CN110523386A - Diethylenetriamine modified magnetic carbon nucleocapsid adsorbent and preparation method thereof and the application in absorption trivalent chromic ion and acid dyes - Google Patents
Diethylenetriamine modified magnetic carbon nucleocapsid adsorbent and preparation method thereof and the application in absorption trivalent chromic ion and acid dyes Download PDFInfo
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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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- 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
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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
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Abstract
The present invention provides a kind of diethylenetriamine modified magnetic carbon nucleocapsid adsorbent and preparation method thereof and the application in absorption trivalent chromic ion and acid dyes, make carbon source and source of iron using ferrocene, and ferroso-ferric oxide magnetic core is generated under the action of oxidant by hydro-thermal method and is coated by agraphitic carbon, to synthesize the magnetic carbon core-shell material of high-specific surface area and abundant oxygen-containing functional group.Material is with high-specific surface area and has abundant surface-active, and by N, N'- diisopropylcarbodiimide promotes diethylenetriamine and the amide of material surface oxygen-containing group to react, and completes diethylenetriamine surface functionalization.It recycles amino group and Cr (III) that complexation reaction occurs and chemisorption occurs with acid dyes, thus the common removal to Cr in aqueous solution (III) and acidic organic dye.
Description
Technical field
The invention belongs to the purification techniques fields of heavy metal in water and organic dyestuff, are related to a kind of modified magnetic of diethylenetriamine
Property carbon nucleocapsid adsorbent and preparation method thereof the and application in absorption trivalent chromic ion and acid dyes.
Background technique
As the recovery and the mankind of global economy sharply increase industrial requirement, heavy metal pollution problem is got worse.
Heavy metal pollution causes to seriously threaten to environment and the mankind.Pollution of chromium is one of heavy metal pollution of most serious, and is answered extensively
For in the industrial productions such as leather, dyestuff, plating, ceramics.
Chromium is existed in the environment with two kinds of valence states of trivalent (Cr (III)) and sexavalence (Cr (VI)).Cr (III) toxicity is smaller, but
Excessive Cr (III) can be oxidized to the stronger Cr of toxicity (VI).The discharge of Cr (III) is adjoint in the industry such as leather, dyestuff
The acidic organic dye of high concentration, the synergy of Cr (III) and acidic organic dye make it be more difficult to remove from water body, and
And human body is entered by food chain, cause cancer, genetic mutation and death.Therefore, efficiently, conveniently, safely there is an urgent need to one
Method eliminate Cr (III) and acidic organic dye in waste water jointly.
Nowadays remove waste water in Cr (III) method include liquid-phase extraction, ion exchange, chemical precipitation, electrochemical reduction and
Absorption.Absorption is a kind of more convenient, simple, efficiently, economic, environmentally friendly method, for removing Cr (III) from solution.Traditional
Adsorbent such as active carbon is expensive, and adsorption process efficiency is lower.Chelating agent and fiber are ground as adsorbent
Study carefully, this adsorbent has high-affinity to metal target.These researchs are without discussing that acidic organic dye is to absorption in waste water
Influence and common removal to acidic organic dye.Therefore, exploitation has jointly organic to Cr (III) and acidity in water body
The new adsorbent of dye efficient removal has been a great concern.
Further, since the difference of adsorbent surface structure and functional group, base material is difficult by organic functional, and difficult
To separate in the liquid phase.
Summary of the invention
The purpose of the present invention is to provide a kind of diethylenetriamine modified magnetic carbon nucleocapsid adsorbent and preparation method thereof and
Application in absorption trivalent chromic ion and acid dyes, gained diethylenetriamine modified magnetic carbon nucleocapsid adsorbent may be implemented
To the eutectoid content of trivalent chromic ion and acidic organic dye in water, there is good environment and economic benefit.
The present invention is to be achieved through the following technical solutions:
The preparation method of diethylenetriamine modified magnetic carbon nucleocapsid adsorbent, comprising the following steps:
1) preparation of magnetic carbon core-shell material: use ferrocene as source of iron and carbon source, hydrogen peroxide is as oxidant, third
Under ketone environment, magnetic carbon core-shell material is made in hydro-thermal reaction；
2) preparation of diethylenetriamine modified magnetic carbon nucleocapsid adsorbent: by magnetic carbon core-shell material ultrasonic disperse in diethyl
In alkene triamine, and N is added, N'- diisopropylcarbodiimide, heating stirring reaction, reaction product washing, drying obtain diethyl
Alkene triamine modified magnetic carbon nucleocapsid adsorbent.
Preferably, in step 1), hydrothermal temperature is 200 DEG C~240 DEG C, and the time is 36~60h.
Preferably, in step 2), reaction temperature is 100~140 DEG C, and the time is 6~18h.
Preferably, in step 1), the mass ratio of ferrocene and hydrogen peroxide is 1:(1.25-2)；In step 2), magnetic carbon
Core-shell material, diethylenetriamine and N, the mass ratio of N'- diisopropylcarbodiimide are 3:(380~95): 8.
The diethylenetriamine modified magnetic carbon nucleocapsid adsorbent obtained using the preparation method.
Diethylenetriamine modified magnetic carbon nucleocapsid adsorbent trivalent chromic ion and acidity in eutectoid content water body has
Application in engine dyeing material.
Preferably, method are as follows: diethylenetriamine modified magnetic carbon nucleocapsid adsorbent is added in the water body to be purified and carries out
Absorption collects diethylenetriamine modified magnetic carbon nucleocapsid adsorbent after the completion of absorption.
Preferably, adsorption time is 5min~8h.
Preferably, the diethylenetriamine modified magnetic carbon nucleocapsid adsorbent of collection is with the mixed aqueous solution of HCl and thiocarbamide
Desorbing agent is desorbed, and the diethylenetriamine modified magnetic carbon nucleocapsid sorbent circulation after desorption utilizes.
Compared with prior art, the invention has the following beneficial technical effects:
The present invention makees carbon source and source of iron using ferrocene, and four oxidations are generated under the action of oxidant by hydro-thermal method
Three ferromagnetic cores are simultaneously coated by agraphitic carbon, to synthesize the magnetic carbon nucleocapsid material of high-specific surface area and abundant oxygen-containing functional group
Material.Material is with high-specific surface area and has abundant surface-active, and by N, N'- diisopropylcarbodiimide promotes divinyl three
Amine is reacted with the amide of material surface oxygen-containing group, completes diethylenetriamine surface functionalization.Recycle amino group and Cr
(III) complexation reaction occurs and chemisorption occurs with acid dyes, thus to Cr in aqueous solution (III) and acidic organic dye
Common removal.
Magnetic carbon core-shell material prepared by the present invention has the characteristics that many that specific surface area is larger, surface have enrich it is oxygen-containing
Group, it is easily separated in water body, it can pass through and apply external magnetic field quick separating；Can simultaneously in water body quick adsorption Cr (III)
And acidic organic dye.Therefore, diethylenetriamine modified magnetic carbon nucleocapsid adsorbent is a kind of novel suction with application prospect
Attached dose,
Diethylenetriamine modified magnetic carbon nucleocapsid adsorbent prepared by the present invention can be used for the absorption Cr in eutectoid content water body
(III) and acidic organic dye, easy to operate, removal effect is significant.
Further, adsorbent is renewable, and adsorbent under thiocarbamide and the strong complexing of hydrochloric acid mixed solution strong acid through being desorbed
It can be recycled after regeneration, there is good economy and environmental benefit.
Detailed description of the invention
Fig. 1 is (a) Fe3O4@C and (b) Fe3O4@C@DETA Electronic Speculum surface sweeping figure.
Fig. 2 is (a) Fe3O4@C and (b) Fe3O4@C@DETA infrared spectrogram.
Specific embodiment
Below with reference to specific embodiment, the present invention is described in further detail, it is described be explanation of the invention and
It is not to limit.
The preparation method of diethylenetriamine modified magnetic carbon nucleocapsid adsorbent of the present invention, comprising the following steps:
1) preparation of magnetic carbon core-shell material: use ferrocene as source of iron and carbon source, hydrogen peroxide is as oxidant, third
Under ketone environment, magnetic carbon core-shell material (Fe is made in hydro-thermal reaction3O4@C)；
2) diethylenetriamine modified magnetic carbon nucleocapsid adsorbent: by magnetic carbon core-shell material ultrasonic disperse in diethylenetriamine
In, and N is added, and N'- diisopropylcarbodiimide, then heating stirring is reacted, and is washed after reaction product is cooling, and it is dry, it obtains
Diethylenetriamine modified magnetic carbon nucleocapsid adsorbent (Fe3O4@C@DETA)；
It is organic to trivalent chromic ion in water body and acidity using the diethylenetriamine modified magnetic carbon nucleocapsid adsorbent of preparation
The method of dyestuff eutectoid content: the diethylenetriamine modified magnetic carbon nucleocapsid of 0.0004 times of its quality is added in the water body to be purified
Adsorbent (Fe3O4@C@DETA), under conditions of 25 DEG C, pH=3 in adsorbed water body concentration be respectively 2.5~50mg/L and 20~
Trivalent chromic ion and acidic organic dye (Acid Light Yellow G) organic dyestuff of 160mg/L, adsorption time are 5min~8h, then
Diethylenetriamine modified magnetic carbon nucleocapsid adsorbent (Fe is collected by external magnetic field3O4@C@DETA)。
Below with reference to the inspection of specific embodiment and trivalent chromic ion and acidic organic dye (Acid Light Yellow G) removal effect
The present invention is described in further detail for survey, described to be the explanation to invention rather than limit.
Preparation example 1
1) by 3.23mmol ferrocene ultrasonic dissolution in acetone, and 3mL hydrogenperoxide steam generator is added, above-mentioned mixing is molten
Liquid is cooled to room temperature after reaction in 210 DEG C of hydro-thermal reaction 48h, and cleaning is dried in vacuo afterwards for several times, obtains magnetic carbon nucleocapsid material
Material.
2) by 0.6g magnetic carbon core-shell material ultrasonic disperse in 40mL diethylenetriamine solution, and the N of 2mL, N'- is added
Above-mentioned solution is placed on the heating stirring 12h in 120 DEG C of oil baths, finally by the solution after reaction by diisopropylcarbodiimide
Cooling and Magneto separate is placed, is dried after cleaning, obtains diethylenetriamine modified magnetic carbon nucleocapsid adsorbent (Fe3O4@C@DETA)。
Fig. 1 shows that preparation example 1 forms the uniform-dimension nanosphere with rough surface.Surface before modified after pattern without bright
Significant difference is different, illustrates Fe3O4It is not influenced by DETA grafting in@C-shaped looks.
Two samples are in 584cm in Fig. 2-1The band at place is due to caused by the iron oxygen vibration of magnetic iron ore phase.Fe3O4@C@
DETA is in 3435cm-1The Fe at place3O4@C band is by 3409cm-1Replaced the strong band at place, this may be due to-OH and-NH2Group
Junction belt.Therefore, the variation of FT-IR spectrum confirms DETA by successfully modification to Fe3O4On@C.
Preparation example 2
1) by 3.23mmol ferrocene ultrasonic dissolution in acetone, and 2.5mL hydrogenperoxide steam generator is added, by above-mentioned mixing
Solution is cooled to room temperature after reaction in 200 DEG C of hydro-thermal reaction 60h, and cleaning is dried in vacuo afterwards for several times, obtains magnetic carbon nucleocapsid
Material.
2) by 0.6g magnetic carbon core-shell material ultrasonic disperse in 80mL diethylenetriamine solution, and the N of 2mL, N'- is added
Above-mentioned solution is placed on the heating stirring 18h in 100 DEG C of oil baths, finally by the solution after reaction by diisopropylcarbodiimide
Cooling and Magneto separate is placed, is dried after cleaning, obtains diethylenetriamine modified magnetic carbon nucleocapsid adsorbent (Fe3O4@C@DETA)。
Preparation example 3
1) by 3.23mmol ferrocene ultrasonic dissolution in acetone, and 3.2mL hydrogenperoxide steam generator is added, it will be above-mentioned mixed
Solution is closed in 220 DEG C of hydro-thermal reaction 55h, is cooled to room temperature after reaction, cleaning is dried in vacuo afterwards for several times, obtains magnetic carbon core
Shell material.
2) by 0.6g magnetic carbon core-shell material ultrasonic disperse in 60mL diethylenetriamine solution, and the N of 2mL, N'- is added
Above-mentioned solution is placed on the heating stirring 10h in 130 DEG C of oil baths, finally by the solution after reaction by diisopropylcarbodiimide
Cooling and Magneto separate is placed, is dried after cleaning, obtains diethylenetriamine modified magnetic carbon nucleocapsid adsorbent (Fe3O4@C@DETA)。
Preparation example 4
1) by 3.23mmol ferrocene ultrasonic dissolution in acetone, and 4mL hydrogenperoxide steam generator is added, above-mentioned mixing is molten
Liquid is cooled to room temperature after reaction in 240 DEG C of hydro-thermal reaction 36h, and cleaning is dried in vacuo afterwards for several times, obtains magnetic carbon nucleocapsid material
Material.
2) by 0.6g magnetic carbon core-shell material ultrasonic disperse in 20mL diethylenetriamine solution, and the N of 2mL, N'- is added
Above-mentioned solution is placed on the heating stirring 6h in 140 DEG C of oil baths, finally puts the solution after reaction by diisopropylcarbodiimide
Cooling and Magneto separate is set, is dried after cleaning, obtains diethylenetriamine modified magnetic carbon nucleocapsid adsorbent (Fe3O4@C@DETA)。
Adsorb example 1
With the Fe prepared in preparation example 13O4@C@DETA adsorbent carries out adsorption test to trivalent chromic ion waste water.Wherein,
The mass ratio of adsorbent and sewage is 0.0004:1, and trivalent chromic ion initial concentration is 10mg/L, and temperature is 25 DEG C, adsorption time
For 6h.Trivalent chromic ion saturated extent of adsorption is 23.59mg/g.
Adsorb example 2
With preparation example 1, trivalent chromic ion initial concentration is 20mg/L, and other conditions are constant, and the trivalent chromic ion measured is full
It is 37.07mg/g with adsorbance.
Preparation example 3
With preparation example 1, trivalent chromic ion initial concentration is 30mg/L, and other conditions are constant, and the trivalent chromic ion measured is full
It is 40.13mg/g with adsorbance.
Preparation example 4
With preparation example 1, trivalent chromic ion initial concentration is 50mg/g, and other conditions are constant, and the trivalent chromic ion measured is full
It is 45.63mg/g with adsorbance.
As it can be seen that within the scope of a certain concentration, suction of the diethylenetriamine modified magnetic carbon nucleocapsid adsorbent to trivalent chromic ion
Attached amount is improved with the raising of trivalent chromic ion concentration in water body.
Preparation example 5
With preparation example 3, adsorbent is magnetic carbon core-shell material, and other conditions are constant, and the trivalent chromic ion saturation measured is inhaled
Attached amount is 4.68mg/g.
As it can be seen that through the modified magnetic carbon nucleocapsid adsorbent of diethylenetriamine compared to magnetic carbon core-shell material to trivalent chromium from
The adsorbance of son is significantly improved.
Preparation example 6
With preparation example 4, adsorption time 5min, other conditions are constant, and the saturated extent of adsorption for measuring trivalent chromic ion is
24.68mg/g。
Preparation example 7
With preparation example 4, adsorption time 60min, other conditions are constant, and the saturated extent of adsorption for measuring trivalent chromic ion is
38.98mg/g。
Preparation example 8
With preparation example 4, adsorption time 240min, other conditions are constant, and the saturated extent of adsorption for measuring trivalent chromic ion is
40.20mg/g。
Preparation example 9
With preparation example 4, adsorption time 480min, other conditions are constant, and the saturated extent of adsorption for measuring trivalent chromic ion is
45.35mg/g。
As it can be seen that adsorption time is longer, and diethylenetriamine modified magnetic carbon nucleocapsid adsorbent is to trivalent before absorption reaches balance
The adsorbance of chromium ion is higher.
Preparation example 10
With preparation example 2, carried out in the condition that acid dyes (Acid Light Yellow G) concentration is 20mg/L in water, other conditions
Constant, the saturated extent of adsorption for measuring trivalent chromic ion is 35.68mg/g, while being 49.85mg/ to the adsorbance of Acid Light Yellow G
g。
Preparation example 11
With preparation example 2, carried out in the condition that acid dyes (Acid Light Yellow G) concentration is 80mg/L in water, other conditions
Constant, the saturated extent of adsorption for measuring trivalent chromic ion is 34.25mg/g, while being 189.84mg/ to the adsorbance of Acid Light Yellow G
g。
Preparation example 12
With preparation example 2, carried out in the condition that acid dyes (Acid Light Yellow G) concentration is 120mg/L in water, other conditions
Constant, the saturated extent of adsorption for measuring trivalent chromic ion is 36.25mg/g, while being 277.19mg/ to the adsorbance of Acid Light Yellow G
g。
Preparation example 13
With preparation example 2, carried out in the condition that acid dyes (Acid Light Yellow G) concentration is 160mg/L in water, other conditions
Constant, the saturated extent of adsorption for measuring trivalent chromic ion is 35.90mg/g, while being 349.83mg/ to the adsorbance of Acid Light Yellow G
g。
As it can be seen that diethylenetriamine modified magnetic carbon nucleocapsid adsorbent is to the adsorbance of trivalent chromic ion not by acid dyes
It influences, acidic organic dye (Acid Light Yellow G) is efficiently removed while removing trivalent chromic ion.
Preparation example 14
With preparation example 4, after adsorption equilibrium, diethylenetriamine modified magnetic carbon nucleocapsid adsorbent is collected with HCl and thiocarbamide
Mixed solution is that desorbing agent is desorbed, 25 DEG C of constant temperature oscillations, desorption mixed solution and diethylenetriamine modified magnetic carbon nucleocapsid
The mass ratio of adsorbent is 1500:1, and (desorption and regeneration rate is this absorption trivalent chromium of adsorbent to measurement first time desorption and regeneration rate
Mass of ion and the trivalent chromic ion mass ratio adsorbed for the first time) it is 85.96%.Adsorbent cleans number with deionized water after desorption
It is secondary, until pH is neutrality, adsorption experiment is carried out again, experiment condition is the same as embodiment 5.Circulation carries out adsorption and desorption regeneration tests, then
After four times raw, desorption and regeneration rate is 79.89%, and is tended towards stability.
As it can be seen that diethylenetriamine modified magnetic carbon nucleocapsid adsorbent is after four regeneration, adsorbance is held essentially constant, table
Bright absorption property is stablized, and can be recycled.
The invention discloses a kind of to remove complicated water using diethylenetriamine modified magnetic carbon nucleocapsid adsorbent and using it
The method of trivalent chromic ion in environment.Using diethylenetriamine modified magnetic carbon nucleocapsid adsorbent as adsorbent, remove in water body
Trivalent chromic ion.The method is specifically includes the following steps: (1) synthesizing magnetic carbon core-shell material；(2) diethylenetriamine changes
The preparation of property magnetic carbon nucleocapsid adsorbent；(3) using diethylenetriamine modified magnetic carbon nucleocapsid adsorbent as adsorbent, in water body
Trivalent chromic ion and acidic organic dye (Acid Light Yellow G) adsorbed jointly.Diethylenetriamine modified magnetic carbon nucleocapsid is inhaled
Attached dose significant to the adsorption effect of trivalent chromic ion in water environment, and can synchronize acidic organic dye in water removal.This hair
Bright easy to operate, material is easy to get, low in cost, obvious processing effect.
Claims (9)
1. the preparation method of diethylenetriamine modified magnetic carbon nucleocapsid adsorbent, which comprises the following steps:
1) preparation of magnetic carbon core-shell material: use ferrocene as source of iron and carbon source, hydrogen peroxide is as oxidant, in acetone ring
Under border, magnetic carbon core-shell material is made in hydro-thermal reaction；
2) preparation of diethylenetriamine modified magnetic carbon nucleocapsid adsorbent: by magnetic carbon core-shell material ultrasonic disperse in divinyl three
In amine, and N is added, N'- diisopropylcarbodiimide, heating stirring reaction, reaction product washing, drying obtain divinyl three
Amine modified magnetic carbon nucleocapsid adsorbent.
2. the preparation method of diethylenetriamine modified magnetic carbon nucleocapsid adsorbent according to claim 1, which is characterized in that
In step 1), hydrothermal temperature is 200 DEG C~240 DEG C, and the time is 36~60h.
3. the preparation method of diethylenetriamine modified magnetic carbon nucleocapsid adsorbent according to claim 1, which is characterized in that
In step 2), reaction temperature is 100~140 DEG C, and the time is 6~18h.
4. the preparation method of diethylenetriamine modified magnetic carbon nucleocapsid adsorbent according to claim 1, which is characterized in that
In step 1), the mass ratio of ferrocene and hydrogen peroxide is 1:(1.25-2)；In step 2), magnetic carbon core-shell material, divinyl
Triamine and N, the mass ratio of N'- diisopropylcarbodiimide are 3:(380~95): 8.
5. the diethylenetriamine modified magnetic carbon nucleocapsid absorption obtained using the described in any item preparation methods of claim 1-4
Agent.
6. diethylenetriamine modified magnetic carbon nucleocapsid adsorbent described in claim 5 in eutectoid content water body trivalent chromic ion and
Application in acidic organic dye.
7. application according to claim 6, which is characterized in that method are as follows: divinyl three is added in the water body to be purified
Amine modified magnetic carbon nucleocapsid adsorbent is adsorbed, and diethylenetriamine modified magnetic carbon nucleocapsid adsorbent is collected after the completion of absorption.
8. application according to claim 7, which is characterized in that adsorption time is 5min~8h.
9. application according to claim 7, which is characterized in that the diethylenetriamine modified magnetic carbon nucleocapsid adsorbent of collection
It is desorbed using the mixed aqueous solution of HCl and thiocarbamide as desorbing agent, the diethylenetriamine modified magnetic carbon nucleocapsid absorption after desorption
Agent recycles.
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