirred anti-
Should after obtain polyurethane solutions；
(2) preparation of polyurethane film: polyurethane solutions obtained by step poly- (1) are placed in container, then dry solvent,
Polyurethane film is obtained after cooling；
(3) preparation of polyurethane hydrogel film: polyurethane film made from step (2) is immersed in the water, until being swelling to flat
Weigh water content, obtains polyurethane hydrogel film；
(4) the polyurethane hydrogel film in step (3) preparation of super wetability water-oil separating material: is subjected to punching work
Sequence obtains super wetability water-oil separating material.
Step (1) solvent A and solvent B independently are DMAC N,N' dimethyl acetamide, N,N-dimethylformamide and two
At least one of methyl sulfoxide；
The molal weight of step (1) described polyethylene glycol is 500-8000g/mol.
The mass volume ratio of step (1) polyethylene glycol and solvent A is 0.1~2g/mL, preferably 0.125~0.8g/
mL。
Step (1) catalyst be dibutyl tin dilaurate, stannous octoate and dibutyltin diacetate at least
It is a kind of.
The mass volume ratio of step (1) polyethylene glycol, isophorone diisocyanate and dibutyl tin dilaurate
For 1~20g；The μ of 1~5g:10~40 L；Preferably 2~16g:3.334g:20 μ L.
In the mixed solution of step (1) the solvent B and water, the volume ratio of water and solvent B are 0.2~0.8:20~80,
Preferably 0.3~0.5:20~40.
Volume ratio 1:1~1:4 of step (1) solvent A and solvent B.
Temperature when step (1) described heating for dissolving is 25~60 DEG C；The temperature reaction is to be warming up to 60~90 DEG C instead
Answer 3~12h；The cooling is to be cooled to 25-40 DEG C；The time being stirred to react is 15~36h.
The solid content of polyurethane solutions obtained by step (1) is 10-40%.
The temperature of step (2) described drying is 25~90 DEG C.
The water content of polyurethane hydrogel film obtained by step (3) is 50~90%.
Step (4) drilling process is that microneedle processes drill process, and using microneedle array punching, (schematic diagram is as schemed
Shown in 1), 50~500 μm, preferably 200~300 μm are divided between two needles of transverse and longitudinal in the microneedle array；It is used
Needle diameter is 150-1000 μm, preferably 250-500 μm.
A kind of super wetability water-oil separating material that the above method is prepared.
Application of the above-mentioned super wetability water-oil separating material in water-oil separating field.
The present invention compared with the existing technology, have the following advantages and the utility model has the advantages that
(1) the cellular polyurethane hydrogel water-oil separationg film invented has high mechanical strength, with traditional water-oil separating material
Than it is not necessarily to rely on substrate support；Process is easy to operate, is suitable for industrialized production；
(2) there is underwater superoleophobic property, underwater contact of the organic oil in cellular polyurethane hydrogel water-oil separationg film
Angle is up to 150 ± 10 DEG C.Only by gravity drive, the maximum pressure of receiving still is able to reach 300 ± 100Pa oil water separation process.
(3) there is acid and alkali-resistance property, still be able to keep underwater superoleophobic property under different pH aqueous solutions.
(4) separative efficiency with higher, separative efficiency is up to 99 ± 0.9%.
(5) there is sustainable character of use, after impregnating 7 days in water, organic oil is in cellular polyurethane hydrogel grease point
Underwater contact angle from film still is able to be maintained at 150 ± 10 °, and the maximum pressure of receiving still is able to reach 300 ± 100Pa.
Detailed description of the invention
Fig. 1 is drilling process schematic diagram of the present invention.
Fig. 2 is one of duct microscope figure of the polyurethane hydrogel water-oil separationg film prepared in embodiment 1, wherein
Scale overall length is 1mm.
Fig. 3 is the water-oil separating schematic diagram of cellular polyurethane hydrogel water-oil separationg film in embodiment 4, wherein figure (a) is
Oily-water seperating equipment figure, figure (b) are oil water separation process figure, and figure (c) is oil-water separation figure.
Fig. 4 is that the breakthrough pressure of cellular polyurethane hydrogel water-oil separationg film in embodiment 4 tests schematic diagram.
Fig. 5 is the graph of stretch performance of cellular polyurethane hydrogel water-oil separationg film in embodiment 4.
Specific embodiment
Below with reference to embodiment and attached drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited
In this.
Agents useful for same can routinely be bought unless otherwise specified from market in embodiment.
Embodiment 1
A kind of cellular polyurethane hydrogel water-oil separationg film, is prepared particular by following steps:
(1) synthesis of polyurethane.
Equipped with mechanical agitator, condenser pipe drying three-necked flask in be added 2.5g polyethylene glycol (500g/mol) and
20mL n,N-dimethylacetamide is heated to 60 DEG C of dissolutions.3.334g isophorone diisocyanate and 20 μ L, bis- laurel is added
Sour dibutyl tin is warming up to 80 DEG C of reaction 5h.Then 40 DEG C are cooled to, 0.36g water is measured and is dissolved in 20mL N, N- dimethyl second
In amide and three-necked flask is added, reacts 36h.Obtain the polyurethane solutions that solid content is 13%.
(2) polyurethane solutions, which are dried, is made polyurethane film.
13% solid content polyurethane solution obtained by step poly- (1) is poured into glass culture dish, 45 DEG C of constant temperature drums are placed in
Wind baking oven 12h is trained polyurethane film from glass with completely, obtaining polyurethane film up to the volatilization of n,N-dimethylacetamide solvent
It is taken off in feeding ware spare.
(3) polyurethane hydrogel film is made in polyurethane film water absorption and swelling.
Polyurethane film made from step (2) is immersed in the water 12h, water absorption and swelling to equilibrium moisture content obtains polyurethane water
Gel mould.
(4) polyurethane hydrogel film, which punches, is made cellular polyurethane hydrogel water-oil separationg film.
Polyurethane hydrogel film in step (3) is subjected to drilling process, the interval of two needles of transverse and longitudinal in microneedle array
It is 250 μm, taking diameter is that 300 μm of needle makees micropore syringe needle, obtains cellular polyurethane hydrogel water-oil separationg film.
Embodiment 2
A kind of cellular polyurethane hydrogel water-oil separationg film, is prepared particular by following steps:
(1) synthesis of polyurethane.
Equipped with mechanical agitator, condenser pipe drying three-necked flask in be added 10g polyethylene glycol (2000g/mol) and
20mL n,N-dimethylacetamide is heated to 60 DEG C of dissolutions.3.334g isophorone diisocyanate and 20 μ L, bis- laurel is added
Sour dibutyl tin is warming up to 80 DEG C of reaction 5h.Then 40 DEG C are cooled to, 0.36g water is measured and is dissolved in 40mL N, N- dimethyl second
In amide and three-necked flask is added, reacts 36h.Obtain the polyurethane solutions that solid content is 20%.
(2) polyurethane solutions, which are dried, is made polyurethane film.
20% solid content polyurethane solution obtained by step poly- (1) is poured into glass culture dish, 45 DEG C of constant temperature drums are placed in
Wind baking oven 12h is trained polyurethane film from glass with completely, obtaining polyurethane film up to the volatilization of n,N-dimethylacetamide solvent
It is taken off in feeding ware spare.
(3) polyurethane hydrogel film is made in polyurethane film water absorption and swelling.
Polyurethane film made from step (2) is immersed in the water 12h, water absorption and swelling to equilibrium moisture content obtains polyurethane water
Gel mould.
(4) polyurethane hydrogel film, which punches, is made cellular polyurethane hydrogel water-oil separationg film.
Polyurethane hydrogel film in step (3) is subjected to drilling process, the interval of two needles of transverse and longitudinal in microneedle array
It is 250 μm, taking diameter is that 200 μm of needle makees micropore syringe needle, obtains cellular polyurethane hydrogel water-oil separationg film.
Embodiment 3
A kind of cellular polyurethane hydrogel water-oil separationg film, is prepared particular by following steps:
(1) synthesis of polyurethane.
Equipped with mechanical agitator, condenser pipe drying three-necked flask in be added 16g polyethylene glycol (8000g/mol) and
20mL n,N-dimethylacetamide is heated to 60 DEG C of dissolutions.3.334g isophorone diisocyanate and 20 μ L, bis- laurel is added
Sour dibutyl tin is warming up to 80 DEG C of reaction 5h.Then 40 DEG C are cooled to, 0.46g water is measured and is dissolved in 40mL N, N- dimethyl second
In amide and three-necked flask is added, reacts 36h.Obtain the polyurethane solutions that solid content is 25%.
(2) polyurethane solutions, which are dried, is made polyurethane film.
25% solid content polyurethane solution obtained by step poly- (1) is poured into glass culture dish, 45 DEG C of constant temperature drums are placed in
Wind baking oven 12h is trained polyurethane film from glass with completely, obtaining polyurethane film up to the volatilization of n,N-dimethylacetamide solvent
It is taken off in feeding ware spare.
(3) polyurethane hydrogel film is made in polyurethane film water absorption and swelling.
Polyurethane film made from step (2) is immersed in the water 12h, water absorption and swelling to equilibrium moisture content obtains polyurethane water
Gel mould.
(4) polyurethane hydrogel film, which punches, is made cellular polyurethane hydrogel water-oil separationg film.
Polyurethane hydrogel film in step (3) is subjected to drilling process, the interval of two needles of transverse and longitudinal in microneedle array
It is 250 μm, taking diameter is that 300 μm of needle makees micropore syringe needle, obtains cellular polyurethane hydrogel water-oil separationg film.
Embodiment 4
(1) underwater contact angle of the different organic oils in cellular polyurethane hydrogel water-oil separationg film
Cellular polyurethane hydrogel water-oil separationg film prepared by embodiment 1 is immersed in the water by step 1
Step 2, measurement n-hexane, hexadecane, toluene, peanut oil, pump oil, diiodomethane are in cellular polyurethane hydrogel oil
The underwater contact angle of water seperation film.
Underwater oily contact angle experiments numerical value of the different organic oils of table 1 in cellular polyurethane hydrogel water-oil separationg film.
As shown in table 1, the underwater contact of the polyurethane hydrogel water-oil separationg film under water of various organic oils described in step 2
Angle is at 150 ± 10 °.
(2) the resistance to harsh environment experiment of cellular polyurethane hydrogel water-oil separationg film
Step 1, the cellular polyurethane hydrogel water-oil separationg film for preparing embodiment 2 immerse the acid or alkali that pH value is 0-14
Solution.
Step 2, under different pH solution environmentals, measure hexadecane in the underwater of cellular polyurethane hydrogel water-oil separationg film
Contact angle.
Underwater contact angle of the 2 cellular polyurethane hydrogel water-oil separationg film of table in the hexadecane of different pH environment.
As shown in table 2, in 14 pH value solution environmentals of 0-14, hexadecane is in cellular polyurethane hydrogel water-oil separating
The underwater contact angle of film is all larger than 150 °.
(3) a kind of oil-water separation test of cellular polyurethane hydrogel water-oil separationg film and separative efficiency test
Step 1 measures 20mL n-hexane and the water mixing of 20mL, and water water soluble dyestuffs contaminate blue, n-hexane oiliness dyestuff
It incarnadines.
Step 2 takes two glass apparatus for similarly having flange base to be open on one side, and base openings, which merge, places, then
The cellular polyurethane hydrogel water-oil separationg film prepared in embodiment 2 is placed on to the centre of two glass apparatus flange bases,
And glass apparatus that two flange bases are open, cellular polyurethane hydrogel water-oil separationg film are fixed together with clip.(tool
Body structure is as shown in Figure 3).
The oil water mixture of 40mL described in step 1 is poured into glass apparatus described in step 2, specific grease from top by step 3
Separation process schematic diagram is as shown in Figure 3.The water that can be seen that and be colored from Fig. 3 (c) can penetrate cellular polyurethane water-setting
Glue water-oil separationg film flows to the lower section oily phase n-hexane being caught, and be colored by beaker due to cellular polyurethane hydrogel grease point
From the top that the underwater superoleophobic property of film is trapped within glass separation.
Step 4, the water for taking beaker to be collected into measure oil content in the water being collected into simultaneously with infrared oil content analyzer
Obtain separative efficiency.Point of the water-oil separating experiment of cellular polyurethane hydrogel water-oil separationg film prepared by embodiment 2
It is 99.9% from efficiency, illustrates to be practically free of n-hexane in the water being collected into, separating effect is preferable.
(4) the breakthrough pressure experiment of a kind of cellular polyurethane hydrogel water-oil separationg film
Step 1 takes two glass apparatus for similarly having flange base to be open on one side, and base openings, which merge, places, then
The cellular polyurethane hydrogel water-oil separationg film prepared in embodiment 2 is placed on to the centre of two glass apparatus flange bases,
And glass apparatus that two flange bases are open, cellular polyurethane hydrogel water-oil separationg film are fixed together with clip.(tool
Body structure is as shown in Figure 4)
Step 2 slowly pours into n-hexane in glass tube upwards.
The height of n-hexane above when step 3, record n-hexane flow into lower section glass tube from top glass tube, this is highly
The maximum n-hexane height that can be born for cellular polyurethane hydrogel water-oil separationg film；
Step 4, according to formula p=ρ gh, wherein ρ is the density of n-hexane, and g is acceleration of gravity, and h is maximum n-hexane
Highly, the cellular polyurethane hydrogel water-oil separationg film breakthrough pressure is calculated to obtain.
Step 5 impregnates a kind of cellular polyurethane hydrogel water-oil separationg film 7 days in water, daily according to step 1 to step
Rapid 4 n-hexane breakthrough pressure.
As shown in figure 4, the breakthrough pressure of cellular polyurethane hydrogel water-oil separationg film prepared in embodiment 2 is
330Pa illustrates in oil water separation process, when oil water mixture is added, as long as the pressure that the n-hexane being added generates exists
330Pa or less can guarantee that n-hexane can not be by cellular polyurethane hydrogel water-oil separationg film.Prepared by after impregnating 7 days
The prominent pressure of the n-hexane of cellular polyurethane hydrogel water-oil separationg film is almost unchanged, illustrates the polyurethane hydrogel grease of preparation
Isolated water resistance is preferable.
(4) a kind of stretching experiment of cellular polyurethane hydrogel water-oil separationg film
Cellular polyurethane hydrogel water-oil separationg film prepared by embodiment 2 is cut 15mm*20mm*1.5mm rectangle by step 1
Fritter.
Step 2 carries out extension test with omnipotent mechanical test instrument.Obtain a kind of cellular polyurethane hydrogel water-oil separationg film
Stretching experiment data.
As shown in figure 5, a kind of cellular polyurethane hydrogel water-oil separating membrane stress is greater than 150kPa, it is strong with high mechanics
Degree, illustrates in oil water separation process, will not rupture because of hydraulic pressure or oil pressure.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of super wetability water-oil separating material, which comprises the following steps:
(1) it synthesis of polyurethane: after polyethylene glycol and solvent A are mixed, dissolves by heating, isophorone diisocyanate is then added
Temperature reaction is carried out with catalyst, cools down after the reaction was completed, the mixed solution of solvent B and water is added, after being stirred to react
Obtain polyurethane solutions；
(2) preparation of polyurethane film: polyurethane solutions obtained by step poly- (1) are placed in container, then dry solvent, cooling
After obtain polyurethane film；
(3) preparation of polyurethane hydrogel film: polyurethane film made from step (2) is immersed in the water, and is contained until being swelling to balance
Water obtains polyurethane hydrogel film；
(4) preparation of super wetability water-oil separating material: the polyurethane hydrogel film in step (3) is subjected to drilling process, is obtained
To super wetability water-oil separating material.
2. the preparation method of wetability water-oil separating material according to claim 1, it is characterised in that:
Step (1) solvent A and solvent B independently are DMAC N,N' dimethyl acetamide, N,N-dimethylformamide and dimethyl
At least one of sulfoxide；
Step (1) catalyst is at least one of dibutyl tin dilaurate, stannous octoate and dibutyltin diacetate.
3. the preparation method of wetability water-oil separating material according to claim 2, it is characterised in that:
The mass volume ratio of step (1) polyethylene glycol, isophorone diisocyanate and dibutyl tin dilaurate be 1~
20g；The μ of 1~5g:10~40 L.
4. the preparation method of wetability water-oil separating material according to claim 2, it is characterised in that:
The mass volume ratio of step (1) polyethylene glycol, isophorone diisocyanate and dibutyl tin dilaurate be 2~
16g:3.334g:20 μ L.
5. the preparation method of wetability water-oil separating material according to claim 1, it is characterised in that:
The molal weight of step (1) described polyethylene glycol is 500-8000g/mol；
The mass volume ratio of step (1) polyethylene glycol and solvent A is 0.1~2g/mL；
In the mixed solution of step (1) the solvent B and water, the volume ratio of water and solvent B are 0.2~0.8:20~80；
Volume ratio 1:1~1:4 of step (1) solvent A and solvent B.
6. the preparation method of wetability water-oil separating material according to claim 1, it is characterised in that:
Temperature when step (1) described heating for dissolving is 25~60 DEG C；The temperature reaction be warming up to 60~90 DEG C reaction 3~
12h；The cooling is to be cooled to 25-40 DEG C；The time being stirred to react is 15~36h.
7. the preparation method of wetability water-oil separating material according to claim 1, it is characterised in that:
Step (4) drilling process is that microneedle processes drill process, is punched using microneedle array, the microneedle array
50~500 μm are divided between two needles of middle transverse and longitudinal, used needle diameter is 150-1000 μm.
8. the preparation method of wetability water-oil separating material according to claim 1, it is characterised in that:
The temperature of step (2) described drying is 25~90 DEG C；
The water content of polyurethane hydrogel film obtained by step (3) is 50~90%.
9. the wetability water-oil separating material that any one the method is prepared according to claim 1~8.
10. application of the wetability water-oil separating material in water-oil separating field according to claim 9.
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