CN108854956A - A kind of preparation method for adsorbing antibiotic catalyst - Google Patents

A kind of preparation method for adsorbing antibiotic catalyst Download PDF

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Publication number
CN108854956A
CN108854956A CN201810658780.7A CN201810658780A CN108854956A CN 108854956 A CN108854956 A CN 108854956A CN 201810658780 A CN201810658780 A CN 201810658780A CN 108854956 A CN108854956 A CN 108854956A
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China
Prior art keywords
catalyst
antibiotic
water
preparation
added
Prior art date
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CN201810658780.7A
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Chinese (zh)
Inventor
陈哲
陈�峰
赵鹤鹏
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Jilin Institute of Chemical Technology
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Jilin Institute of Chemical Technology
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Priority to CN201810658780.7A priority Critical patent/CN108854956A/en
Publication of CN108854956A publication Critical patent/CN108854956A/en
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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
    • B01J20/0203Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0218Compounds of Cr, Mo, W
    • 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
    • B01J20/0203Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0274Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
    • B01J20/0285Sulfides of compounds other than those provided for in B01J20/045
    • 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
    • B01J20/06Solid 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
    • 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
    • B01J20/205Carbon nanostructures, e.g. nanotubes, nanohorns, nanocones, nanoballs
    • 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
    • C02F1/281Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • 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
    • C02F1/288Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Hydrology & Water Resources (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Nanotechnology (AREA)
  • Catalysts (AREA)

Abstract

The invention discloses one kind to have absorption antibiotic catalyst method, while having recyclability.Specifically include following steps:Graphene, sodium molybdate, L-cysteine are dissolved in water, the Fe prepared in advance is added after stirring and dissolving into mixed solution3O4Mixed system is finally transferred in water heating kettle and reacts by powder, ultrasonic disperse, and after reaction, resulting product is roasted at high temperature after washing and drying and obtain flower pattern MoS by product centrifuge separation2/Fe3O4/ rGO composite catalyst.Compared with prior art, the method for the present invention, equipment are simple, low in cost, non-environmental-pollution.Resulting magnetic composite shows excellent absorption property and solves the problems, such as that catalyst recycling is difficult, can be widely applied to organic wastewater processing, with good application prospect.

Description

A kind of preparation method for adsorbing antibiotic catalyst
Technical field
The invention belongs to the preparation methods of catalyst material, belong to environmental catalysis and water pollution processing technology field.
Background technique
Since antibiotic is found so far, antibiotic is just liked by our mankind.It cures the disease as civilized society good Medicine.But as we depend on antibiotic unduly, cause all very can easily detect in rivers,lakes and seas all over the world The residual of antibiotic.This to we can the health of the mankind there are also ecological environments all to cause imprint.Tolerance Increasing significantly to pathogenic bacteria and drug resistant gene the antibiotic being simply due in water can be in water environment, thus the ecological balance Threat is received with human health.So the antibiotic in water removal how to be gone to have become for a horse back problem to be solved.Its Middle absorption method is due to various advantages such as easy to operate, inexpensive, high efficiency, the risk generated without highly toxic by-product It is widely paid close attention to, so the research and development with high-efficiency and economic adsorbent as adsorption technology key just seem and its again It wants.
Summary of the invention
It is compound it is an object of the invention to prepare the MoS2/Fe3O4/rGO of the monodisperse flower type structure with recuperability Material.
Technical scheme is as follows:
Firstly, spare with the graphene of 30ml ultrapure water ultrasound 0.25mg/ml.The amount that wherein graphene is added shares 6 kinds, point For:Graphene plus 0.5ml plus 1ml plus 2ml plus 3ml plus 4ml is not added.Then, with 10ml ultrapure water stirring and dissolving 0.121g L-cysteine [HSCH2CH (NH2) CO2H analysis pure] be denoted as " (1) ", with the two of 10ml ultrapure water stirring and dissolving 0.121g Water sodium molybdate(Na2Mo4·2H2O)" (2) " are denoted as, 2) will be added in (1) gradually, continue stirring 30 minutes.By first step ultrasound The graphene of 0.25mg/ml be added in the mixed solution of (1) and (2), ultrasonic 30 minutes.Solution after above-mentioned ultrasonic disperse The Fe3O4 of 2mL (10mg/L) is added.Continue ultrasound 30 minutes.Finally, it is dry to be put into air blast for prepared solution reaction cartridge kettle Dry case, temperature 180oC, the time is for 24 hours.It carries out centrifugal water after taking-up to wash, alcohol, which is washed respectively alternately to clean to be dissolved in dehydrated alcohol three times, to dry in the air It is dry, it is spare to be packed into drug bottle.
Detailed description of the invention:
Fig. 1 MoS2/Fe3O4/rGO scanning electron microscope (SEM) photograph.
Fig. 2 .MoS2/Fe3O4/rGO adsorbs antibiotic properties figure
Specific embodiment:Technical solution of the present invention and effect are further described below with reference to embodiment.But made Specific method, formula and explanation are not limitation of the present invention.
The L-cysteine [HSCH2CH (NH2) CO2H analysis pure] of 0.121g, which is denoted as " (1) " and is dissolved in 10mL water, to be stirred It mixes;Simultaneously by the Sodium Molybdate Dihydrate of 0.121g(Na2Mo4·2H2O)Stirring in 10mL water is dissolved in be denoted as " (2) ", it will(2)Add Enter in (1), continues stirring 30 minutes.The graphene of the 0.25mg/ml of first step ultrasound is added to the mixed solution of (1) and (2) In, ultrasound 30 minutes.The Fe3O4 of 2mL (10mg/L) is added in solution after above-mentioned ultrasonic disperse.Continue ultrasound 30 minutes.Most Afterwards, by prepared solution reaction cartridge kettle, it is put into air dry oven, temperature 180oC, the time is for 24 hours.Centrifugal water is carried out after taking-up It washes, alcohol, which is washed respectively alternately to clean to be dissolved in dehydrated alcohol three times, to be dried, and it is spare to be packed into drug bottle.
Case study on implementation 2:
RGO additional amount in case study on implementation 1 is increased into 4ml from 0, other experiment conditions reach maximal absorptive capacity with embodiment 1 The rGO being added is 2ml(0.25mg/L).

Claims (5)

1. synthesizing a kind of with the preparation method that can adsorb antibiotic catalysis material.
2. method for preparing catalyst according to claim 1, feature is being with recuperability.
3. method for preparing catalyst according to claim 1, feature is being that graphene, optimised quantity 2mL is added (0.25mg/L).
4. method for preparing catalyst according to claim 1, it is characterized in that the adsorption rate of quadracycline is 97.6%.
5. according to claim 1 have MoS2/Fe3O4The preparation method of/rGO catalyst, obtained catalyst are ruler Very little uniform bouquet, it is a diameter of between 1-1.5 μm.
CN201810658780.7A 2018-06-25 2018-06-25 A kind of preparation method for adsorbing antibiotic catalyst Pending CN108854956A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201810658780.7A CN108854956A (en) 2018-06-25 2018-06-25 A kind of preparation method for adsorbing antibiotic catalyst

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201810658780.7A CN108854956A (en) 2018-06-25 2018-06-25 A kind of preparation method for adsorbing antibiotic catalyst

Publications (1)

Publication Number Publication Date
CN108854956A true CN108854956A (en) 2018-11-23

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110228838A (en) * 2019-06-19 2019-09-13 南开大学 A kind of RGO/MoS2/Ce0.75Zr0.25O2Cathode material and its preparation method and application

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106378096A (en) * 2016-11-21 2017-02-08 南京医科大学 Preparation method and application of graphene-molybdenum disulfide composite material
CN107064040A (en) * 2017-06-23 2017-08-18 江苏省环境科学研究院 The efficiently concentrating and separation method of traces of antibiotic in water environment

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106378096A (en) * 2016-11-21 2017-02-08 南京医科大学 Preparation method and application of graphene-molybdenum disulfide composite material
CN107064040A (en) * 2017-06-23 2017-08-18 江苏省环境科学研究院 The efficiently concentrating and separation method of traces of antibiotic in water environment

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
JAGDEES PRASAD ET AL: "Synthesis of MoS2-Reduced Graphene Oxide/Fe3O4 Nanocomposite for Enhanced Electromagnetic Interference Shielding Effectiveness", 《MATERIALS RESEARCH EXPRESS》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110228838A (en) * 2019-06-19 2019-09-13 南开大学 A kind of RGO/MoS2/Ce0.75Zr0.25O2Cathode material and its preparation method and application

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