CN113549242B - Sponge-like structure gel for water purification and preparation and application thereof - Google Patents
Sponge-like structure gel for water purification and preparation and application thereof Download PDFInfo
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- CN113549242B CN113549242B CN202110853714.7A CN202110853714A CN113549242B CN 113549242 B CN113549242 B CN 113549242B CN 202110853714 A CN202110853714 A CN 202110853714A CN 113549242 B CN113549242 B CN 113549242B
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 104
- 238000000746 purification Methods 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000002131 composite material Substances 0.000 claims abstract description 65
- 239000002243 precursor Substances 0.000 claims abstract description 31
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 33
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 20
- 238000005286 illumination Methods 0.000 claims description 14
- KJFMBFZCATUALV-UHFFFAOYSA-N phenolphthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C(=O)O1 KJFMBFZCATUALV-UHFFFAOYSA-N 0.000 claims description 13
- 239000012153 distilled water Substances 0.000 claims description 12
- 230000001678 irradiating effect Effects 0.000 claims description 12
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 claims description 11
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 10
- 239000000499 gel Substances 0.000 abstract description 79
- 239000000017 hydrogel Substances 0.000 abstract description 26
- 239000011148 porous material Substances 0.000 abstract description 19
- 239000000463 material Substances 0.000 abstract description 11
- 238000010521 absorption reaction Methods 0.000 abstract description 8
- 239000003960 organic solvent Substances 0.000 abstract description 5
- 239000010865 sewage Substances 0.000 abstract description 3
- 230000010485 coping Effects 0.000 abstract 1
- 229920006395 saturated elastomer Polymers 0.000 abstract 1
- PIZHFBODNLEQBL-UHFFFAOYSA-N 2,2-diethoxy-1-phenylethanone Chemical group CCOC(OCC)C(=O)C1=CC=CC=C1 PIZHFBODNLEQBL-UHFFFAOYSA-N 0.000 description 24
- 239000000178 monomer Substances 0.000 description 22
- 239000003344 environmental pollutant Substances 0.000 description 14
- 231100000719 pollutant Toxicity 0.000 description 14
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 13
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 12
- 238000000034 method Methods 0.000 description 12
- 230000006835 compression Effects 0.000 description 11
- 238000007906 compression Methods 0.000 description 11
- 239000000126 substance Substances 0.000 description 8
- 238000006116 polymerization reaction Methods 0.000 description 7
- 239000002904 solvent Substances 0.000 description 7
- 238000001179 sorption measurement Methods 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 239000003431 cross linking reagent Substances 0.000 description 5
- 239000000975 dye Substances 0.000 description 5
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 239000000654 additive Substances 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 230000008961 swelling Effects 0.000 description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 3
- 239000003463 adsorbent Substances 0.000 description 3
- 150000001555 benzenes Chemical class 0.000 description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 3
- 239000003999 initiator Substances 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 description 3
- 235000011152 sodium sulphate Nutrition 0.000 description 3
- 238000003911 water pollution Methods 0.000 description 3
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-M acrylate group Chemical group C(C=C)(=O)[O-] NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 2
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- 239000002351 wastewater Substances 0.000 description 2
- 239000003403 water pollutant Substances 0.000 description 2
- 229920003169 water-soluble polymer Polymers 0.000 description 2
- ACZGCWSMSTYWDQ-UHFFFAOYSA-N 3h-1-benzofuran-2-one Chemical class C1=CC=C2OC(=O)CC2=C1 ACZGCWSMSTYWDQ-UHFFFAOYSA-N 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229930002877 anthocyanin Natural products 0.000 description 1
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- 150000004636 anthocyanins Chemical class 0.000 description 1
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- 238000001816 cooling Methods 0.000 description 1
- 229920006037 cross link polymer Polymers 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
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- 239000008367 deionised water Substances 0.000 description 1
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- 230000018109 developmental process Effects 0.000 description 1
- 125000004386 diacrylate group Chemical group 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
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- 239000003937 drug carrier Substances 0.000 description 1
- 230000009881 electrostatic interaction Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
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- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- DCYOBGZUOMKFPA-UHFFFAOYSA-N iron(2+);iron(3+);octadecacyanide Chemical compound [Fe+2].[Fe+2].[Fe+2].[Fe+3].[Fe+3].[Fe+3].[Fe+3].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] DCYOBGZUOMKFPA-UHFFFAOYSA-N 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 229910000403 monosodium phosphate Inorganic materials 0.000 description 1
- 235000019799 monosodium phosphate Nutrition 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 239000013225 prussian blue Substances 0.000 description 1
- 229960003351 prussian blue Drugs 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000004043 responsiveness Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 235000017550 sodium carbonate Nutrition 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 description 1
- 239000001488 sodium phosphate Substances 0.000 description 1
- 229910000162 sodium phosphate Inorganic materials 0.000 description 1
- 235000011008 sodium phosphates Nutrition 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
- MLIKYFGFHUYZAL-UHFFFAOYSA-K trisodium;hydron;phosphonato phosphate Chemical compound [Na+].[Na+].[Na+].OP([O-])(=O)OP([O-])([O-])=O MLIKYFGFHUYZAL-UHFFFAOYSA-K 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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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
- C08J9/26—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a solid phase from a macromolecular composition or article, e.g. leaching out
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
- A61K47/32—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds, e.g. carbomers, poly(meth)acrylates, or polyvinyl pyrrolidone
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/06—Ointments; Bases therefor; Other semi-solid forms, e.g. creams, sticks, gels
-
- 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
-
- 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
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
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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
- C08F290/00—Macromolecular compounds obtained by polymerising monomers on to polymers modified by introduction of aliphatic unsaturated end or side groups
- C08F290/02—Macromolecular compounds obtained by polymerising monomers on to polymers modified by introduction of aliphatic unsaturated end or side groups on to polymers modified by introduction of unsaturated end groups
- C08F290/06—Polymers provided for in subclass C08G
- C08F290/062—Polyethers
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- 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
- C08J2201/042—Elimination of an organic solid phase
- C08J2201/0422—Elimination of an organic solid phase containing oxygen atoms, e.g. saccharose
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- 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
- C08J2201/044—Elimination of an inorganic solid phase
- C08J2201/0444—Salts
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- C08J2351/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
- C08J2351/08—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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Abstract
The invention relates to a preparation method and application of sponge-like structure water/oil composite gel for water purification, which comprises the following steps: (1) Adding the gelling component, the organic solvent and the soluble pore-forming agent into water, and stirring until the gelling component, the organic solvent and the soluble pore-forming agent are completely dissolved to form a transparent and uniform solution, so as to obtain a gel precursor solution; (2) Curing the gel precursor solution obtained in the step (1) into gel to prepare hydrogel with a special pore structure; (3) And (3) extruding the hydrogel prepared in the step (2), putting the hydrogel into sewage to be adsorbed until the hydrogel is saturated, and extruding water to purify the sewage. The preparation method has the advantages of simple and efficient preparation process, cheap and easily-obtained materials, higher mechanical strength and water absorption, flexible adjustment of shape and size without affecting the performance according to different environments and system use requirements, capability of maintaining the temperature stability of the system in a short time even in extreme environments, and great significance in coping with disasters such as fire and the like.
Description
Technical Field
The invention relates to a water/oil composite gel material, in particular to a sponge-like structure gel for water purification and preparation and application thereof.
Background
The quality of water bodies is always the most concerned environmental problem, but in recent years, with the development of economic society and the expansion of industrialization, more and more water bodies are polluted to different degrees and in different modes. Water pollution has become one of the major problems that must be dealt with worldwide. The water pollutants mainly comprise oil, organic matters, heavy metal ions, dye molecules and the like, which seriously destroy the balance of an ecological system and a water environment, so that the effective treatment of the water pollutants is very important. The existing water pollution treatment methods mainly include adsorption method, flocculation precipitation method, biodegradation method, etc., which adsorb related impurities by using adsorbents such as activated carbon, prussian blue, activated alumina, etc. However, the adsorbent has low adsorption capacity, poor regeneration capacity, low flux, easy secondary pollution after saturation, difficult adaptation to continuous purification treatment and other requirements, and thus, the large-scale application of the adsorbent is limited.
Hydrogel as a material with a 3D pore network structure has the advantages of low apparent density, large specific surface area, low cost and chemical stability, and has been used in water pollution treatment to remove oil stains, organic matters and macromolecular dyes. Meanwhile, the hydrogel has abundant chemical composition and a large amount of internal spatial structures, so that the hydrogel can be modified and further modified, and is endowed with more functions. The hydrogels commonly used for water purification are mainly classified into: hydrogel beads, hydrogel films, and hydrogel nanocomposites. They are based on different chemical properties and utilize one or more of electrostatic interaction, chelation, ion exchange, hydrophobic interaction, trapping separation to realize the removal of pollutants.
In addition, the hydrogel has the condition of serving as a water purification material due to the strong water absorption capacity, the flexibility, the ductility and the porosity of the hydrogel are also caused due to the strong water absorption capacity, the hydrogel can be shaped to be prepared into shapes and sizes required by various devices, and the hydrogel can respond to the surrounding environment such as pH, temperature and the like, so that the hydrogel can be well adapted to various extreme environments, and the application range of the water purification material is greatly expanded.
However, hydrogel materials also have some problems in water purification, the most important of which is the contradiction between mechanical properties and water absorption capacity. The hydrogel with better water absorption performance has low mechanical strength, particularly after water absorption and swelling saturation, the compression modulus is only several kilopascals to dozens of kilopascals, the requirement of high-flux water purification cannot be met far away, and most hydrogel water purification materials are disposable products and cannot be used for a second time after water absorption and extrusion purification. This not only causes waste of resources and improvement of cost, but also reduces the efficiency of water purification work.
Disclosure of Invention
The invention aims to overcome the existing defects and provide a sponge-like structure gel for water purification and preparation and application thereof.
The purpose of the invention can be realized by the following technical scheme:
a preparation method of gel with a sponge-like structure for water body purification comprises the following steps:
(1) Adding the gelling component, the organic solvent and the soluble pore-forming agent into water, and stirring until the gelling component, the organic solvent and the soluble pore-forming agent are completely dissolved to form a transparent and uniform solution, so as to obtain a gel precursor solution;
(2) Polymerizing the gel precursor solution obtained in the step (1) to form gel, and preparing sponge-like hydrogel with a special pore structure;
(3) And (3) squeezing the water in the hydrogel prepared in the step (2) to obtain the sponge-like hydrogel capable of absorbing sewage.
Preferably, in step (1): the gel-forming component is a monomer polymerization system.
Preferably, the monomer polymerization system contains a monomer, a cross-linking agent, an organic/water composite solvent, a pore-forming agent and an ultraviolet initiator, wherein the monomer is an acrylate monomer or an acrylic monomer, the cross-linking agent is polyethylene glycol (glycol) diacrylate (PEGDA), the organic solvent is glycerol or glycol water-soluble organic matter, the pore-forming agent is a mixture of macromolecular compounds such as benzofuranones and inorganic salts, and the ultraviolet initiator is 2,2-Diethoxyacetophenone (DEAP).
Preferably, the monomer is one or more of acrylate, methacrylate, 2-hydroxyethyl acrylate (HEA) and 2-hydroxyethyl methacrylate (HEMA).
Preferably, the addition amount of the monomer is 20-50% of the total weight of the organic/water composite solvent, the addition amount of the cross-linking agent is 0.1-1% of the total weight of the monomer, and the addition amount of the ultraviolet initiator is 0.1-1% of the total weight of the monomer.
Preferably, when the gel-forming component is a monomer polymerization system, the gel-forming manner in step (2) is as follows: placing the gel precursor solution in a place with the light intensity of 25-30 mW/cm 2 The reaction time is 20-45 min;
preferably, in step (1): the composite solvent is one or more of deionized water, glycerol, glycol, ethanol and dimethyl sulfoxide.
Preferably, in step (1): the soluble pore-forming agent is a compound of one or more of 3,3-bis (4-hydroxyphenyl) -3H-isobenzofuranone, anthocyanin and one or more of sodium carbonate, sodium bicarbonate, sodium sulfate, sodium phosphate, sodium dihydrogen phosphate and sodium hydrogen diphosphate.
Preferably, the addition amount of the soluble pore-forming agent is 0.1-0.5% of the total weight of water.
Preferably, in step (1): stirring at 20-40 deg.C for 5-10min.
The application of composite hydrogel with a sponge-like structure in a water purification system.
The process conditions in the present invention are the most suitable preparation conditions. Stirring is for rapid dissolution of monomers, solvents and additives; the pore-forming agent is added to control and adjust the hollow island structure of the hydrogel, the higher the content of the additive is, the larger the pore channel of the hydrogel is, but the lower the water purification efficiency is; the illumination intensity corresponds to the reaction time, and the required reaction time is prolonged if the illumination intensity is too low; the illumination length corresponds to the reaction degree, and too short a time period can reduce the polymerization degree of the reaction, thereby affecting the mechanical property; the addition amount of reactants can affect the performance of the finally obtained water purification gel, especially the adsorption performance of the water purification gel, for example, if the content of the monomer or the crosslinking agent is too low, the mechanical strength of the water purification gel is reduced, even the gelling is not formed, and if the content of the monomer or the crosslinking agent is too high, the gel network is too compact, so that the water purification effect cannot be realized.
The invention adjusts the hydrogel network structure of a monomer with amphipathy by using additives such as pore-forming agent and the like, and obtains the water/oil composite gel which has a sponge-like structure at normal temperature and normal pressure and can be used for water purification. Wherein, the composite gel contains a cross-linked polymer gel matrix material and a composite solvent formed by organic/water according to a certain proportion; the polymer gel matrix can form a three-dimensional space network structure through monomer polymerization or polymer physical crosslinking, and the pore-forming agent is filled in gaps of the network structure to realize the adjustment of the network structure.
The invention relates to a novel method for preparing water purification composite gel, which comprises the steps of firstly adding a proper amount of pore-forming agent and composite solvent into precursor liquid, cooling the precursor liquid after gelling to form special polymer chain conformation and network structure, and obtaining the composite gel with excellent mechanical property and reusable sponge-like structure.
The method has the advantages of simple process, strong controllability and easy operation. The sponge-like structure composite gel prepared by the method has ultrahigh mechanical strength, can be recycled for more than 1000 times, and is thousands of times of pure water gel. In addition, the composite gel monomer molecule has amphipathy, and the composite solvent and a proper amount of pore-forming agent can enable the structure of the composite gel monomer molecule to have good adjustability, so that the composite gel monomer molecule can be used as an effective and reliable adsorbing material to be applied to water resource purification without introducing other additives or operation means. In the process of monomer polymerization, the conformation of the polymer chain segment is converted into a proper form along with system design, and the affinity degree to water is reduced, so that the adsorption capacity of the gel material is improved, and the water treatment efficiency is higher.
In addition, because the selected monomer structure has good biocompatibility, temperature responsiveness and ionic effect, the sponge composite gel can be used for separating biomacromolecules by designing the structure of a gel pore channel, such as: bacteria, proteins, etc. In addition, the composite gel has excellent structural performance and amphipathy, so that the composite gel can be used as a drug carrier to carry out controllable release of in-vivo drugs.
Compared with the prior art, the invention has the following beneficial effects:
(1) Compared with the traditional water purification gel, the sponge-like structure water/oil composite gel prepared by the invention has higher mechanical strength, adsorption capacity and reliability due to the special performance of the structure, and is more efficient and safer in the application of water treatment and purification;
(2) Compared with activated carbon adsorption water purification materials, the sponge-like structure water/oil composite gel prepared by the invention has more adjustable pore channel structures, can realize the directional adsorption and treatment of pollutants with target molecular weight, and can enable the material to obtain better water treatment performance and more functions;
(3) The composite gel has the structural characteristics of water absorption/extrusion, so that the composite gel can be stably and repeatedly used for a long time. The swelling stability of the water-soluble polymer enables the water-soluble polymer to have higher water environment tolerance when being used for water treatment equipment, and the safety and the stability are ensured;
(4) In the monomer polymerization process, the conformation of a molecular chain is changed, so that molecules are subjected to phase separation at a certain temperature, the temperature response is realized, the structure ratio is adjusted, the method can be used for roughly estimating the temperature of wastewater and carrying out pretreatment, the temperature window of water treatment equipment is widened, and the water treatment equipment can still normally work at a low temperature;
(5) The sponge-like structure water/oil composite gel can purify pollutants in wastewater, particularly macromolecular dyes and benzene series, and does not cause environmental pollution;
(6) The preparation process is simple, and the raw materials are cheap and easy to obtain.
Drawings
FIG. 1 is a pictorial view of a sponge-like structured water/oil composite gel of example 1;
FIG. 2 is a scanning electron microscope image of the sponge-like structure water/oil composite gel of example 1;
FIG. 3 is a rheological profile during gelling of the sponge-like structured water/oil composite gel of example 1;
FIG. 4 is a graph showing the compression curves of the sponge-like structure water/oil composite gel of example 1;
FIG. 5 is a graph showing the cyclic compression use of the sponge-like structure water/oil composite gel of example 1;
FIG. 6 shows the purification of the sponge-like water/oil composite gel of example 1 for macromolecular dyes (rhodamine as an example);
FIG. 7 shows the recycling of the sponge-like water/oil composite gel of example 1 for macromolecular dyes (rhodamine as an example);
FIG. 8 shows the purification of benzene series (phenol as an example) by the sponge-like water/oil composite gel of example 1;
FIG. 9 is the swelling stability in water of the sponge-like structure water/oil composite gel of example 1.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
Example 1
0.3g of 2-hydroxyethyl methacrylate (HEMA), 0.35mg of glycerol (Gly), 1. Mu.L of 2,2-Diethoxyacetophenone (DEAP), 5mg of a sodium carbonate solution (2% by weight, containing 0.02% of 3, 3-bis (4-hydroxyphenyl) -3H-isobenzofuranone) was added to 0.35mL of distilled water, and stirred at room temperature for 5min to form a transparent and uniform precursor-containing solution. Irradiating the precursor solution with ultraviolet light at 25 deg.C with illumination intensity of about 25mW/cm 2 And reacting for 25min to obtain the sponge-like structure water/oil composite gel with a proper pore diameter. The compressive modulus of the resulting composite gel was 3.35MPa.
As shown in fig. 1, the sponge-like water/oil composite gel of this example has good usability and recovery after use. FIG. 2 is a scanning electron microscope image showing that the gel has a clear and uniform pore structure with a pore size of 20-30 μm. FIG. 3 is the rheological curve of the water/oil composite gel with sponge-like structure in the gelling process, which shows that the system effectively forms the gel structure. Fig. 4 and 5 are mechanical property images of the sponge-like water/oil composite gel, and the results show that the composite gel of the embodiment has excellent mechanical properties and can be recycled more than 1000 times.
In the sponge-like structure water/oil composite gel of the embodiment, after macromolecular pollutants (rhodamine for example) are evolved for 4 times, the purification rate can reach more than 98% (fig. 6); for the same concentration of macromolecular pollutants (rhodamine is taken as an example), the sponge-like structure water/oil composite gel of the embodiment can be used for more than 10 times (FIG. 7). The purification ability of the benzene series (phenol) is excellent (figure 8).
Fig. 9 shows that the sponge-like water/oil composite gel of this example has high stability in water, undergoes little swelling, and can maintain a good morphology for a long period of time.
Example 2
0.3g of 2-hydroxyethyl methacrylate (HEMA), 0.4mg of glycerol (Gly), 1. Mu.L of 2,2-Diethoxyacetophenone (DEAP), 5mg of a sodium carbonate solution (2% by weight, containing 0.02% of 3, 3-bis (4-hydroxyphenyl) -3H-isobenzofuranone) was added to 0.6mL of distilled water, and stirred at room temperature for 5 minutes to form a precursor solution containing a transparent and uniform substance. Irradiating the precursor solution with ultraviolet light at 25 deg.C with illumination intensity of about 25mW/cm 2 And reacting for 25min to obtain the water/oil composite gel with the sponge-like structure and the proper pore diameter. The compressive modulus of the resulting composite gel was 4.72MPa.
Example 3
0.2g of 2-hydroxyethyl methacrylate (HEMA), 0.4mg of glycerol (Gly), 1. Mu.L of 2,2-Diethoxyacetophenone (DEAP), 5mg of a sodium carbonate solution (2% by weight, containing 0.02% of 3, 3-bis (4-hydroxyphenyl) -3H-isobenzofuranone) was added to 0.6mL of distilled water, and stirred at room temperature for 5 minutes to form a precursor solution containing a transparent and uniform substance. Irradiating the precursor solution with ultraviolet light at 25 deg.C with illumination intensity of about 25mW/cm 2 And reacting for 25min to obtain the sponge-like structure water/oil composite gel with a proper pore diameter. The compression modulus of the obtained composite gel is 0.27MPa, and the purification rate of the composite gel for 1 time of macromolecular pollutants (such as rhodamine) is 74 percent.
Example 4
0.4g of 2-hydroxyethyl methacrylate (HEMA), 0.4mg of glycerol (Gly), 1. Mu.L of 2,2-Diethoxyacetophenone (DEAP), 5mg of a sodium carbonate solution (2% by weight, containing 0.02% of 3, 3-bis (4-hydroxyphenyl) -3H-isobenzofuranone) was added to 0.6mL of distilled water,stirring at room temperature for 5min to form a transparent and uniform precursor solution. Irradiating the precursor solution with ultraviolet light at 25 deg.C with illumination intensity of about 25mW/cm 2 And reacting for 25min to obtain the sponge-like structure water/oil composite gel with a proper pore diameter. The compression modulus of the obtained composite gel is 5.61MPa, and the purification rate of 1 time for macromolecular pollutants (such as rhodamine) is 10%.
Example 5
0.3g of 2-hydroxyethyl methacrylate (HEMA), 0.4mg of glycerol (Gly), 1. Mu.L of 2,2-Diethoxyacetophenone (DEAP), 5mg of a sodium sulfate solution (2% by weight, containing 0.02% of 3, 3-bis (4-hydroxyphenyl) -3H-isobenzofuranone) was added to 0.6mL of distilled water, and stirred at room temperature for 5 minutes to form a precursor solution containing a transparent and uniform substance. Irradiating the precursor solution with ultraviolet light at 25 deg.C with illumination intensity of about 25mW/cm 2 And reacting for 25min to obtain the sponge-like structure water/oil composite gel with a proper pore diameter. The compressive modulus of the obtained composite gel is 2.21MPa, and the purification rate of 1 time for macromolecular pollutants (rhodamine is taken as an example) is 60.3 percent.
Example 6
0.3g of 2-hydroxyethyl methacrylate (HEMA), 0.4mg of glycerol (Gly), 1. Mu.L of 2,2-Diethoxyacetophenone (DEAP), 5mg of a sodium chloride solution (2% by weight, containing 0.02% of 3, 3-bis (4-hydroxyphenyl) -3H-isobenzofuranone) was added to 0.6mL of distilled water, and stirred at room temperature for 5 minutes to form a precursor solution containing a transparent and uniform substance. Irradiating the precursor solution with ultraviolet light at 25 deg.C with illumination intensity of about 25mW/cm 2 And reacting for 25min to obtain the sponge-like structure water/oil composite gel with a proper pore diameter. The compression modulus of the obtained composite gel is 2.77MPa, and the purification rate of 1 time of macromolecular pollutants (such as rhodamine) is 63.5 percent.
Example 7
0.3g of 2-hydroxyethyl acrylate (HEA), 0.4mg of glycerol (Gly), 1. Mu.L of 2,2-Diethoxyacetophenone (DEAP), 5mg of a sodium carbonate solution (2% by weight, containing 0.02% to 3, 3-bis (4-hydroxyphenyl) -3H-isobenzofuranone) was added to 0.6mL of distilled water, and stirred at room temperature for 5 minutes to form a transparent and uniform precursor solution. Irradiating the precursor solution with ultraviolet light at 25 deg.CIllumination intensity of about 25mW/cm 2 And reacting for 25min to obtain the water/oil composite gel with the sponge-like structure and the proper pore diameter. The compression modulus of the obtained composite gel is 3.31MPa, and the purification rate of 1 time of macromolecular pollutants (such as rhodamine) is 12.6 percent.
Example 8
0.3g of methacrylate, 0.4mg of glycerol (Gly), 1. Mu.L of 2,2-Diethoxyacetophenone (DEAP), 5mg of a sodium carbonate solution (2% by weight, containing 0.02% by weight of 3, 3-bis (4-hydroxyphenyl) -3H-isobenzofuranone) was added to 0.6mL of distilled water, and stirred at room temperature for 5 minutes to form a precursor solution containing a transparent and uniform substance. Irradiating the precursor solution with ultraviolet light at 25 deg.C with illumination intensity of about 25mW/cm 2 And reacting for 25min to obtain the sponge-like structure water/oil composite gel with a proper pore diameter. The compression modulus of the obtained composite gel is 1.13MPa, and the purification rate of 1 time for macromolecular pollutants (such as rhodamine) is 11.4 percent.
Example 9
0.3g of 2-hydroxyethyl methacrylate (HEMA), 0.4mg of ethylene glycol, 1. Mu.L of 2,2-Diethoxyacetophenone (DEAP), 5mg of a sodium carbonate solution (2% by weight, containing 0.02% of 3, 3-bis (4-hydroxyphenyl) -3H-isobenzofuranone) was added to 0.6mL of distilled water, and stirred at room temperature for 5 minutes to form a transparent and uniform precursor solution. Irradiating the precursor solution with ultraviolet light at 25 deg.C with illumination intensity of about 25mW/cm 2 And reacting for 25min to obtain the sponge-like structure water/oil composite gel with a proper pore diameter. The compression modulus of the obtained composite gel is 1.78MPa, and the purification rate of 1 time for macromolecular pollutants (such as rhodamine) is 12.1%.
Example 10
0.3g of 2-hydroxyethyl methacrylate (HEMA), 0.4mg of ethanol, 1. Mu.L of 2,2-Diethoxyacetophenone (DEAP), 5mg of sodium carbonate solution (2% by weight, containing 0.02% by weight of 3, 3-bis (4-hydroxyphenyl) -3H-isobenzofuranone) was added to 0.6mL of distilled water, and stirred at room temperature for 5min to form a transparent and uniform precursor solution. Irradiating the precursor solution with ultraviolet light at 25 deg.C with illumination intensity of about 25mW/cm 2 And reacting for 25min to obtain the sponge-like structure water/oil composite gel with a proper pore diameter. Of the resulting composite gelThe compression modulus is 0.63MPa, and the purification rate for 1 time of macromolecular pollutants (rhodamine is taken as an example) is 1.3 percent.
Example 11
0.3g of 2-hydroxyethyl methacrylate (HEMA), 0.4mg of ethylene glycol, 1. Mu.L of 2,2-Diethoxyacetophenone (DEAP), 5mg of a sodium sulfate solution (2% by weight, containing 0.02% of 3, 3-bis (4-hydroxyphenyl) -3H-isobenzofuranone) was added to 0.6mL of distilled water, and stirred at room temperature for 5 minutes to form a transparent and uniform precursor solution. Irradiating the precursor solution with ultraviolet light at 25 deg.C with illumination intensity of about 25mW/cm 2 And reacting for 25min to obtain the sponge-like structure water/oil composite gel with a proper pore diameter. The compression modulus of the obtained composite gel is 0.99MPa, and the purification rate of 1 time of macromolecular pollutants (such as rhodamine) is 10.4 percent.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make modifications and alterations without departing from the scope of the present invention.
Claims (3)
1. A preparation method of a gel with a sponge-like structure for water body purification is characterized by comprising the following steps:
adding 0.3g methacrylic acid-2-hydroxyethyl ester, 0.35mg glycerol, 1 mu L2,2-diethoxyacetophenone and 5mg soluble pore-forming agent solution into 0.35mL of distilled water, and stirring at room temperature for 5min to form a transparent and uniform precursor solution;
irradiating the precursor solution with ultraviolet light at 25 deg.C with illumination intensity of 25mW/cm 2 Reacting for 25min to obtain the water/oil composite gel with the sponge-like structure;
wherein the soluble pore-forming agent solution is 2wt% of sodium carbonate solution and contains 0.02% of 3,3-bis (4-hydroxyphenyl) -3H-isobenzofuranone.
2. A sponge-like structure gel for water purification, which is prepared by the preparation method of claim 1.
3. Use of a sponge-like structured gel for the purification of a body of water according to claim 2 in a water purification system.
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