CN109012603A - Molybdic adsorbent and preparation method thereof in a kind of processing alkaline waste water - Google Patents

Molybdic adsorbent and preparation method thereof in a kind of processing alkaline waste water Download PDF

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Publication number
CN109012603A
CN109012603A CN201811249870.7A CN201811249870A CN109012603A CN 109012603 A CN109012603 A CN 109012603A CN 201811249870 A CN201811249870 A CN 201811249870A CN 109012603 A CN109012603 A CN 109012603A
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adsorbent
waste water
preparation
molybdic
alkaline waste
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孙国新
靳丽敏
陈文鑫
梁帅
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University of Jinan
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University of Jinan
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20Solid 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054Solid 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 surface properties or porosity
    • B01J20/28057Surface area, e.g. B.E.T specific surface area
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30Processes for preparing, regenerating, or reactivating
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/285Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Inorganic Chemistry (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The invention discloses a kind of adsorbents and preparation method thereof of sexavalence molybdenum (Mo (VI)) in processing alkaline waste water, belong to sewage treatment and field of environment protection.The structural formula of the adsorbent of Mo (VI) is N in the processing alkaline waste water4O6CXH2X+1Wherein 15≤X≤37-GO, and X is positive integer, synthesis graphene oxide (GO) first, and then carries out functionalization to it, obtains functional graphene oxide adsorbent.The obtained adsorbent large specific surface area, selectivity is good, and adsorption efficiency is high, is greater than 86% to the adsorption rate of Mo (VI) within the scope of pH=4-9.The advantages of preparation method of molybdic adsorbent has reaction temperature low in a kind of processing alkaline waste water of the present invention, and the time is short, and purification is simple, strong operability.

Description

Molybdic adsorbent and preparation method thereof in a kind of processing alkaline waste water
Technical field
The present invention relates to molybdic adsorbents in a kind of processing alkaline waste water and preparation method thereof to belong at trade effluent Range is managed, is generated specifically, being handled in industrial processes under alkaline condition using functional graphene oxide adsorbent Molybdenum waste water containing sexavalence, make up to country to the discharge standard of molybdenum requirement.
Background technique
With industrial boom, molybdate is widely applied to zinc-plated, buffing compound, alkaloid, ink, light-resistant pigment Deng manufacture production process, huge harm is caused to environmental balance and human health.Sodium molybdate belongs to low toxicity compounds.Molybdenum Poisoning can cause arthralgia, cause blood pressure relatively low and fluctuation of blood pressure, obstacle occurs in nerve dysfunction, metabolic process.Country Standard is 2mg/m, dust 4mg/m to soluble molybdenum compound aerosol maximum permissible concentration.China Jiangxi Dayu County tailing water Middle molybdenum content is excessively high, and the livestock of this area is once caused the symptom of molybdenosis occur.
The present invention uses graphene oxide for raw material, since graphene oxide itself is rich in hydroxyl, epoxy group, carboxyl, carbonyl The oxygen-containing functional groups such as base.To its functionalization, it is expected that being realized in neutral conditions to Mo (VI) selective cleaning effect.Therefore, The present invention will provide molybdic adsorbent and preparation method thereof in a kind of processing alkaline waste water.
Summary of the invention
It is almost non-adsorbable under neutral and alkaline condition to ask for adsorption effect is good in acid condition in the prior art Topic, it is described it is an object of the present invention to provide molybdic adsorbent in a kind of processing alkaline waste water and preparation method thereof The pH of adsorbent processed is applied widely, cheap, raw material is easy to get.
The two of goal of the invention are the provision of molybdic adsorbent and preparation method thereof in a kind of processing alkaline waste water.Institute Adsorbent large specific surface area, the size distribution for stating method preparation are uniform.
To achieve the above object, technical scheme is as follows:
Molybdic adsorbent in a kind of processing alkaline waste water: the structure of the adsorbent is N2CXH2X+1- GO, wherein 9≤X≤ 29, (X is positive integer).
The specific surface area of the adsorbent is 30m2/g-250m2/ g, single, the applicable pH range 2-9 of selectivity.
The preparation method of molybdic adsorbent, the method are as follows in a kind of processing alkaline waste water:
Step 1: modified Hummer method synthesizes GO;
Step 2: tetramethylmethane diamines and brominated alkanes react in a solvent obtains product I;
Step 3: the reaction was continued prepares functionalized reagent I by product I;
Functional graphene oxide is synthesized on GO Step 4: functionalized reagent I is loaded in a solvent;
Wherein, the brominated alkanes in step 2 are bromo pentane, bromo hexane, heptane bromide, bromooctane, bromo nonane, bromine For decane, bromododecane, bromotetradecane, bromohexadecane;
Wherein, reaction dissolvent is dimethylformamide, dimethyl acetamide, tetrahydrofuran, acetonitrile in step 2;
Used solvent is acetone, ethyl acetate, butyl acetate in step 4;
The quality of tetramethylmethane diamines is 1-2 g in step 2, and solvent volume is 3-6 mL, and brominated alkanes quality is 4-14 G, reaction temperature 55-85oC, reaction time are 10-24 h, and the EtOH-EtOAc purification for being 1:2-1:5 with volume ratio is more It is secondary to be recrystallized to give product I;
Product I is dissolved in ethyl acetate in step 3 and 3 mol/L NaOH solutions are reacted, deionized water is repeatedly washed to neutrality, It is further continued for the HNO with 4 mol/L3Reaction, deionized water are repeatedly washed to neutrality, and functionalized reagent I is obtained;
Functionalized reagent I mass is that 0.5-1g is dissolved in solvent in step 4, and GO mass is that 1-2 g disperses wherein, and reaction temperature is 15-45 oC, reaction time are 8-15 h;Centrifugation, washs, is dried to obtain functional graphene oxide adsorbent;
Beneficial effect
1, molybdic adsorbent is hybrid inorganic-organic materials in processing alkaline waste water of the present invention, at low cost, can be It is mass produced in practice;Structure and function admirable are to be greater than in 2-9 environment to the adsorption rate of Mo (VI) in pH range 86%;
2, molybdic adsorbent reactivation performance is good in processing alkaline waste water of the present invention, and desorption-regeneration cost is low, can follow Ring uses;
3, the preparation method of the present invention for handling sexavalence molybdenum adsorbent in alkaline waste water, has reaction temperature lower, reaction The advantages of time is shorter, and subsequent processes are simple and convenient, strong operability.
Detailed description of the invention
Fig. 1 is a kind of nucleus magnetic hydrogen spectrum figure for functionalized reagent I that embodiment 1 is prepared;
Fig. 2 is a kind of structure chart for functional graphene oxide adsorbent that embodiment 2 is prepared;
Fig. 3 is a kind of infrared spectrum for functional graphene oxide adsorbent that embodiment 2 is prepared.
Specific embodiment
Carry out the present invention is described in detail below by specific embodiment:
The final product of 1-9 of the embodiment of the present invention is detected by following apparatus and method: total through totally digitilized nuclear-magnetism Spectrometer (Advance III400 MHz) analyzing molecules structure of shaking and product purity;Use Fourier Transform Infrared Spectrometer (Vertex 70) is to adsorbent qualitative analysis;BET type specific-surface area detection instrument (M9-3H-2000BET-M) compares table to adsorbent Area estimation;It is measured with inductively coupled plasma atomic emission spectrometry (ICP-AES) and has adsorbed that supernatant is molybdic to be contained Amount.
Determination step of the final product of 1-5 of the embodiment of the present invention to sexavalence molybdenum adsorption rate: by 0.1 g functionalization graphene Adsorbent is placed in conical flask, is then added and is contained 0.2 g/L Mo (VI), and 10 mL of the solution of pH=8.0 is stirred at room temperature 30 min and reaches absorption Balance, centrifuging and taking supernatant, atomic absorption method survey Mo (VI) content, and according to formula(E It is adsorption rate, COIt is the initial concentration of Mo (VI), CeConcentration when being adsorption equilibrium) calculate adsorption rate.
Embodiment 1
1 g of quality of tetramethylmethane diamines, 5.5 g of quality of bromododecane, dimethylformamide make 3 mL of solvent, reaction Temperature 80oC, 12 h of reaction time;It is recrystallized to give product I three times with EtOH-EtOAc;Product I is dissolved in ethyl acetate With 20 mL, the reaction of 3mol/L NaOH solution, deionized water is repeatedly washed to neutrality;Continue and 20 mL, the HNO of 4mol/L3Instead It answers, deionized water is repeatedly washed to neutrality, and functionalized reagent I is obtained, and quality is 5.1 g;Desired structure is detected as through nuclear-magnetism (see attached drawing 1).
Embodiment 2
0.5 g functionalized reagent I is dissolved in acetone, the GO ultrasonic disperse of 1 g wherein, 25oC is stirred to react 10 h, and centrifugation is gone Ion water washing, 60oC be dried in vacuo 12 h obtain functional graphene oxide I adsorbent, through infrared detection load successfully (see Attached drawing 3), calculate to be shown in Table 1 greater than 86%(in adsorption rate of the pH=4-9 to Mo (VI) according to the method described above).
Embodiment 3
1 g of quality of tetramethylmethane diamines, 4.3 g of quality of heptane bromide, 4 mL acetonitrile as solvents, reaction temperature 75oC, 10 h of reaction time;It is recrystallized to give product II three times with EtOH-EtOAc;Product II is dissolved in ethyl acetate and 20 mL, The reaction of 3mol/L NaOH solution, deionized water are repeatedly washed to neutrality;Continue and 20 mL, the HNO of 4mol/L3Reaction, go from Sub- water is repeatedly washed to neutrality, obtains functionalized reagent II, and quality is 3.2 g;0.5 g functionalized reagent II is dissolved in acetone, The GO ultrasonic disperse of 1.0 g wherein, 30oC is stirred to react 12 h, centrifugation, deionized water washing, and 60oC is dried in vacuo 12 h and obtains To functional graphene oxide II adsorbent, calculate according to the method described above to the adsorption rate 87.2% of Mo (VI).
Embodiment 4
1 g of quality of tetramethylmethane diamines, 4.8 g of quality of bromo nonane, 4 mL dimethyl acetamides make solvent, reaction temperature Degree 65oC, 12 h of reaction time;It is recrystallized to give product III three times with EtOH-EtOAc;Product III is dissolved in acetic acid second Ester and 20 mL, the reaction of 3mol/L NaOH solution, deionized water are repeatedly washed to neutrality;Continue and 20 mL, the HNO of 4mol/L3 Reaction, deionized water are repeatedly washed to neutrality, and functionalized reagent II is obtained, and quality is 3.4 g;0.5 g functionalized reagent III is molten In in butyl acetate, the GO ultrasonic disperse of 1.0 g wherein, 28oC is stirred to react 10 h, centrifugation, deionized water washing, and 60oC is true Dry 12 h of sky obtain functional graphene oxide III adsorbent, calculate according to the method described above Mo (VI) adsorption rate 83.9%。
Embodiment 5
1 g of quality of tetramethylmethane diamines, 5.4 g of quality of bromodecane, 5 mL tetrahydrofurans make solvent, reaction temperature 70oC, 10 h of reaction time;It is recrystallized to give product IV three times with EtOH-EtOAc;Product IV is dissolved in ethyl acetate and 20 The reaction of mL, 3mol/L NaOH solution, deionized water are repeatedly washed to neutrality;Continue and 20 mL, the HNO of 4mol/L3Reaction, goes Ionized water is repeatedly washed to neutrality, obtains functionalized reagent IV, and quality is 3.4 g;0.5 g functionalized reagent III is dissolved in acetic acid In butyl ester, the GO ultrasonic disperse of 1.0 g wherein, 28oC is stirred to react 10 h, centrifugation, deionized water washing, and 60oC vacuum drying 12 h obtain functional graphene oxide IV adsorbent, calculate according to the method described above Mo (VI) adsorption rate 87.7%.
Embodiment 6
0.2 g/L, 10 mL containing Mo (VI) solution is taken, KCl, KNO of 0.2 g is added3、KCO3、K2SO4、K3PO4Adjust the pH of solution =6.5,0.1 g functional graphene oxide I adsorbent is added, is stirred at room temperature 30 minutes and reaches adsorption equilibrium, is centrifuged, takes supernatant Liquid surveys the content of Mo (VI) with atomic absorption method, calculates to obtain Mo (VI) adsorption rate 86.3%.
Embodiment 7
0.2 g/L, 10 mL containing Mo (VI) solution is taken, 0.3 ZnCl is added2、CoCl2、CuCl2、NiCl2、CdCl2、MgCl2It adjusts PH=6.9 of solution are added 0.1 g functional graphene oxide I adsorbent, are stirred at room temperature 30 minutes and reach adsorption equilibrium, from The heart takes supernatant atomic absorption method to survey the content of Mo (VI), calculates to obtain Mo (VI) adsorption rate 86.9%.

Claims (7)

1. molybdic adsorbent and preparation method thereof in a kind of processing alkaline waste water, which is characterized in that the knot of the adsorbent Structure is N4O6CXH2X+1- GO, wherein 15≤X≤37, (X is positive integer).
2. molybdic adsorbent and preparation method thereof in a kind of processing alkaline waste water according to claim 1, special Sign is: the specific surface area of adsorbent is 30m2/g-250m2/ g, single, the applicable pH range 2-9 of selectivity.
3. molybdic adsorbent and preparation method thereof in a kind of processing alkaline waste water according to claim 1, special Sign is: specific preparation process is as follows:
Step 1: modified Hummer method synthesizes GO;
Step 2: tetramethylmethane diamines and brominated alkanes react in a solvent obtains product 1;
Step 3: the reaction was continued prepares functionalized reagent for product 1;
Step 4: functionalized reagent to be loaded to synthesis functional graphene oxide adsorbent on GO in a solvent;
Wherein the brominated alkanes in step 2 are bromo pentane, bromo hexane, heptane bromide, bromooctane, bromo nonane, bromo One or more of decane, bromododecane, bromotetradecane, bromohexadecane;
Reaction dissolvent is one or more of dimethylformamide, dimethyl acetamide, tetrahydrofuran, acetonitrile in step 2;
Solvent for use is one or more of acetone, acetonitrile, ethyl acetate, butyl acetate in step 4.
4. molybdic adsorbent and preparation method thereof in a kind of processing alkaline waste water according to claim 3, special Sign is: the quality of tetramethylmethane diamines is 1-2 g in step 2, and solvent volume is 3-6 mL, and brominated alkanes quality is 4- 14 g, reaction temperature 55-85oC, reaction time are 10-24 h.
5. molybdic adsorbent and preparation method thereof in a kind of processing alkaline waste water according to claim 3, special Sign is: the EtOH-EtOAc repeated recrystallize that purification is 1:2-1:5 with volume ratio in step 2 obtains product I.
6. molybdic adsorbent and preparation method thereof in a kind of processing alkaline waste water according to claim 3, special Sign is: product I being dissolved in ethyl acetate in step 3 and 3mol/L NaOH solution is reacted, deionized water is repeatedly washed into Property, continue the HNO with 4 mol/L3Reaction, deionized water are repeatedly washed to neutrality, and functionalized reagent I is obtained.
7. molybdic adsorbent and preparation method thereof in a kind of processing alkaline waste water according to claim 3, special Sign is: functionalized reagent I mass is that 0.5-1g is dissolved in solvent in step 4, and GO mass is that 1-2 g disperses wherein, reaction temperature Degree is 15-45oC, reaction time are 8-15 h;Centrifugation, washs, is dried to obtain functional graphene oxide adsorbent.
CN201811249870.7A 2018-10-25 2018-10-25 Molybdic adsorbent and preparation method thereof in a kind of processing alkaline waste water Withdrawn CN109012603A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111644162A (en) * 2020-06-18 2020-09-11 济南大学 Adsorbent for treating hexavalent molybdenum in alkaline wastewater
CN111790359A (en) * 2020-06-18 2020-10-20 济南大学 Adsorbent for treating hexavalent chromium in wastewater

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111644162A (en) * 2020-06-18 2020-09-11 济南大学 Adsorbent for treating hexavalent molybdenum in alkaline wastewater
CN111790359A (en) * 2020-06-18 2020-10-20 济南大学 Adsorbent for treating hexavalent chromium in wastewater

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Application publication date: 20181218