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 PDF

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Publication number
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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Prior art keywords
hydrogel
oil suction
dimensional porous
porous oil
deionized water
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CN201910347069.4A
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Chinese (zh)
Inventor
林凌
汪一鸣
何宁
曾金金
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Third Institute of Oceanography MNR
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Third Institute of Oceanography MNR
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D17/00Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
    • B01D17/02Separation of non-miscible liquids
    • B01D17/0202Separation of non-miscible liquids by ab- or adsorption
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/0052Preparation of gels
    • B01J13/0065Preparation of gels containing an organic phase
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/26Synthetic macromolecular compounds
    • B01J20/261Synthetic macromolecular compounds obtained by reactions only involving carbon to carbon unsaturated bonds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014Solid 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
    • B01J20/28047Gels
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/281Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/285Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/40Devices for separating or removing fatty or oily substances or similar floating material
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F120/00Homopolymers 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
    • C08F120/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F120/52Amides or imides
    • C08F120/54Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00Aspects relating to sorbent materials
    • B01J2220/40Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/46Materials comprising a mixture of inorganic and organic materials
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00Aspects relating to sorbent materials
    • B01J2220/40Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48Sorbents characterised by the starting material used for their preparation
    • B01J2220/4806Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00Aspects relating to sorbent materials
    • B01J2220/40Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48Sorbents characterised by the starting material used for their preparation
    • B01J2220/4812Sorbents characterised by the starting material used for their preparation the starting material being of organic character

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Analytical Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Dispersion Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

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

A kind of three-dimensional porous oil suction hydrogel and its preparation method and application
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.
CN201910347069.4A 2019-04-26 2019-04-26 A kind of three-dimensional porous oil suction hydrogel and its preparation method and application Pending CN110180508A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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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Application publication date: 20190830