CN106423072A - Graphene oxide-sulfhydryl compound composite capable of adsorbing heavy metal ions and preparation method of graphene oxide-sulfhydryl compound composite - Google Patents
Graphene oxide-sulfhydryl compound composite capable of adsorbing heavy metal ions and preparation method of graphene oxide-sulfhydryl compound composite Download PDFInfo
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- CN106423072A CN106423072A CN201610837300.4A CN201610837300A CN106423072A CN 106423072 A CN106423072 A CN 106423072A CN 201610837300 A CN201610837300 A CN 201610837300A CN 106423072 A CN106423072 A CN 106423072A
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- 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
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- 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
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- 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
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Abstract
The invention relates to the technical field of adsorbing materials, and particularly discloses a graphene oxide-sulfhydryl compound composite capable of adsorbing heavy metal ions and a preparation method of the graphene oxide-sulfhydryl compound composite. The composite is prepared from graphene oxide and a sulfhydryl-containing organic compound through a grafting reaction. The graphene oxide-sulfhydryl compound composite is prepared through the grafting reaction of oxygen-containing functional groups (carboxyl groups and hydroxyl groups) on the surface of the graphene oxide with amino groups or hydroxyl groups in the sulfhydryl-containing organic compound. The effect of removing pollution of the heavy metal ions (Cd<2+> and Ni<2+>) is realized by the larger specific surface area of the graphene oxide as well as an action of strong chelation of the heavy metal ions (Cd<2+> and Ni<2+>) with the oxygen-containing functional groups on the surface of the graphene oxide and the sulfydryl groups of the composite. The novel graphene-based adsorbing material adopting a preparation process and having high adsorbing capacity is provided, the application range of the graphene material in the field of environmental protection is broadened, the purpose of environmental protection is achieved, and good social benefit and environmental protection benefit are realized.
Description
Technical field
The present invention relates to sorbing material technical field, in particular it relates to the graphene oxide of a kind of Adsorption of Heavy Metal Ions-
Sulfhydryl compound composite and preparation method thereof.
Background technology
Along with works such as the fast development of human society, mine, smelting, electrolysis, plating, agricultural chemicals, medicine, paint, pigment
A large amount of heavy metal-containing waste waters that industry production activity produces are also increasingly severe to the pollution of environment.Owing to heavy metal ion has not
The feature being easily biodegradable, it can be circulated by biological chain progress into plant, animal body, and is enriched with wherein, and
Jeopardize the own health of the mankind eventually.Therefore how effectively to remove heavy metal ions in wastewater have become as the mankind must faced by
Problem.Comparing other heavy metals removal methods, absorption method is owing to having low cost, and efficiency is high, and operation is simple, widely should have
Use prospect.
The main active charcoal of adsorbent common in engineering field, zeolite, mesoporous material, resin and high molecular polymer
Deng.But there is the defects such as adsorption capacity is little, adsorption efficiency is on the low side in these common adsorbents.In recent years, with graphene oxide（GO）
For the carbon nanomaterial representing, owing to it has the hollow structure of uniqueness, powerful adsorption capacity and high surface area etc.,
Through becoming the focus of countries in the world environmental area expert research.Zhao Xiaowei et al. GO/ZnO is that adsorbent is to Cu2+And Pb2+Enter
Row absorption, its maximal absorptive capacity is respectively 37.45mg/g and 23.42mg/g.Li Jie et al. uses GO/Fe3O4As adsorbent pair
Cu2+Adsorbing, its maximal absorptive capacity is 18.26mg/g.Yellow center of percussion et al. low temperature peels off graphene nanometer sheet to Pb2+Enter
Row absorption, its maximal absorptive capacity is 22.42～35.46mg/g.Wu Wenqing et al. uses GO as adsorbent to Cu2+Adsorb,
Its maximal absorptive capacity is 117.5mg/g.Although existing multiple ABSORBENTS ABSORPTION gold including graphene oxide composite material
Belong to ion there is certain absorption to remove effect, but have that composite preparation process is complicated or adsorption effect is not also especially good
Defect.
Content of the invention
The invention aims to overcome the inefficient difficult problem of existing sorbing material Adsorption of Heavy Metal Ions, one is provided
The graphene oxide of Adsorption of Heavy Metal Ions-sulfhydryl compound composite.
Graphene oxide-the sulfhydryl compound that it is a further object to provide a kind of Adsorption of Heavy Metal Ions is combined
The preparation method of material.
To achieve these goals, the present invention is achieved by the following technical programs：
The graphene oxide of a kind of Adsorption of Heavy Metal Ions-sulfhydryl compound composite, has by graphene oxide with containing sulfydryl
Machine compound grafting reaction prepares；Described organic compound containing sulfydryl is simultaneously also with amino or hydroxyl.
The present invention utilizes the oxygen-containing functional group of surface of graphene oxide（Carboxyl and hydroxyl）With in organic compound containing sulfydryl
Amino or hydroxyl grafting reaction, quickly, simply prepare a kind of novel oxidized Graphene-sulfhydryl compound sorbing material, multiple
-SH the base that sulfhydryl compound molecule in condensation material contains can be with heavy metal ion（Especially Cd2+、Ni2+）Strong chelating, right
Heavy metal ion has very strong suction-operated；Graphene oxide has gap structure, and there are a large amount of oxygen-containing functional group, and specific surface in surface
Long-pending relatively big, utilize amino or the hydroxyl grafting of graphene oxide oxygen-containing functional group and sulfhydryl compound to react the composite adsorption obtaining
Material can good Adsorption of Heavy Metal Ions.
Preferably, described organic compound containing sulfydryl is Cys, nabam, 2-amino-5-mercapto
Base-1,3,4-thiadiazoles, ethyl mercaptan or thioxanthamide.
The present invention is also claimed application in Adsorption of Heavy Metal Ions for the composite.Especially composite is in absorption
Cd2+、Ni2+In application.
The preparation method of the graphene oxide of a kind of Adsorption of Heavy Metal Ions-sulfhydryl compound composite, comprises following
Step：
(1) add graphene oxide into ultrasonic disperse in ultra-pure water, obtain relatively uniform graphene oxide suspension；
(2) adding compounds containing thiol groups in above-mentioned graphene oxide suspension, then adding NaOH, mixed solution continues super
Sound；
(3) after above-mentioned mixed liquor Ethanol Treatment, through ultrafiltration membrance filter, ethanol/water solution is washed, and vacuum drying obtains oxidation
Graphene-sulfhydryl compound composite.
Preferably, the concentration of described graphene oxide suspension is 0.5～1mg/mL.
Preferably, the mass ratio of described graphene oxide and compounds containing thiol groups is 1：0.1～0.5.
Preferably, the mol ratio of described compounds containing thiol groups and NaOH is 1：1～1.5.
Preferably, described organic compound containing sulfydryl is Cys, nabam, 2-amino-5-mercapto
Base-1,3,4-thiadiazoles, ethyl mercaptan or thioxanthamide.
Preferably, described ethanol/water solution is the ethanol/water solution of 0.5%.
A kind of method that heavy-metal ion removal pollutes, comprises the following steps：With the injected volume of 2.0～2.5g/L by this
Bright composite put into 25～45mg/L contain Cd2+、Ni2+In sewage, concussion, adsorb 20～30min, compound after absorption
Material is to Cd2+、Ni2+Adsorbance be 72～88mg/g.
Compared with prior art, the present invention has the advantages that：
Graphene oxide-sulfhydryl compound composite that the present invention provides, preparation technology is simple, raw material sources are extensive, price
Cheap, it is easy to industrialized production；Composite after a procedure, can reclaim heavy metal ion, heavy metal through simple chemical treatment
Adsorbance is big, and adsorption process non-secondary pollution has widened the range of application at field of Environment Protection for the grapheme material, it is achieved that protection ring
The purpose in border, has good social benefit and environmental benefit.
Detailed description of the invention
Making the present invention below in conjunction with specific embodiment and elaborating further, described embodiment is served only for explaining this
Invention, is not intended to limit the scope of the present invention.Test method used in following embodiment if no special instructions, is often
Rule method；The material that used, reagent etc., if no special instructions, for the reagent that commercially obtains and material.
Embodiment 1
A kind of graphene oxide-sulfhydryl compound composite, is prepared by following methods：
(1) add graphene oxide into ultrasonic vibration 1h in ultra-pure water, obtain relatively uniform graphene oxide suspension, oxidation
Graphene suspension concentration is 1mg/mL；
(2) in above-mentioned 10mL graphene oxide suspension, add the Cys of 1 mg, make graphene oxide and L-half Guang
Propylhomoserin mass ratio is 1：0.1, then add the NaOH of equimolar amounts, mixed solution ultrasonic reaction 1h；
(3), after above-mentioned mixed liquor 40ml Ethanol Treatment, with 0.22 μm of ultrafiltration membrance filter, the ethanol/water solution washing of 0.5%, incite somebody to action
Gained solids is vacuum dried at 80 DEG C, graphene oxide/Cys composite adsorbing material.
Graphene oxide-sulfhydryl compound composite is to Cd2+Absorption：Under the steady temperature of 25 DEG C, by 0.05g's
Graphene oxide/Cys composite adsorbing material is placed in the Cd of 20ml concentration series change2+Solution is respectively placed in some tools
In plug conical flask, regulate pH=6.0 with the diluted sodium hydroxide solution and hydrogenperoxide steam generator of 0.1mol/L, in constant temperature oscillator
Concussion 1h, makes graphene oxide/Cys composite to Cd2+Absorption reach saturated.With 0.22 μm of ultrafiltration membrance filter,
The ethanol/water solution washing of 0.5%, collects filtrate, with ICP-OES test, calculates graphene oxide/Cys and is combined
Sorbing material is to Cd2+Adsorbance be 84mg/g.
Embodiment 2
A kind of graphene oxide-sulfhydryl compound composite, is prepared by following methods：
(1) add graphene oxide into ultrasonic vibration 1h in ultra-pure water, obtain relatively uniform graphene oxide suspension, oxidation
Graphene suspension concentration is 1mg/mL；
(2) in above-mentioned 10mL graphene oxide suspension, add the nabam of 1 mg, make graphene oxide with
Nabam mass ratio is 1：0.1, then add the NaOH of equimolar amounts, mixed solution ultrasonic reaction 1h；
(3), after above-mentioned mixed liquor 40ml Ethanol Treatment, with 0.22 μm of ultrafiltration membrance filter, the ethanol/water solution washing of 0.5%, incite somebody to action
Gained solids is vacuum dried at 80 DEG C, graphene oxide/nabam composite adsorbing material.
Graphene oxide-sulfhydryl compound composite is to Cd2+Absorption：Under the steady temperature of 25 DEG C, by 0.05g's
Graphene oxide/nabam composite is placed in the Cd of 20ml concentration series change2+Solution, is respectively placed in some
In tool plug conical flask, regulate pH=6.0 with the diluted sodium hydroxide solution and hydrogenperoxide steam generator of 0.1mol/L, at constant temperature oscillator
Middle concussion 1h, makes graphene oxide/nabam composite adsorbing material to Cd2+Absorption reach saturated.Use 0.22 μ
M ultrafiltration membrance filter, the ethanol/water solution washing of 0.5%, collect filtrate, with ICP-OES test, calculate graphene oxide/bis-
Thiocarbamic acid sodium composite adsorbing material is to Cd2+Adsorbance be 77mg/g.
Embodiment 3
A kind of graphene oxide-sulfhydryl compound composite, is prepared by following methods：
(1) add graphene oxide into ultrasonic vibration 1h in ultra-pure water, obtain relatively uniform graphene oxide suspension, oxidation
Graphene suspension concentration is 0.5mg/mL；
(2) in above-mentioned 10mL graphene oxide suspension, add 2-amino-5-sulfydryl-1 of 1 mg, 3,4-thiadiazoles, make oxygen
Functionalized graphene and 2-amino-5-sulfydryl-1,3,4-thiadiazoles mass ratio are 1：0.2, then add the NaOH of equimolar amounts, mixed
Close solution ultrasonic reaction 1h；
(3), after above-mentioned mixed liquor 40ml Ethanol Treatment, with 0.22 μm of ultrafiltration membrance filter, the ethanol/water solution washing of 0.5%, incite somebody to action
Gained solids is vacuum dried at 80 DEG C, graphene oxide/2-amino-5-sulfydryl-1,3,4-thiadiazoles are compound to be inhaled
Enclosure material.
Graphene oxide-sulfhydryl compound composite adsorbing material is to Cd2+Absorption：Under the steady temperature of 25 DEG C, will
The graphene oxide of 0.05g/2-amino-5-sulfydryl-1,3,4-thiadiazoles composite adsorbing material is placed in the change of 20ml concentration series
Cd2+Solution is respectively placed in some tool plug conical flasks, is adjusted by the diluted sodium hydroxide solution and hydrogenperoxide steam generator of 0.1mol/L
Joint pH=6.0, shakes 1h in constant temperature oscillator, makes graphene oxide/2-amino-5-sulfydryl-1,3,4-thiadiazoles composite adsorptions
Material is to Cd2+Absorption reach saturated.With 0.22 μm of ultrafiltration membrance filter, the ethanol/water solution washing of 0.5%, collect filtrate, use
ICP-OES tests, and calculates graphene oxide/2-amino-5-sulfydryl-1, and 3,4-thiadiazoles composite adsorbing materials are to Cd2+Suction
Attached amount is 72mg/g.
Embodiment 4
A kind of graphene oxide-sulfhydryl compound composite, is prepared by following methods：
(1) add graphene oxide into ultrasonic vibration 1h in ultra-pure water, obtain relatively uniform graphene oxide suspension, oxidation
Graphene suspension concentration is 1mg/mL；
(2) in above-mentioned 10mL graphene oxide suspension, add the ethyl mercaptan of 3 mg, make graphene oxide and ethyl mercaptan quality
Ratio is 1：0.3, then add the NaOH of equimolar amounts, mixed solution ultrasonic reaction 1h；
(3), after above-mentioned mixed liquor 40ml Ethanol Treatment, with 0.22 μm of ultrafiltration membrance filter, the ethanol/water solution washing of 0.5%, incite somebody to action
Gained solids is vacuum dried at 80 DEG C, graphene oxide/ethyl mercaptan composite adsorbing material.
Graphene oxide-sulfhydryl compound composite adsorbing material is to Cd2+Absorption：Under the steady temperature of 25 DEG C, will
The graphene oxide of 0.05g/ethyl mercaptan composite adsorbing material is placed in the Cd of 20ml concentration series change2+Solution is respectively placed in some
In tool plug conical flask, regulate pH=6.0 with the diluted sodium hydroxide solution and hydrogenperoxide steam generator of 0.1mol/L, at constant temperature oscillator
Middle concussion 1h, makes graphene oxide/ethyl mercaptan composite adsorbing material to Cd2+Absorption reach saturated.By 0.22 μm of milipore filter mistake
Filter, the ethanol/water solution washing of 0.5%, collect filtrate, with ICP-OES test, calculate the compound suction of graphene oxide/ethyl mercaptan
Enclosure material is to Cd2+Adsorbance be 88mg/g.
Embodiment 5
A kind of graphene oxide-sulfhydryl compound composite, is prepared by following methods：
(1) add graphene oxide into ultrasonic vibration 1h in ultra-pure water, obtain relatively uniform graphene oxide suspension, oxidation
Graphene suspension concentration is 0.5mg/mL；
(2) in above-mentioned 10mL graphene oxide suspension, add the thioxanthamide of 2 mg, make graphene oxide with
Thioxanthamide mass ratio is 1:0.4, then add the NaOH of equimolar amounts, mixed solution ultrasonic reaction 1h；
(3), after above-mentioned mixed liquor 40ml Ethanol Treatment, with 0.22 μm of ultrafiltration membrance filter, the ethanol/water solution washing of 0.5%, incite somebody to action
Gained solids is vacuum dried at 80 DEG C, graphene oxide/thioxanthamide composite adsorbing material.
Graphene oxide-sulfhydryl compound composite adsorbing material is to Cd2+Absorption：Under the steady temperature of 25 DEG C, will
The graphene oxide of 0.05g/thioxanthamide composite adsorbing material is placed in the Cd of 20ml concentration series change2+Solution divides
It is not placed in some tool plug conical flasks, regulate pH=6.0 with the diluted sodium hydroxide solution and hydrogenperoxide steam generator of 0.1mol/L,
Constant temperature oscillator shakes 1h, makes graphene oxide/thioxanthamide composite adsorbing material to Cd2+Absorption reach full
With.With 0.22 μm of ultrafiltration membrance filter, the ethanol/water solution washing of 0.5%, collect filtrate, with ICP-OES test, calculate oxidation
Graphene/thioxanthamide composite adsorbing material is to Cd2+Adsorbance be 80mg/g.
Embodiment 6
A kind of graphene oxide-sulfhydryl compound composite, is prepared by following methods：
(1) add graphene oxide into ultrasonic vibration 1h in ultra-pure water, obtain relatively uniform graphene oxide suspension, oxidation
Graphene suspension concentration is 1mg/mL；
(2) in above-mentioned 10mL graphene oxide suspension, add the Cys of 3 mg, make graphene oxide and L-half Guang
Propylhomoserin mass ratio is 1:0.3, then add the NaOH of equimolar amounts, mixed solution ultrasonic reaction 1h；
(3), after above-mentioned mixed liquor 40ml Ethanol Treatment, with 0.22 μm of ultrafiltration membrance filter, the ethanol/water solution washing of 0.5%, incite somebody to action
Gained solids is vacuum dried at 80 DEG C, graphene oxide/Cys composite adsorbing material.
Graphene oxide-sulfhydryl compound composite adsorbing material is to Ni2+Absorption：Under the steady temperature of 25 DEG C, will
The graphene oxide of 0.05g/Cys composite adsorbing material is placed in the Ni of 20ml concentration series change2+Solution is respectively placed in
In some tool plug conical flasks, regulate pH=6.0 with the diluted sodium hydroxide solution and hydrogenperoxide steam generator of 0.1mol/L, shake at constant temperature
Swing concussion 1h in device, make graphene oxide/Cys composite adsorbing material to Ni2+Absorption reach saturated.With 0.22 μm
Ultrafiltration membrance filter, the ethanol/water solution washing of 0.5%, collect filtrate, with ICP-OES test, calculate graphene oxide/L-half
Cystine composite adsorbing material is to Ni2+Adsorbance be 76mg/g.
Embodiment 7
A kind of graphene oxide-sulfhydryl compound composite, is prepared by following methods：
(1) add graphene oxide into ultrasonic vibration 1h in ultra-pure water, obtain relatively uniform graphene oxide suspension, oxidation
Graphene suspension concentration is 0.5mg/mL；
(2) in above-mentioned 10mL graphene oxide suspension, add the nabam of 1 mg, make graphene oxide with
Nabam mass ratio is 1:0.2, then add the NaOH of equimolar amounts, mixed solution ultrasonic reaction 1h；
(3), after above-mentioned mixed liquor 40ml Ethanol Treatment, with 0.22 μm of ultrafiltration membrance filter, the ethanol/water solution washing of 0.5%, incite somebody to action
Gained solids is vacuum dried at 80 DEG C, graphene oxide/nabam composite adsorbing material.
Graphene oxide-sulfhydryl compound composite adsorbing material is to Ni2+Absorption：Under the steady temperature of 25 DEG C, will
The graphene oxide of 0.05g/nabam composite adsorbing material is placed in the Ni of 20ml concentration series change2+Solution divides
It is not placed in some tool plug conical flasks, regulate pH=6.0 with the diluted sodium hydroxide solution and hydrogenperoxide steam generator of 0.1mol/L,
Constant temperature oscillator shakes 1h, makes graphene oxide/nabam composite adsorbing material to Ni2+Absorption reach full
With.With 0.22 μm of ultrafiltration membrance filter, the ethanol/water solution washing of 0.5%, collect filtrate, with ICP-OES test, calculate oxidation
Graphene/nabam composite adsorbing material is to Ni2+Adsorbance be 76mg/g.
Embodiment 8
A kind of graphene oxide-sulfhydryl compound composite, is prepared by following methods：
(1) add graphene oxide into ultrasonic vibration 1h in ultra-pure water, obtain relatively uniform graphene oxide suspension, oxidation
Graphene suspension concentration is 1mg/mL；
(2) in above-mentioned 10mL graphene oxide suspension, add 2-amino-5-sulfydryl-1 of 3 mg, 3,4-thiadiazoles, make oxygen
Functionalized graphene and 2-amino-5-sulfydryl-1,3,4-thiadiazoles mass ratio are 1:0.3, then add the NaOH of equimolar amounts, mixed
Close solution ultrasonic reaction 1h；
(3), after above-mentioned mixed liquor 40ml Ethanol Treatment, with 0.22 μm of ultrafiltration membrance filter, the ethanol/water solution washing of 0.5%, incite somebody to action
Gained solids is vacuum dried at 80 DEG C, graphene oxide/2-amino-5-sulfydryl-1,3,4-thiadiazoles are compound to be inhaled
Enclosure material.
Graphene oxide-sulfhydryl compound composite adsorbing material is to Ni2+Absorption：Under the steady temperature of 25 DEG C, will
The graphene oxide of 0.05g/2-amino-5-sulfydryl-1,3,4-thiadiazoles composite adsorbing material is placed in the change of 20ml concentration series
Ni2+Solution is respectively placed in some tool plug conical flasks, is adjusted by the diluted sodium hydroxide solution and hydrogenperoxide steam generator of 0.1mol/L
Joint pH=6.0, shakes 1h in constant temperature oscillator, makes graphene oxide/2-amino-5-sulfydryl-1,3,4-thiadiazoles composite adsorptions
Material is to Ni2+Absorption reach saturated.With 0.22 μm of ultrafiltration membrance filter, the ethanol/water solution washing of 0.5%, collect filtrate, use
ICP-OES tests, and calculates graphene oxide/2-amino-5-sulfydryl-1, and 3,4-thiadiazoles composite adsorbing materials are to Ni2+Suction
Attached amount is 78mg/g.
Embodiment 9
A kind of graphene oxide-sulfhydryl compound composite, is prepared by following methods：
(1) add graphene oxide into ultrasonic vibration 1h in ultra-pure water, obtain relatively uniform graphene oxide suspension, oxidation
Graphene suspension concentration is 0.5mg/mL；
(2) in above-mentioned 10mL graphene oxide suspension, add the ethyl mercaptan of 1 mg, make graphene oxide and ethyl mercaptan quality
Ratio is 1:0.2, then add the NaOH of equimolar amounts, mixed solution ultrasonic reaction 1h；
(3), after above-mentioned mixed liquor 40ml Ethanol Treatment, with 0.22 μm of ultrafiltration membrance filter, the ethanol/water solution washing of 0.5%, incite somebody to action
Gained solids is vacuum dried at 80 DEG C, graphene oxide/ethyl mercaptan composite adsorbing material.
Graphene oxide-sulfhydryl compound composite adsorbing material is to Ni2+Absorption：Under the steady temperature of 25 DEG C, will
The graphene oxide of 0.05g/ethyl mercaptan composite adsorbing material is placed in the Ni of 20ml concentration series change2+Solution is respectively placed in some
In tool plug conical flask, regulate pH=6.0 with the diluted sodium hydroxide solution and hydrogenperoxide steam generator of 0.1mol/L, at constant temperature oscillator
Middle concussion 1h, makes graphene oxide/ethyl mercaptan composite adsorbing material to Ni2+Absorption reach saturated.By 0.22 μm of milipore filter mistake
Filter, the ethanol/water solution washing of 0.5%, collect filtrate, with ICP-OES test, calculate the compound suction of graphene oxide/ethyl mercaptan
Enclosure material is to Ni2+Adsorbance be 81mg/g.
Embodiment 10
A kind of graphene oxide-sulfhydryl compound composite, is prepared by following methods：
(1) add graphene oxide into ultrasonic vibration 1h in ultra-pure water, obtain relatively uniform graphene oxide suspension, oxidation
Graphene suspension concentration is 1mg/mL；
(2) in above-mentioned 10mL graphene oxide suspension, add the thioxanthamide of 3 mg, make graphene oxide with
Thioxanthamide mass ratio is 1:0.3, then add the NaOH of equimolar amounts, mixed solution ultrasonic reaction 1h；
(3), after above-mentioned mixed liquor 40ml Ethanol Treatment, with 0.22 μm of ultrafiltration membrance filter, the ethanol/water solution washing of 0.5%, incite somebody to action
Gained solids is vacuum dried at 80 DEG C, graphene oxide/thioxanthamide composite adsorbing material.
Graphene oxide-sulfhydryl compound composite adsorbing material is to Ni2+Absorption：Under the steady temperature of 25 DEG C, will
The graphene oxide of 0.05g/thioxanthamide composite adsorbing material is placed in the Ni of 20ml concentration series change2+Solution divides
It is not placed in some tool plug conical flasks, regulate pH=6.0 with the diluted sodium hydroxide solution and hydrogenperoxide steam generator of 0.1mol/L,
Constant temperature oscillator shakes 1h, makes graphene oxide/thioxanthamide composite adsorbing material to Ni2+Absorption reach full
With.With 0.22 μm of ultrafiltration membrance filter, the ethanol/water solution washing of 0.5%, collect filtrate, with ICP-OES test, calculate oxidation
Graphene/thioxanthamide composite adsorbing material is to Ni2+Adsorbance be 73mg/g.
Claims (8)
1. the graphene oxide of an Adsorption of Heavy Metal Ions-sulfhydryl compound composite, it is characterised in that by graphite oxide
Alkene and the grafting of organic compound containing sulfydryl reaction prepare；Described organic compound containing sulfydryl is simultaneously also with amino or hydroxyl.
2. composite according to claim 1, it is characterised in that described organic compound containing sulfydryl is L-half Guang ammonia
Acid, nabam, 2-amino-5-sulfydryl-1,3,4-thiadiazoles, ethyl mercaptan or thioxanthamide.
3. application in Adsorption of Heavy Metal Ions for the composite described in claim 1 or 2.
4. the preparation method of composite described in claim 1 or 2, it is characterised in that comprise the steps of：
(1) add graphene oxide into ultrasonic disperse in ultra-pure water, obtain relatively uniform graphene oxide suspension；
(2) adding compounds containing thiol groups in above-mentioned graphene oxide suspension, then adding NaOH, mixed solution continues super
Sound；
(3) after above-mentioned mixed liquor Ethanol Treatment, through ultrafiltration membrance filter, ethanol/water solution is washed, and vacuum drying obtains oxidation
Graphene-sulfhydryl compound composite.
5. preparation method according to claim 4, it is characterised in that the concentration of described graphene oxide suspension is 0.5
～1mg/mL.
6. the preparation method according to claim 4 or 5, it is characterised in that described graphene oxide and organising containing sulfydryl
The mass ratio of compound is 1：0.1～0.5.
7. preparation method according to claim 6, it is characterised in that described organic compound containing sulfydryl and NaOH mole
Ratio is 1：1～1.5.
8. preparation method according to claim 4, it is characterised in that described organic compound containing sulfydryl is L-half Guang ammonia
Acid, dithiocar-bamate, 2-amino-5-sulfydryl-1,3,4-thiadiazoles, ethyl mercaptan or thioxanthamide.
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| CN201610837300.4A CN106423072A (en) | 2016-09-21 | 2016-09-21 | Graphene oxide-sulfhydryl compound composite capable of adsorbing heavy metal ions and preparation method of graphene oxide-sulfhydryl compound composite |
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| CN201610837300.4A CN106423072A (en) | 2016-09-21 | 2016-09-21 | Graphene oxide-sulfhydryl compound composite capable of adsorbing heavy metal ions and preparation method of graphene oxide-sulfhydryl compound composite |
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| CN110102263A (en) * | 2019-04-10 | 2019-08-09 | 中国药科大学 | Mercaptoethylmaine functional magnetic graphene oxide adsorbent and its preparation method and application |
| CN110394153A (en) * | 2019-07-05 | 2019-11-01 | 重庆科技学院 | A kind of composite material preparation method and product thereof for adsorbing palladium ions |
| CN111014275A (en) * | 2019-12-19 | 2020-04-17 | 江苏华东新能源勘探有限公司（江苏省有色金属华东地质勘查局八一三队） | Heavy metal soil remediation agent and application thereof |
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| CN112547016A (en) * | 2020-11-06 | 2021-03-26 | 惠州学院 | Graphene oxide composite material and preparation method and application thereof |
| CN112958037A (en) * | 2021-02-03 | 2021-06-15 | 中南大学 | Heteroatom-rich functionalized graphene oxide composite material and preparation method and application thereof |
| CN113070041A (en) * | 2021-04-29 | 2021-07-06 | 中科院过程工程研究所南京绿色制造产业创新研究院 | Graphene oxide-organic composite adsorption material and preparation method and application thereof |
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