CN107774237A - The Preparation method and use of CNT hydrogel - Google Patents

The Preparation method and use of CNT hydrogel Download PDF

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Publication number
CN107774237A
CN107774237A CN201711067872.XA CN201711067872A CN107774237A CN 107774237 A CN107774237 A CN 107774237A CN 201711067872 A CN201711067872 A CN 201711067872A CN 107774237 A CN107774237 A CN 107774237A
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cnt
hydrogel
water
carbon nanotube
walled carbon
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刘淼
陈宇
于萌
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Jilin University
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Jilin University
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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
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • B01J20/205—Carbon nanostructures, e.g. nanotubes, nanohorns, nanocones, nanoballs
    • 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
    • B01J20/264—Synthetic macromolecular compounds derived from different types of monomers, e.g. linear or branched copolymers, block copolymers, graft copolymers
    • 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
    • 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
    • C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
    • 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

Abstract

The invention discloses a kind of Preparation method and use of CNT hydrogel, preparation method is：Step 1: CNT is modified into processing, hydrophilic multi-walled carbon nanotube is made；Step 2: hydrophily multi-walled carbon nanotube made from step 1 is placed in beaker, add ultra-pure water, ultrasonic disperse, acrylamide and acrylic acid are added, is sealed after adding crosslinking agent and initiator, in 60 DEG C of 6h of water bath with thermostatic control polymerisation 2, obtained product will be reacted with water washing, immersion, timing changes water to go unless gel section, 60 DEG C of 80 DEG C of freeze-day with constant temperature to constant weight, you can obtain CNT hydrogel.Obtained CNT hydrogel is removing the application of Wastewater Dyes.Beneficial effects of the present invention：Be advantageous to hydrogel to adsorb dye ions.The preparation method of the CNT hydrogel of the present invention has simple to operate, prepares the advantages of convenient, solves CNT and the drawback such as is difficult to collect in water process because size is small.

Description

The Preparation method and use of CNT hydrogel
Technical field
The present invention relates to a kind of Preparation method and use of hydrogel, more particularly to a kind of preparation of CNT hydrogel Method and purposes.
Background technology
At present, substantial amounts of waste water from dyestuff is produced while dyestuff extensive use to be discharged into environment water, it is saturating to reduce water body Lightness, aquatile and microorganism growth are influenceed, is unfavorable for the self-purification of water, pollution is caused to natural water.Therefore, how to close The dyestuff removed in waste water of reason has turned into heat subject of the environmental administration compared with care.Wherein, absorption method is as a kind of important Physico-chemical process, can from waste water concentration and separation organic pollution, realize changing waste into resources, have in waste water from dyestuff is handled It is widely applied.
Hydrogel is a kind of polymer with three-dimensional net structure, and it can absorb the substantial amounts of hydrosol in water, and It can continue to keep its original structure and be not dissolved after swelling, be a kind of novel environmental friendly sorbing material.
For CNT as a kind of new material, specific surface area is big, has loose structure.Pass through the acid to CNT Change, be modified, its structure is changed, there is more excellent absorption property, being the effective way for expanding its application.
The content of the invention
The invention aims to the concentration and separation organic pollution from waste water, is provided so as to realize changing waste into resources A kind of CNT hydrogel Preparation method and use.
The preparation method of CNT hydrogel provided by the invention, its method are as described below：
Step 1: CNT is modified into processing, hydrophilic multi-walled carbon nanotube is made, takes CNT 4mol/L HCL be heated to reflux 6h, after filtration washing, with the H that concentration is 98%2SO4And HNO3Mixed liquor in be heated to reflux 30min, mix Close H in liquid2SO4And HNO3Volume ratio be 3:1, dried after washing repeatedly；
Step 2: hydrophily multi-walled carbon nanotube made from step 1 is placed in beaker, ultra-pure water, ultrasound point are added Dissipate, with 1：1 or 1：2 or 2:1 mol ratio of one of them adds acrylamide and acrylic acid, adds acrylamide and acrylic acid Gross weight 0.4%-1.6% crosslinking agent N, N'- methylene-bisacrylamide, magnetic agitation 1h add propylene to being completely dissolved Sealed after acid amides and acrylic acid gross weight 1%-4% initiator ammonium persulfate, will in 60 DEG C of water bath with thermostatic control polymerisation 2-6h Obtained product is reacted with water washing, immersion, regularly changes water to go unless gel section, 60 DEG C of -80 DEG C of freeze-day with constant temperature to constant weight, It can obtain CNT hydrogel.
A diameter of 20-30nm of CNT in step 1, length are 0.5-2 μm.
The input amount of hydrophilic multi-walled carbon nanotube is the 0.03% of acrylamide and acrylic acid gross weight in step 2.
CNT hydrogel obtained above is removing the application of Wastewater Dyes.
Beneficial effects of the present invention：
Amplify after 50,000 times it can be seen that prepared CNT hydrogel surface is uneven, there is clearly aperture. Hydrogel surface has been covered with cylindrical protrusion of the diameter range between 30-50nm, and these numerous projections increase with loose structure The big specific surface area of hydrogel, is advantageous to hydrogel and dye ions is adsorbed.The CNT hydrogel of the present invention Preparation method has simple to operate, prepares the advantages of convenient, solves CNT and be difficult to because size is small in water process The drawbacks such as collection.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph that CNT hydrogel produced by the present invention amplifies 50000 times.
Fig. 2 is that CNT hydrogel adsorbent dosage influences to scheme on dye base safranine adsorption effect.
Fig. 3 is that CNT hydrogel adsorbent dosage influences to scheme on Crystal Violet adsorption effect.
Fig. 4 is that CNT hydrogel adsorbent dosage influences to scheme on dyestuff malachite green adsorption effect.
Fig. 5 is influence schematic diagram of the CNT hydrogel to Dye Adsorption effect under different temperatures.
Fig. 6 is influence schematic diagram of the pH value to CNT hydrogel adsorption effect of different dyes solution.
Fig. 7 is curve of adsorption kinetics schematic diagram of the CNT hydrogel to dyestuff.
Fig. 8 is adsorption isotherm schematic diagram of the CNT hydrogel to dyestuff.
Embodiment
Refer to shown in Fig. 1 to Fig. 8：
The following examples are that the present invention is described in further detail.
Embodiment 1：
Step 1: CNT is modified into processing, hydrophilic multi-walled carbon nanotube is made.CNT is taken to be put into 4mol/L HCL is heated to reflux 6h, is 98%H with concentration after filtration washing2SO4And HNO3Mixed liquor (volume ratio V:V=3: 1) 30min is heated to reflux in, is dried after washing repeatedly.
Step 2: taking hydrophily multi-walled carbon nanotube 50mg to be placed in 100mL small beakers, the ultrapure ultrasounds point of 20mL are added Dissipate.Sequentially add acrylamide 1.7777g, acrylic acid 1.8015g, crosslinking agent N, N'- methylene-bisacrylamide 0.0062g. Magnetic agitation about 1h seals to being completely dissolved after adding initiator ammonium persulfate 0.0228g, anti-in 60 DEG C of water bath with thermostatic control polymerizations Answer 6h.Obtained product will be reacted to distill water washing, soaked 3 days afterwards, regularly change water daily to go unless gel section, 70 DEG C freeze-day with constant temperature sieves standby to constant weight after xerogel is crushed.
Embodiment 2：
Step 1: CNT is modified into processing, hydrophilic multi-walled carbon nanotube is made.CNT is taken to be put into 4mol/L HCL is heated to reflux 6h, is 98%H with concentration after filtration washing2SO4And HNO3Mixed liquor (volume ratio V:V=3: 1) 30min is heated to reflux in, is dried after washing repeatedly.
Step 2: taking hydrophily multi-walled carbon nanotube 100mg to be placed in 100mL small beakers, the ultrapure ultrasounds point of 20mL are added Dissipate.Sequentially add acrylamide 1.7777g, acrylic acid 1.8015g, crosslinking agent N, N'- methylene-bisacrylamide 0.0124g. Magnetic agitation about 1h seals to being completely dissolved after adding initiator ammonium persulfate 0.0456g, anti-in 60 DEG C of water bath with thermostatic control polymerizations Answer 6h.Obtained product will be reacted to distill water washing, soaked 3 days afterwards, regularly change water daily to go unless gel section, 70 DEG C freeze-day with constant temperature sieves standby to constant weight after xerogel is crushed.
Embodiment 3：
Step 1: CNT is modified into processing, hydrophilic multi-walled carbon nanotube is made.CNT is taken to be put into 4mol/L HCL is heated to reflux 6h, is 98%H with concentration after filtration washing2SO4And HNO3Mixed liquor (volume ratio V:V=3: 1) 30min is heated to reflux in, is dried after washing repeatedly.
Step 2: taking hydrophily multi-walled carbon nanotube 25mg to be placed in 100mL small beakers, the ultrapure ultrasounds point of 20mL are added Dissipate.Sequentially add acrylamide 1.7777g, acrylic acid 1.8015g, crosslinking agent N, N'- methylene-bisacrylamide 0.0031g. Magnetic agitation about 1h seals to being completely dissolved after adding initiator ammonium persulfate 0.0114g, anti-in 60 DEG C of water bath with thermostatic control polymerizations Answer 6h.Obtained product will be reacted to distill water washing, soaked 3 days afterwards, regularly change water daily to go unless gel section, 70 DEG C freeze-day with constant temperature sieves standby to constant weight after xerogel is crushed.
Embodiment 4：
Step 1: CNT is modified into processing, hydrophilic multi-walled carbon nanotube is made.CNT is taken to be put into 4mol/L HCL is heated to reflux 6h, is 98%H with concentration after filtration washing2SO4And HNO3Mixed liquor (volume ratio V:V=3: 1) 30min is heated to reflux in, is dried after washing repeatedly.
Step 2: taking hydrophily multi-walled carbon nanotube 50mg to be placed in 100mL small beakers, the ultrapure ultrasounds point of 20mL are added Dissipate.Sequentially add acrylamide 2.3693g, acrylic acid 1.201g, crosslinking agent N, N'- methylene-bisacrylamide 0.0031g.Magnetic Power stirs about 1h to being completely dissolved, and is sealed after adding initiator ammonium persulfate 0.0228g, in 60 DEG C of water bath with thermostatic control polymerisations 6h.Obtained product will be reacted to distill water washing, soaked 3 days afterwards, regularly change water daily to go unless gel section, 70 DEG C Freeze-day with constant temperature sieves standby to constant weight after xerogel is crushed.
Embodiment 5：
Step 1: CNT is modified into processing, hydrophilic multi-walled carbon nanotube is made.CNT is taken to be put into 4mol/L HCL is heated to reflux 6h, is 98%H with concentration after filtration washing2SO4And HNO3Mixed liquor (volume ratio V:V=3: 1) 30min is heated to reflux in, is dried after washing repeatedly.
Step 2: taking hydrophily multi-walled carbon nanotube 100mg to be placed in 100mL small beakers, the ultrapure ultrasounds point of 20mL are added Dissipate.Sequentially add acrylamide 2.3693g, acrylic acid 1.201g, crosslinking agent N, N'- methylene-bisacrylamide 0.0062g.Magnetic Power stirs about 1h to being completely dissolved, and is sealed after adding initiator ammonium persulfate 0.0114g, in 60 DEG C of water bath with thermostatic control polymerisations 6h.Obtained product will be reacted to distill water washing, soaked 3 days afterwards, regularly change water daily to go unless gel section, 70 DEG C Freeze-day with constant temperature sieves standby to constant weight after xerogel is crushed.
Embodiment 6：
Step 1: CNT is modified into processing, hydrophilic multi-walled carbon nanotube is made.CNT is taken to be put into 4mol/L HCL is heated to reflux 6h, is 98%H with concentration after filtration washing2SO4And HNO3Mixed liquor (volume ratio V:V=3: 1) 30min is heated to reflux in, is dried after washing repeatedly.
Step 2: taking hydrophily multi-walled carbon nanotube 25mg to be placed in 100mL small beakers, the ultrapure ultrasounds point of 20mL are added Dissipate.Sequentially add acrylamide 2.3693g, acrylic acid 1.201g, crosslinking agent N, N'- methylene-bisacrylamide 0.0124g.Magnetic Power stirs about 1h to being completely dissolved, and is sealed after adding initiator ammonium persulfate 0.0228g, in 60 DEG C of water bath with thermostatic control polymerisations 6h.Obtained product will be reacted to distill water washing, soaked 3 days afterwards, regularly change water daily to go unless gel section, 70 DEG C Freeze-day with constant temperature sieves standby to constant weight after xerogel is crushed.
Embodiment 7：
Step 1: CNT is modified into processing, hydrophilic multi-walled carbon nanotube is made.CNT is taken to be put into 4mol/L HCL is heated to reflux 6h, is 98%H with concentration after filtration washing2SO4And HNO3Mixed liquor (volume ratio V:V=3: 1) 30min is heated to reflux in, is dried after washing repeatedly.
Step 2 takes hydrophily multi-walled carbon nanotube 50mg to be placed in 100mL small beakers, adds the ultrapure ultrasonic disperses of 20mL. Sequentially add acrylamide 1.1847g, acrylic acid 2.402g, crosslinking agent N, N'- methylene-bisacrylamide 0.0124g.Magnetic force Stirring about 1h is sealed, in 60 DEG C of water bath with thermostatic control polymerisations to being completely dissolved after adding initiator ammonium persulfate 0.0114g 6h.Obtained product will be reacted to distill water washing, soaked 3 days afterwards, regularly change water daily to go unless gel section, 70 DEG C Freeze-day with constant temperature sieves standby to constant weight after xerogel is crushed.
Embodiment 8：
Step 1: CNT is modified into processing, hydrophilic multi-walled carbon nanotube is made.CNT is taken to be put into 4mol/L HCL is heated to reflux 6h, is 98%H with concentration after filtration washing2SO4And HNO3Mixed liquor (volume ratio V:V=3: 1) 30min is heated to reflux in, is dried after washing repeatedly.
Step 2: taking hydrophily multi-walled carbon nanotube 100mg to be placed in 100mL small beakers, the ultrapure ultrasounds point of 20mL are added Dissipate.Sequentially add acrylamide 1.1847g, acrylic acid 2.402g, crosslinking agent N, N'- methylene-bisacrylamide 0.0031g.Magnetic Power stirs about 1h to being completely dissolved, and is sealed after adding initiator ammonium persulfate 0.0228g, in 60 DEG C of water bath with thermostatic control polymerisations 6h.Obtained product will be reacted to distill water washing, soaked 3 days afterwards, regularly change water daily to go unless gel section, 70 DEG C Freeze-day with constant temperature sieves standby to constant weight after xerogel is crushed.
Embodiment 9：
Step 1: CNT is modified into processing, hydrophilic multi-walled carbon nanotube is made.CNT is taken to be put into 4mol/L HCL is heated to reflux 6h, is 98%H with concentration after filtration washing2SO4And HNO3Mixed liquor (volume ratio V:V=3: 1) 30min is heated to reflux in, is dried after washing repeatedly.
Step 2: taking hydrophily multi-walled carbon nanotube 25mg to be placed in 100mL small beakers, the ultrapure ultrasounds point of 20mL are added Dissipate.Sequentially add acrylamide 1.1847g, acrylic acid 2.402g, crosslinking agent N, N'- methylene-bisacrylamide 0.0062g.Magnetic Power stirs about 1h to being completely dissolved, and is sealed after adding initiator ammonium persulfate 0.0456g, in 60 DEG C of water bath with thermostatic control polymerisations 6h.Obtained product will be reacted to distill water washing, soaked 3 days afterwards, regularly change water daily to go unless gel section, 70 DEG C Freeze-day with constant temperature sieves standby to constant weight after xerogel is crushed.
Embodiment 10：
Step 1: CNT is modified into processing, hydrophilic multi-walled carbon nanotube is made.CNT is taken to be put into 4mol/L HCL is heated to reflux 6h, is 98%H with concentration after filtration washing2SO4And HNO3Mixed liquor (volume ratio V:V=3: 1) 30min is heated to reflux in, is dried after washing repeatedly.
Step 2: taking hydrophily multi-walled carbon nanotube 50mg to be placed in 100mL small beakers, the ultrapure ultrasounds point of 20mL are added Dissipate.Sequentially add acrylamide 1.1847g, acrylic acid 2.402g, crosslinking agent N, N'- methylene-bisacrylamide 0.0124g.Magnetic Power stirs about 1h to being completely dissolved, and is sealed after adding initiator ammonium persulfate 0.0228g, in 60 DEG C of water bath with thermostatic control polymerisations 6h.Obtained product will be reacted to distill water washing, soaked 3 days afterwards, regularly change water daily to go unless gel section, 70 DEG C Freeze-day with constant temperature sieves standby to constant weight after xerogel is crushed.
Experimental example 1：
CNT hydrogel made from embodiment 10 is carried out into influence of the dosage to Dye Adsorption effect to test.
Configuration concentration is 1000mg/L alkaline safranine, crystal violet, malachite green dye solution.Weigh after drying screening Each three parts of CNT hydrogel powders 0.0063g, 0.0125g, 0.025g, 0.05g, 0.1g, 0.15g, 0.2g, 0.25g In 100mL conical flasks, 50mL, 1000mg/L three kinds of dye solutions are separately added into, with 200r/min constant temperature oscillations 24h.
It is static after taking-up, supernatant is taken, is diluted, surveys the extinction of solution in maximum absorption wave strong point with ultraviolet specrophotometer Degree, adsorbance Qe (mg/g) and clearance R (%) are calculated by the change of absorbance before and after absorption.
As a result show, adsorbance declines significantly depending on the increase of adsorbent amount, and adsorption rate increases with the increase of dosage Add, during adsorbent amount 0.05g, adsorption rate rises slow, hereafter continues to increase adsorbent amount, adsorption rate gaining rate tends to be flat Surely.Economically to set out, it is contemplated that adsorbance and adsorption rate are all tried one's best in the case of higher, therefore, this experimental selection Alkaline safranine, crystal violet, the adsorbent amount of malachite green are advisable for 0.05g (1g/L).
Experimental example 2：
CNT hydrogel made from embodiment 10 is carried out into influence of the adsorption temp to Dye Adsorption effect to test.
Configuration concentration is 1000mg/L alkaline safranine, crystal violet, malachite green dye solution.Weigh after drying screening CNT hydrogel powders 0.05g in each 100mL conical flasks, three kinds of dyestuffs for being separately added into 50mL, 1000mg/L are molten Liquid, respectively in 10 DEG C, 20 DEG C, 30 DEG C, 40 DEG C, 50 DEG C with 200r/min constant temperature oscillations 24h.
It is static after taking-up, supernatant is taken, is diluted, surveys the extinction of solution in maximum absorption wave strong point with ultraviolet specrophotometer Degree, adsorbance Qe (mg/g) and clearance R (%) are calculated by the change of absorbance before and after absorption.
Generally, MWNT/P (AA-AM) hydrogels are not single to the adsorbance variation with temperature of dyestuff, and this can When can be due to temperature change, absorption-desorption balance to adsorb and desorption direction moves back and forth so that adsorbance rise and under Drop.
Experimental example 3：
CNT hydrogel made from embodiment 10 is carried out into influence of the solution PH to Dye Adsorption effect to test.
Configuration concentration is 1000mg/L alkaline safranine, crystal violet, malachite green dye solution.Weigh after drying screening CNT hydrogel powders 0.05g in each 100mL conical flasks, three kinds of dyestuffs for being separately added into 50mL, 1000mg/L are molten Liquid, regulation solution PH is respectively to 3,5,7,9, with 200r/min constant temperature oscillations 24h.
It is static after taking-up, supernatant is taken, is diluted, surveys the extinction of solution in maximum absorption wave strong point with ultraviolet specrophotometer Degree, adsorbance Qe (mg/g) and clearance R (%) are calculated by the change of absorbance before and after absorption.
As a result show, when pH value of solution=7, the adsorbance of three kinds of dyestuffs reaches maximum, illustrates dye solution in pH Value level off to neutrality when be more conducive to the progress of adsorption reaction.This may be because under strongly acidic conditions, H+ be more adsorbed onto water On gel, so as to cause the decline to Dye Adsorption ability.
Experimental example 4：
CNT hydrogel made from embodiment 10 is carried out into influence of the adsorption time to Dye Adsorption effect to test.
Configuration concentration is 1000mg/L alkaline safranine, crystal violet, malachite green dye solution.Weigh after drying screening CNT hydrogel powders 0.05g several pieces in 100mL conical flasks, be separately added into three kinds of 50mL, 1000mg/L dyes Solution is expected, with 200r/min constant temperature oscillations.30s, 1min, 2min, 3min, 4min, 5min, 10min, 15min, 20min, 25min, 30min, 35min, 40min, 45min, 50min, 55min, 60min, 90min, 120min, 150min, 180min points Not Qu Chu three kinds of dyestuff supernatants, dilution, with ultraviolet specrophotometer maximum absorption wave strong point survey solution absorbance, pass through The change of absorbance calculates adsorbance Qe (mg/g) and clearance R (%) before and after absorption.
Experimental example 5：
CNT hydrogel made from embodiment 10 is carried out into influence of the dye strength to adsorption effect to test.
Configuration concentration is respectively 25,50,75,100,200,400,600,800,1000,2000mg/L alkaline safranine, Crystal violet, malachite green dye solution, 50mL is respectively taken in 100mL conical flasks.The carbon nanometer added in every part after drying screening Pipe hydrogel powders 0.05g, with 200r/min constant temperature oscillations 24h.
It is static after taking-up, supernatant is taken, is diluted, surveys the extinction of solution in maximum absorption wave strong point with ultraviolet specrophotometer Degree, adsorbance Qe (mg/g) and clearance R (%) are calculated by the change of absorbance before and after absorption.
Experimental example 6：
0.05g dry gel powders absorption 1000mg/L three kinds of dye solutions are taken, after adsorption equilibrium, takes filtrate to survey solution and inhales Luminosity draws adsorbance.Gel after absorption is full weighs 0.05g, is put into 0.1mol/L HCL solution solutions through being dehydrated, after drying 24h is inhaled, removes dyestuff of the absorption on gel.After desorption, with a small amount of ultrapure water gel surface, dehydrate.Again with again Gel after life does adsorption experiment, seeks its adsorbance.Repeated regeneration 3 times, the results are shown in Table 1.By the absorption regeneration of 3 times repeatedly Afterwards, the regenerative adsorption amount of hydrogel is still preferable, and after adsorption/desorption, the hydrogel regenerative adsorption amount after desorbing twice is several It is not affected, or even third time absorption is once adsorbed better than preceding.Illustrate that this hydrogel can be reclaimed to a certain extent Recycle.
Table 1

Claims (4)

  1. A kind of 1. preparation method of CNT hydrogel, it is characterised in that：Its method is as described below：
    Step 1: CNT is modified into processing, hydrophilic multi-walled carbon nanotube is made, takes CNT 4mol/L's HCL is heated to reflux 6h, after filtration washing, with the H that concentration is 98%2SO4And HNO3Mixed liquor in be heated to reflux 30min, mix H in liquid2SO4And HNO3Volume ratio be 3:1, dried after washing repeatedly；
    Step 2: hydrophily multi-walled carbon nanotube made from step 1 is placed in beaker, addition ultra-pure water, ultrasonic disperse, with 1：1 or 1：2 or 2:1 mol ratio of one of them adds acrylamide and acrylic acid, adds acrylamide and acrylic acid gross weight 0.4%-1.6% crosslinking agent N, N'- methylene-bisacrylamide is measured, magnetic agitation 1h adds acrylamide to being completely dissolved Seal with after acrylic acid gross weight 1%-4% initiator ammonium persulfate, in 60 DEG C of water bath with thermostatic control polymerisation 2-6h, will react Obtained product regularly changes water to go unless gel section, 60 DEG C of -80 DEG C of freeze-day with constant temperature to constant weight with water washing, immersion, you can Obtain CNT hydrogel.
  2. A kind of 2. preparation method of CNT hydrogel according to claim 1, it is characterised in that：Described step one A diameter of 20-30nm of middle CNT, length are 0.5-2 μm.
  3. A kind of 3. preparation method of CNT hydrogel according to claim 1, it is characterised in that：Described step two In the input amount of hydrophilic multi-walled carbon nanotube be the 0.03% of acrylamide and acrylic acid gross weight.
  4. 4. the CNT hydrogel described in claims 1 to 3 is removing the application of Wastewater Dyes.
CN201711067872.XA 2017-11-03 2017-11-03 The Preparation method and use of CNT hydrogel Pending CN107774237A (en)

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CN111085178A (en) * 2018-10-24 2020-05-01 中国石油化工股份有限公司 Preparation method and application of acrylamide polymer containing carbon nano-tube
CN110201652A (en) * 2019-06-17 2019-09-06 甘肃农业大学 A kind of preparation method of the Carbon Nanotubes/Chitosan hydrogel with three-dimensional net structure
US11746177B2 (en) 2019-10-18 2023-09-05 Imam Abdulrahman Bin Faisal University Method for removing organic pollutants from water
US11976152B2 (en) 2019-10-18 2024-05-07 Imam Abdulrahman Bin Faisal University Water purification method with nanocomposite sorbent
US11414513B2 (en) 2019-10-18 2022-08-16 Imam Abdulrahman Bin Faisal University Method of producing a carbon nanotube grafted acrylic acid/acrylamide copolymer nanocomposite sorbent
CN112625769A (en) * 2020-11-30 2021-04-09 青岛科技大学 Method for promoting rapid generation of methane hydrate by using carbon nano tube composite hydrogel
CN113307909A (en) * 2021-06-22 2021-08-27 武汉轻工大学 Hydrogel filled with nitrogen-doped carbon nanotubes and preparation method thereof
US20230312840A1 (en) * 2021-12-13 2023-10-05 Guangdong Ocean University Method for preparing carbon nanotube/polyacrylic acid hydrogel, product and application thereof
WO2023108868A1 (en) * 2021-12-13 2023-06-22 广东海洋大学 Preparation method for carbon nano tube/polyacrylic acid hydrogel, and product and application of carbon nano tube/polyacrylic acid hydrogel
US11958946B2 (en) * 2021-12-13 2024-04-16 Guangdong Ocean University Method for preparing carbon nanotube/polyacrylic acid hydrogel, product and application thereof
CN114031710A (en) * 2021-12-13 2022-02-11 广东海洋大学 Preparation method of carbon nanotube/polyacrylic acid hydrogel, product and application thereof
CN115746486A (en) * 2022-10-28 2023-03-07 青岛科技大学 Preparation method of efficient and stable hydrogel-based gas hydrate accelerant
CN115746486B (en) * 2022-10-28 2023-10-24 青岛科技大学 Preparation method of efficient and stable hydrogel-based gas hydrate accelerator

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