CN110180508A - A kind of three-dimensional porous oil suction hydrogel and its preparation method and application - Google Patents
A kind of three-dimensional porous oil suction hydrogel and its preparation method and application Download PDFInfo
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- CN110180508A CN110180508A CN201910347069.4A CN201910347069A CN110180508A CN 110180508 A CN110180508 A CN 110180508A CN 201910347069 A CN201910347069 A CN 201910347069A CN 110180508 A CN110180508 A CN 110180508A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0052—Preparation of gels
- B01J13/0065—Preparation of gels containing an organic phase
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/261—Synthetic macromolecular compounds obtained by reactions only involving carbon to carbon unsaturated bonds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28047—Gels
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F120/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
- C08F120/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F120/52—Amides or imides
- C08F120/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/46—Materials comprising a mixture of inorganic and organic materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
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- Engineering & Computer Science (AREA)
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- Water Supply & Treatment (AREA)
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Abstract
The invention discloses a kind of three-dimensional porous oil suction hydrogels and its preparation method and application, it is made of the component for including following ratio: acrylamide monomers: sheet hydrophilic clay: persulfide: deionized water: N, N, N, N- tetramethylethylenediamine=1-3g: 2-6g: 60-100mg: 20-25mL: 100-200 μ L.Hydrogel surface of the invention is coarse and internal porous has far-reaching significance in terms of preparing loose porous oil suction hydrogel material simultaneously as the hydrophobic grouping of acrylamide monomers, the hydrogel after alloing drying adsorb a large amount of oily substance.Prepared by the method hydrogel adsorbs oil slick, and significant effect, separation is thoroughly.
Description
Technical field
The invention belongs to hydrogel preparation technical fields, and in particular to a kind of three-dimensional porous oil suction hydrogel and its preparation side
Method and application.
Background technique
Hydrogel has a wide range of applications because of its powerful water absorption character in fields such as environmental protection, medicine and organizational projects.
Most of hydrogel hydrophilic functional groups rich in, have good suction-operated to water.Some good water of water absorbing properties
Gel can pass through water swelling to the several times of itself original volume.But the water absorption character of general hydrogel is can not to change
, this characteristic has limited to application of the hydrogel in terms of water-oil separating, reported almost without documents and materials and utilizes hydrogel
To adsorb oily substance.
Summary of the invention
It is an object of the invention to overcome prior art defect, a kind of three-dimensional porous oil suction hydrogel is provided.
Another object of the present invention is to provide the preparation methods of above-mentioned three-dimensional porous oil suction hydrogel.
A further object of the present invention is to provide the applications of above-mentioned three-dimensional porous oil suction hydrogel.
Technical scheme is as follows:
A kind of three-dimensional porous oil suction hydrogel is made of the component for including following ratio: acrylamide monomers: sheet parent
Water nanoclay: persulfide: deionized water: N, N, N, N- tetramethylethylenediamine=1-3g:2-6g:60-100mg:20-
25mL:100-200 μ L, wherein sheet hydrophilic clay is as crosslinking agent, and persulfide is as initiator, N, N, N, N- tetramethyl
Base ethylenediamine is as catalyst.
In a preferred embodiment of the invention, the acrylamide monomers include n-isopropyl acrylamide,
Acrylamide, N,N-DMAA and N, N- methylene-bisacrylamide.
In a preferred embodiment of the invention, the sheet hydrophilic clay include natural kaolin, cover it is de-
Soil, illitic soil, bentonite, attapulgite and sepiolite.
In a preferred embodiment of the invention, the persulfide includes ammonium persulfate and potassium peroxydisulfate.
The preparation method of above-mentioned three-dimensional porous oil suction hydrogel, includes the following steps:
(1) in 800- after acrylamide monomers, sheet hydrophilic clay, persulfide and deionized water being mixed
The revolving speed of 1000rpm stirs 10-15min, adds N, N, N, and N- tetramethylethylenediamine is stirred in the revolving speed of 800-1000rpm
1-2mi is after n, in 30-60 DEG C of standing 30-50min;
(2) step (1) resulting material is impregnated into 20-40min with the sodium hydroxide solution that concentration is 1-2mol/L, then
It is washed with deionized, 48-60h is then impregnated in deionized water, wherein every 4-6h changes a deionized water, obtain gel material
Material;
(3) to get the three-dimensional porous oil suction hydrogel after gel rubber material being freeze-dried.
In a preferred embodiment of the invention, the step (3) are as follows: gel rubber material is cold in -80 DEG C of refrigerators
Freeze 10-14h, after 20-24h is freeze-dried in freeze drier.
Application of the above-mentioned three-dimensional porous oil suction hydrogel in oil-water separation mixture.
In a preferred embodiment of the invention, the oil includes chloroform, n-hexane and paraffin.
The beneficial effects of the present invention are:
1, hydrogel surface of the invention is coarse and internal porous, simultaneously as the hydrophobic grouping of acrylamide monomers,
Hydrogel after alloing drying adsorbs a large amount of oily substance, has in terms of preparing loose porous oil suction hydrogel material
Profound significance.Prepared by the method hydrogel adsorbs oil slick, and significant effect, separation is thoroughly.
2, for the present invention using being freeze-dried after water swelling, hole configurations is abundant, and porosity is high, even aperture distribution.
3, large amount of adsorption of the present invention, reusing are good.
4, preparation method of the invention is simple and environmentally-friendly, pollution-free.
Detailed description of the invention
Fig. 1 is the stereoscan photograph of three-dimensional porous oil suction hydrogel prepared by the embodiment of the present invention 1.
Fig. 2 is the graph of pore diameter distribution of three-dimensional porous oil suction hydrogel prepared by the embodiment of the present invention 1.
Fig. 3 is the stereoscan photograph of three-dimensional porous oil suction hydrogel prepared by the embodiment of the present invention 2.
Fig. 4 is the graph of pore diameter distribution of three-dimensional porous oil suction hydrogel prepared by the embodiment of the present invention 2.
Fig. 5 is the stereoscan photograph of three-dimensional porous oil suction hydrogel prepared by the embodiment of the present invention 3.
Fig. 6 is the graph of pore diameter distribution of three-dimensional porous oil suction hydrogel prepared by the embodiment of the present invention 3.
Specific embodiment
Technical solution of the present invention is further explained and described below by way of specific embodiment combination attached drawing.
Embodiment 1:
By n-isopropyl acrylamide, nanoclay, ammonium persulfate and deionized water according to the ratio of 2g:4g:80mg:20mL
Example mixing, 800rpm stirs 15min, rear that 200 μ LN, N, N, N- tetramethylethylenediamines are added, and pours into after 1000rpm stirring 1min
It is covered in the culture dish of sand paper, is placed in 60 DEG C of baking ovens and stands 30min, impregnated in 1mol/L sodium hydroxide solution after taking-up
60h in deionized water is impregnated in 30min, deionized water washing afterwards three times, and it is primary that every 6h changes water, obtains gel rubber material.Taking out should
Gel rubber material freezes 12h in -80 DEG C of refrigerators, after in freeze drier it is dry for 24 hours, obtain the three-dimensional as shown in Figure 1
Porous oil-absorbing hydrogel.It is in contact using the water, air, material three that contact angle measurement tests the three-dimensional porous oil suction hydrogel
Angle, measured value are 141 degree.
30 hole diameters of the random statistical three-dimensional porous oil suction hydrogel, basic Normal Distribution, average diameter
It is 44.22 microns, pore-size distribution is as shown in Figure 2.
Embodiment 2:
By n-isopropyl acrylamide, nanoclay, ammonium persulfate and deionized water according to the ratio of 2g:5g:70mg:20mL
Example mixing, 800rpm stirs 15min, rear that 150 μ LN, N, N, N- tetramethylethylenediamines are added, and pours into after 1000rpm stirring 2min
It is covered in the culture dish of sand paper, is placed in 60 DEG C of baking ovens and stands 30min, impregnated in 1mol/L sodium hydroxide solution after taking-up
48h in deionized water is impregnated in 30min, deionized water washing afterwards three times, and it is primary that every 6h changes water, obtains gel rubber material.Taking out should
Gel rubber material freezes 12h in -80 DEG C of refrigerators, after in freeze drier it is dry for 24 hours, obtain the three-dimensional as shown in Figure 3
Porous oil-absorbing hydrogel.It is in contact using the water, air, material three that contact angle measurement tests the three-dimensional porous oil suction hydrogel
Angle, measured value are 133 degree.
30 hole diameters of the random statistical three-dimensional porous oil suction hydrogel, basic Normal Distribution, average diameter
It is 32.89 microns, pore-size distribution is as shown in Figure 4.
Embodiment 3:
By n-isopropyl acrylamide, nanoclay, ammonium persulfate and deionized water according to the ratio of 1g:4g:60mg:20mL
Example mixing, 800rpm stirs 15min, rear that 150 μ LN, N, N, N- tetramethylethylenediamines are added, and pours into after 1000rpm stirring 2min
It is covered in the culture dish of sand paper, is placed in 50 DEG C of baking ovens and stands 40min, impregnated in 1mol/L sodium hydroxide solution after taking-up
48h in deionized water is impregnated in 30min, deionized water washing afterwards three times, and it is primary that every 8h changes water, obtains gel rubber material.Taking out should
Gel rubber material freezes 12h in -80 DEG C of refrigerators, after in freeze drier it is dry for 24 hours, obtain the three-dimensional as shown in Figure 5
Porous oil-absorbing hydrogel.It is in contact using the water, air, material three that contact angle measurement tests the three-dimensional porous oil suction hydrogel
Angle, measured value are 121 degree.
330 hole diameters of the random statistical three-dimensional porous oil suction hydrogel, basic Normal Distribution, average diameter
It is 32.37 microns, pore-size distribution is as shown in Figure 6.
The foregoing is only a preferred embodiment of the present invention, the range that the present invention that therefore, it cannot be limited according to is implemented, i.e.,
Equivalent changes and modifications made in accordance with the scope of the invention and the contents of the specification should still be within the scope of the present invention.
Claims (8)
1. a kind of three-dimensional porous oil suction hydrogel, it is characterised in that: be made of the component for including following ratio: acrylic amide list
Body: sheet hydrophilic clay: persulfide: deionized water: N, N, N, N- tetramethylethylenediamine=1-3g: 2-6g: 60-
100mg: 20-25mL: 100-200 μ L, wherein sheet hydrophilic clay is as crosslinking agent, and persulfide is as initiator, N,
N, N, N- tetramethylethylenediamine are as catalyst.
2. a kind of three-dimensional porous oil suction hydrogel as described in claim 1, it is characterised in that: the acrylamide monomers packet
Include n-isopropyl acrylamide, acrylamide, N,N-DMAA and N, N- methylene-bisacrylamide.
3. a kind of three-dimensional porous oil suction hydrogel as described in claim 1, it is characterised in that: the sheet hydrophilic clay
Including natural kaolin, montmorillonite, illitic soil, bentonite, attapulgite and sepiolite.
4. a kind of three-dimensional porous oil suction hydrogel as described in claim 1, it is characterised in that: the persulfide includes over cure
Sour ammonium and potassium peroxydisulfate.
5. a kind of preparation method of three-dimensional porous oil suction hydrogel, feature described in any claim in Claims 1-4
It is: includes the following steps:
(1) in 800- after acrylamide monomers, sheet hydrophilic clay, persulfide and deionized water being mixed
The revolving speed of 1000rpm stirs 10-15min, adds N, N, N, and N- tetramethylethylenediamine is stirred in the revolving speed of 800-1000rpm
1-2mi is after n, in 30-60 DEG C of standing 30-50min;
(2) step (1) resulting material is impregnated into 20-40min with the sodium hydroxide solution that concentration is 1-2mol/L, then spent
Ion water washing, then impregnates 48-60h in deionized water, wherein every 4-6h changes a deionized water, obtains gel rubber material;
(3) to get the three-dimensional porous oil suction hydrogel after gel rubber material being freeze-dried.
6. preparation method as claimed in claim 5, it is characterised in that: the step (3) are as follows: by gel rubber material in -80 DEG C of ice
10-14h is freezed in case, after 20-24h is freeze-dried in freeze drier.
7. three-dimensional porous oil suction hydrogel described in any claim is in oil-water separation mixture in Claims 1-4
Using.
8. the use as claimed in claim 7, it is characterised in that: the oil includes chloroform, n-hexane and paraffin.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN114656655A (en) * | 2022-03-29 | 2022-06-24 | 中国科学院宁波材料技术与工程研究所 | Oil-water gel for storing circulating information under visible light and preparation method and application thereof |
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Cited By (2)
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CN114656655A (en) * | 2022-03-29 | 2022-06-24 | 中国科学院宁波材料技术与工程研究所 | Oil-water gel for storing circulating information under visible light and preparation method and application thereof |
CN114656655B (en) * | 2022-03-29 | 2024-01-26 | 中国科学院宁波材料技术与工程研究所 | Oil-water gel for storing circulation information under visible light and preparation method and application thereof |
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