CN109894100A - A kind of preparation and application of graphene oxide/iron oxide/poly- trithiocyanuric acid trisodium salt porous adsorbing material - Google Patents
A kind of preparation and application of graphene oxide/iron oxide/poly- trithiocyanuric acid trisodium salt porous adsorbing material Download PDFInfo
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- CN109894100A CN109894100A CN201910301428.2A CN201910301428A CN109894100A CN 109894100 A CN109894100 A CN 109894100A CN 201910301428 A CN201910301428 A CN 201910301428A CN 109894100 A CN109894100 A CN 109894100A
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- trisodium salt
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Abstract
The invention belongs to nanocomposites and environment remediation technical field, are related to the preparation of graphene oxide/iron oxide/poly- trithiocyanuric acid trisodium salt layered porous adsorbent material and its application in environment remediation.The present invention is anchored magnetic iron oxide, then the composite material prepared by the poly- trithiocyanuric acid trisodium salt of surface of graphene oxide in-situ deposition using graphene oxide composite material as substrate, using oxygen-containing functional group abundant.Purification of the composite material prepared by the present invention for heavy metal leads and cadmium pollution environment such as water body, soil repairs field in Heavy-metal Polluted Environment and has broad application prospects.The method of the present invention raw material is easy to get, and preparation is simple, is suitable for amplification production.
Description
Technical field
The invention belongs to nanocomposites and environment remediation technical field, and in particular to a kind of graphene oxide/oxidation
Iron/poly- trithiocyanuric acid trisodium salt layered porous adsorbent material preparation and application.
Background technique
With the development of world economy, the discharges wantonly of the trade effluents such as papermaking, electricity edge, mining, chemical fertilizer, pesticide do not conform to
Reason uses and the discharge of sanitary sewage, so that heavy metal pollution has become one of maximum water pollution problems of harm at present.By
In heavy metal ion, there are Accumulative effects, and human body can be entered by food chain and is enriched with, and damage Human autopsy tissues function
Can, seriously threaten the life and health safety of people.And heavy metal pollution of water body is administered, such as chemical precipitation method, ion are handed over
Method, membrane separation process, biomass method, electrochemical process and flocculation sedimentation etc. is changed to be reported successively and for heavy metal pollution of water body
It administers.Facts have proved: the above method has certain effect to the purification removal of heavy metal ion, but also all there are many disadvantages
End, such as be easy to cause secondary pollution, preparation method and process are more complicated, with high costs, poor selectivity etc..Absorption method is due to material
Expect from a wealth of sources, simple process, the advantages such as the rate of adsorption is fast, removal efficiency is high and can be recycled and by extensive concern.Graphite
Olefinic carbon nano material is due to huge specific surface area, unique sp2 hybridized orbit honeycomb carbon skeleton structure, stable object
Reason/chemical characteristic, and by extensive concern.
Compared with traditional materials, nano material has completely new excellent physical/chemical properties.Especially its huge compares table
Area makes it have excellent adsorption capacity to pollutant, and by extensive concern and expectation.In recent years, magnetic Nano composite wood
Material due to its can magnetic recovery, and the advantages of can cooperate with each material component of utilization and as a kind of with the new of wide application prospect
Type composite material.But there are shape unevenness for composite material synthesized by magnetic nanometer composite material preparation process in existing report
Even, functional layer material content is low, and the technical deficiencies such as easy to fall off cause magnetic nanometer composite material still not answered widely
With.
Application No. is 201310377886.7 Chinese invention patent, to disclose a kind of graphene oxide-rhamnolipid multiple
The preparation method of condensation material, specific steps are as follows: add graphene oxide into dispersing agent, form graphite oxide after ultrasonic disperse
Alkene mixed liquor;Rhamnolipid, 1- ethyl-(3- dimethylaminopropyl) carbodiimide hydrochloride and 4- are added into mixed liquor
Dimethylamino naphthyridine and ultrasonic reaction add a certain amount of anhydrous methanol stirring to generate precipitating;Precipitated product is washed and is centrifuged,
Graphene oxide-rhamnolipid composite material most is made through vacuum freeze drying afterwards.
Application No. is 201410511058.2 Chinese invention patent, to disclose a kind of use in waste water treatment graphene oxide more
Hole composite material, the parts by weight including following components and each component are respectively as follows: graphene oxide: 3-5 parts;Phyllosilicate:
2-3 parts;Gelatin: 3-5 parts.The composite porous good mechanical property of the graphene oxide that method described in the invention is prepared,
Institutional framework is regular, porosity is high and good biocompatibility, is highly suitable for absorption industry.
In recent years magnetic composite due to recycle it is convenient, while can cooperate with using each material component excellent properties and
As a kind of star's material with wide application prospect.But up to the present, graphene oxide/iron oxide/poly- three polysulfide
There is not been reported for the preparation of the layered porous adsorbent material of cyanic acid trisodium salt.
Summary of the invention
The purpose of the present invention is to provide a kind of graphene oxide/iron oxide with layered porous structure/poly- three polysulfides
The preparation method and applications of cyanic acid trisodium salt compound adsorbent.
Graphene oxide/iron oxide with layered porous structure/poly- trithiocyanuric acid trisodium salt proposed by the invention
Composite material is to be anchored magnetic iron oxide using oxygen-containing functional group abundant, then aoxidizing using graphene oxide composite material as substrate
Composite material prepared by the poly- trithiocyanuric acid trisodium salt of graphene surface in-situ deposition is simultaneously used for Heavy Metals in Waters lead
With the purification of cadmium.Its high efficiency of additive capability for combining magnetic recovery and porous material, in heavy metal-polluted water processing etc.
Field has broad application prospects.
The present invention is achieved through the following technical solutions above-mentioned technical purpose:
A kind of preparation method of graphene oxide/iron oxide/layered porous adsorbent material of poly- trithiocyanuric acid trisodium salt, including such as
Lower step:
1) by graphene oxide ultrasonic disperse into deionized water, dispersion liquid A is obtained;
2) by Superparamagnetic Iron Oxide nanoparticle ultrasonic disperse into nitric acid solution, by it after sufficiently being washed using deionized water
Again ultrasonic disperse obtains dispersion liquid B into deionized water;5min is mixed in dispersion liquid A and dispersion liquid B, obtains suspension C;
3) sodium hydroxide is dissolved in deionized water, trithiocyanuric acid stirring and dissolving is added, obtains glassy yellow clear solution D;It is mechanical
Solution d is slowly dropped into above-mentioned suspension C under stirring, room temperature continues stirring 2h and obtains mixed liquor E;
4) under ice bath and mechanical stirring, saturation KI-I is added dropwise in Xiang Shangshu mixed liquor E2Rear ice bath is added dropwise in solution
Under the conditions of continue stir 2h after be slowly increased to room temperature, be stirred overnight;It successively washs 1 time and uses using dilute hydrochloric acid after Magnetic Isolation
Deionized water is washed 3 times, and 40 DEG C of drying are cooled to room temperature to get graphene oxide/iron oxide/poly- trithiocyanuric acid trisodium salt
Layered porous adsorbent material.
As a further improvement of the present invention, the quality of the volume of the deionized water in the step 1) and graphene oxide
The ratio between be 0.4: 1~0.8: 1, wherein the volume of deionized water is in terms of milliliter, and the quality of graphene oxide is in terms of milligram.
Magnetic ferric oxide nano particles in the step 2 are one of ferroso-ferric oxide or r- di-iron trioxide.
Magnetic iron oxide partial size in the step 2 is 8-12nm, and the concentration of nitric acid is 2M.
The volume ratio of the quality of iron oxide in the step 2, the volume of nitric acid and deionized water is 1: (1~2):
(0.8~1), wherein deionized water and the volume of nitric acid are in terms of milliliter, and the quality of graphene oxide is in terms of milligram.
The mass ratio of the volume of deionized water in the step 3), the quality of sodium hydroxide and trithiocyanuric acid is 1:
(46~50): (70~72), wherein the volume of deionized water is in terms of milliliter, and the quality of sodium hydroxide and trithiocyanuric acid is with milligram
Meter.
Saturation KI-I in the step 4)2The volume ratio of deionized water is 1: 20 in solution and mixed liquor (3).The step
It is rapid 4) in dilute hydrochloric acid concentration be 0.1M.
The present invention also provides a kind of graphene oxide/iron oxide prepared by the above method/poly- trithiocyanuric acids
The layered porous adsorbent material of trisodium salt.
In addition, the present invention also provides a kind of graphene oxide/iron oxide/layered porous absorption of poly- trithiocyanuric acid trisodium salt
Application of the material in the reparation of heavy metal lead and cadmium pollution environment.
Obtained graphene oxide/iron oxide prepared by the present invention/layered porous absorption of poly- trithiocyanuric acid trisodium salt
The structure of material is layered porous compound as shown in Figure 1, composite shapes rule prepared by the present invention as seen from Figure 1
Material.
Compared with prior art, the beneficial effects of the present invention are:
(1) the method for the present invention takes full advantage of the characteristic of magnetic material, and magnet separation can be used, there is raw material to be easy to get, prepare letter
Single feature.Due to the bigger serface that it has, efficient heavy metal adsorption performance, in necks such as heavy metal-polluted water processing
Domain is with important application prospects.
(2) graphene oxide/iron oxide/layered porous adsorption material of poly- trithiocyanuric acid trisodium salt prepared in the present invention
Material, for the purification of the heavy metal Hgs such as water body, soil, lead and cadmium pollution environment, removal rate is reachable in middle low pollution environment
To 96% or more.
Detailed description of the invention
Fig. 1 is the scanning electricity of the layered porous adsorbent material sample of graphene oxide/iron oxide/poly- trithiocyanuric acid trisodium salt
Sub- microscope figure.
Specific embodiment
The present invention is further described below by way of specific embodiment, but those skilled in the art should be able to know, the implementation
Example does not limit the invention patent protection scope in any way.
A kind of graphene oxide/the iron oxide of embodiment 1/poly- trithiocyanuric acid trisodium salt layered porous adsorbent material system
Preparation Method
The preparation method specifically comprises the following steps:
1) by 375mg graphene oxide ultrasonic disperse into 300mL deionized water, dispersion liquid A is obtained;
2) it by the ferriferrous oxide nano-particle ultrasonic disperse of 300mg superparamagnetism 8nm into 600mL2M nitric acid solution, uses
Deionized water sufficiently wash after by it ultrasonic disperse obtains dispersion liquid B into 300mL deionized water again;By dispersion liquid A and dispersion
5min is mixed in liquid B, obtains suspension C;
3) 2300mg sodium hydroxide is dissolved in 50ml ionized water, 3500mg trithiocyanuric acid stirring and dissolving is added, obtains bright orange
Color clear solution D;Solution d is slowly dropped into above-mentioned suspension C under mechanical stirring, room temperature continues stirring 2h and obtains mixed liquor E;
4) under ice bath and mechanical stirring, 30mL saturation KI-I is added dropwise in Xiang Shangshu mixed liquor E2Solution, under condition of ice bath
Continue to be slowly increased to room temperature after stirring 2h, be stirred overnight;The hydrochloric acid solution stirring 20min of appropriate 0.1M is added in Magnetic Isolation.Magnetic
Property separation, and be washed with deionized 3 times, 40 DEG C of drying are cooled to room temperature to get graphene oxide/iron oxide/poly- three polysulfide
The layered porous adsorbent material of cyanic acid trisodium salt.
A kind of graphene oxide/the iron oxide of embodiment 2/poly- trithiocyanuric acid trisodium salt layered porous adsorbent material system
Preparation Method
The preparation method specifically comprises the following steps:
1) by 750mg graphene oxide ultrasonic disperse into 300mL deionized water, dispersion liquid A is obtained;
2) the r- ferric oxide nanoparticles ultrasonic disperse of 375mg superparamagnetism 12nm is made into 375mL2M nitric acid solution
By it, ultrasonic disperse obtains dispersion liquid B into 300mL deionized water again after sufficiently being washed with deionized water;By dispersion liquid A and divide
5min is mixed in dispersion liquid B, obtains suspension C;
3) 2500mg sodium hydroxide is dissolved in 50ml ionized water, 3600mg trithiocyanuric acid stirring and dissolving is added, obtains bright orange
Color clear solution D;Solution d is slowly dropped into above-mentioned suspension C under mechanical stirring, room temperature continues stirring 2h and obtains mixed liquor E;
4) under ice bath and mechanical stirring, 30mL saturation KI-I is added dropwise in Xiang Shangshu mixed liquor E2Solution, under condition of ice bath
Continue to be slowly increased to room temperature after stirring 2h, be stirred overnight;The hydrochloric acid solution stirring 20min of appropriate 0.1M is added in Magnetic Isolation.Magnetic
Property separation, and be washed with deionized 3 times, 40 DEG C of drying are cooled to room temperature to get graphene oxide/iron oxide/poly- three polysulfide
The layered porous adsorbent material of cyanic acid trisodium salt.
A kind of graphene oxide/the iron oxide of embodiment 3/poly- trithiocyanuric acid trisodium salt layered porous adsorbent material system
Preparation Method
The preparation method specifically comprises the following steps:
1) by 500mg graphene oxide ultrasonic disperse into 300mL deionized water, dispersion liquid A is obtained;
2) it by the ferriferrous oxide nano-particle ultrasonic disperse of 333mg superparamagnetism 10nm into 500mL2M nitric acid solution, uses
Deionized water sufficiently wash after by it ultrasonic disperse obtains dispersion liquid B into 300mL deionized water again;By dispersion liquid A and dispersion
5min is mixed in liquid B, obtains suspension C;
3) 2400mg sodium hydroxide is dissolved in 50ml ionized water, 3545mg trithiocyanuric acid stirring and dissolving is added, obtains bright orange
Color clear solution D;Solution d is slowly dropped into above-mentioned suspension C under mechanical stirring, room temperature continues stirring 2h and obtains mixed liquor E;
4) under ice bath and mechanical stirring, 30mL saturation KI-I is added dropwise in Xiang Shangshu mixed liquor E2Solution, under condition of ice bath
Continue to be slowly increased to room temperature after stirring 2h, be stirred overnight;The hydrochloric acid solution stirring 20min of appropriate 0.1M is added in Magnetic Isolation.Magnetic
Property separation, and be washed with deionized 3 times, 40 DEG C of drying are cooled to room temperature to get graphene oxide/iron oxide/poly- three polysulfide
The layered porous adsorbent material of cyanic acid trisodium salt.
Comparative example 1
In addition to the partial size of magnetic ferric oxide nano particles is 14nm, remaining preparation process is the same as embodiment 3.
Comparative example 2
In addition to the partial size of magnetic ferric oxide nano particles is 6nm, remaining preparation process is the same as embodiment 3.
The measuring physical properties of the composite material of the present invention of embodiment 4
1- of embodiment of the present invention embodiment 3, the shape of adsorbent material prepared by comparative example 1- comparative example 2 are measured respectively
Variance rate, the rate of recovery, expulsion rate.Wherein shape difference rate is the shape difference to form adsorbent material, using scanning electron microscopy
Mirror is measured.The rate of recovery is the percentage that the reasonable opinion of the weight of the adsorbent material actually obtained in step 3) obtains adsorbent material
Rate;Expulsion rate is expulsion rate after adsorbent material impregnates for 24 hours in 0.1M hydrochloric acid solution.The measurement result of each parameter is as shown in table 1.
The measuring physical properties result of the adsorbent material of the present invention of table 1
Graphene oxide/iron oxide prepared by the comparing embodiment 1- embodiment 3/layered porous suction of poly- trithiocyanuric acid trisodium salt
Enclosure material can be seen that when iron oxide, graphene oxide and poly- trithiocyanuric acid trisodium salt mass ratio be 1:1.5:10.6,
The performance of its physical property is more excellent.
Graphene oxide/iron oxide prepared by 1-3 of the embodiment of the present invention/layered porous suction of poly- trithiocyanuric acid trisodium salt
Enclosure material shape difference rate expulsion rate is low, and the rate of recovery is high, with conspicuousness compared with comparative example 1- comparative example 2
Difference, wherein it is the most excellent with the quality of adsorbent material prepared by embodiment 3, it is highly preferred embodiment of the present invention.Work as magnetic
Property ferric oxide nano particles partial size be 10nm, the mass ratio of iron oxide, graphene oxide and poly- trithiocyanuric acid trisodium salt is
The shape difference rate of 1:1.5:10.6, preparation-obtained composite material are minimum, rate of recovery highest, and expulsion rate is minimum.
Embodiment 5
It is with graphene oxide/iron oxide made from above-described embodiment 3/layered porous adsorbent material of poly- trithiocyanuric acid trisodium salt
Example carries out wastewater treatment adsorption test, wherein Pb in waste water2+And Cd2+The initial concentration of solution is 10mg/L, pH=5.5,
Adsorption temp is 30 DEG C, adsorption time 6h.It is contained in outer draining after adsorption treatment in embodiment 1 to 3 and comparative example 1 to 2
Ion concentration be shown in Table 2.
The ion concentration contained in outer draining after distinct methods adsorption treatment of table 2
Sample | Pb2+Residual concentration (mg/L) | Cd2+Residual concentration (mg/L) | Hg2+ Residual concentration (mg/L) |
Embodiment 1 is discharged | 0.28 | 0.03 | 0.02 |
Embodiment 2 is discharged | 0.32 | 0.03 | 0.02 |
Embodiment 3 is discharged | 0.21 | 0.02 | 0.01 |
Comparative example 1 is discharged | 0.45 | 0.06 | 0.09 |
Comparative example 2 is discharged | 0.42 | 0.05 | 0.06 |
Discharge standard | 0.5 | 0.05 | 0.03 |
Comparing embodiment 1-4 and comparative example 1-2 is it is found that the graphene oxide/oxidation prepared using the embodiment of the present application 1-4
Iron/layered porous adsorbent material of poly- trithiocyanuric acid trisodium salt can effectively remove heavy metal, purification removal rate up to 96% with
On, while treated that purified water can directly carry out outlet.It, can by contrast after the adsorbent material processing of embodiment 1-2 preparation
To effectively remove heavy metal ion, but it is not able to satisfy the discharge standard to cadmium and mercury.Above-mentioned removal effect comparative experiments proves, this
The layered porous adsorbent material large specific surface area of preparation is invented, adsorption capacity is strong, can efficiently remove lead, mercury, cadmium etc. in water removal
A variety of harmful heavy metals are suitble to the depths reason of sewage.
The above is only a preferred embodiment of the present invention, protection scope of the present invention is not limited merely to above-mentioned implementation
Example.All technical solutions belonged under thinking of the present invention all belong to the scope of protection of the present invention.It is noted that for the art
Those of ordinary skill for, improvements and modifications without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of graphene oxide/iron oxide/poly- trithiocyanuric acid trisodium salt layered porous adsorbent material preparation method, special
Sign is comprising following steps:
1) by graphene oxide ultrasonic disperse into deionized water, dispersion liquid A is obtained;
2) by Superparamagnetic Iron Oxide nanoparticle ultrasonic disperse into nitric acid solution, by it after sufficiently being washed using deionized water
Again ultrasonic disperse obtains dispersion liquid B into deionized water;5min is mixed in dispersion liquid A and dispersion liquid B, obtains suspension C;
3) sodium hydroxide is dissolved in deionized water, trithiocyanuric acid stirring and dissolving is added, obtains glassy yellow clear solution D;It is mechanical
Solution d is slowly dropped into above-mentioned suspension C under stirring, room temperature continues stirring 2h and obtains mixed liquor E;
4) under ice bath and mechanical stirring, saturation KI-I is added dropwise in Xiang Shangshu mixed liquor E2Rear ice bath item is added dropwise in solution
Continue to be slowly increased to room temperature after stirring 2h under part, be stirred overnight;It is successively washed 1 time using dilute hydrochloric acid after Magnetic Isolation and use is gone
Ion water washing 3 times, 40 DEG C of drying are cooled to room temperature to get graphene oxide/iron oxide/poly- trithiocyanuric acid trisodium salt deposit
Shape porous adsorbing material.
2. graphene oxide/iron oxide according to claim 1/layered porous the adsorbent material of poly- trithiocyanuric acid trisodium salt
Preparation method, it is characterised in that: the volume of the deionized water in the step 1) and the mass ratio of graphene oxide are 0.4
: 1~0.8: 1, wherein the volume of deionized water is in terms of milliliter, and the quality of graphene oxide is in terms of milligram.
3. graphene oxide/iron oxide according to claim 1/layered porous the adsorbent material of poly- trithiocyanuric acid trisodium salt
Preparation method, which is characterized in that magnetic ferric oxide nano particles in the step 2 are that ferroso-ferric oxide or r- tri- are aoxidized
One of two iron.
4. graphene oxide/iron oxide according to claim 1/layered porous the adsorbent material of poly- trithiocyanuric acid trisodium salt
Preparation method, which is characterized in that magnetic iron oxide partial size in the step 2 is 8-12nm, and the concentration of nitric acid is 2M.
5. graphene oxide/iron oxide according to claim 1/layered porous the adsorbent material of poly- trithiocyanuric acid trisodium salt
Preparation method, which is characterized in that the volume ratio of the quality of the iron oxide in the step 2, the volume of nitric acid and deionized water
Be 1: (1~2): (0.8~1), wherein deionized water and the volume of nitric acid are in terms of milliliter, and the quality of graphene oxide is with milligram
Meter.
6. graphene oxide/iron oxide according to claim 1/layered porous the adsorbent material of poly- trithiocyanuric acid trisodium salt
Preparation method, which is characterized in that the volume of the deionized water in the step 3), the quality of sodium hydroxide and trithiocyanuric acid
Mass ratio be 1: (46~50): (70~72), wherein the volume of deionized water is in terms of milliliter, sodium hydroxide and trithiocyanuric acid
Quality in terms of milligram.
7. graphene oxide/iron oxide according to claim 1/layered porous the adsorbent material of poly- trithiocyanuric acid trisodium salt
Preparation method, which is characterized in that the saturation KI-I in the step 4)2The volume ratio of deionized water in solution and mixed liquor E
It is 1: 21.7.
8. graphene oxide/iron oxide according to claim 1/layered porous the adsorbent material of poly- trithiocyanuric acid trisodium salt
Preparation method, which is characterized in that the concentration of the dilute hydrochloric acid in the step 4) be 0.1M.
9. a kind of graphene oxide/iron oxide being prepared according to any claim of claim 1-7/poly- three polysulfide
The layered porous adsorbent material of cyanic acid trisodium salt.
10. graphene oxide/iron oxide according to any one of claims 8/layered porous adsorbent material of poly- trithiocyanuric acid trisodium salt exists
Application in the reparation of heavy metal lead and cadmium pollution environment.
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CN113952941A (en) * | 2021-11-08 | 2022-01-21 | 江苏乐尔环境科技股份有限公司 | Preparation method of heavy metal chelating agent |
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