CN105944702A - Preparation method of hierarchical porous carbon material for adsorption of tetracycline antibiotics - Google Patents

Preparation method of hierarchical porous carbon material for adsorption of tetracycline antibiotics Download PDF

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CN105944702A
CN105944702A CN201610299434.5A CN201610299434A CN105944702A CN 105944702 A CN105944702 A CN 105944702A CN 201610299434 A CN201610299434 A CN 201610299434A CN 105944702 A CN105944702 A CN 105944702A
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porous carbon
preparation
stage porous
absorption
wicker
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何劲松
戴江栋
闫永胜
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Jiangsu University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • 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
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • 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
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid 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
    • B01J20/28057—Surface area, e.g. B.E.T specific surface area
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • 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
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid 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
    • B01J20/28057—Surface area, e.g. B.E.T specific surface area
    • B01J20/28066—Surface area, e.g. B.E.T specific surface area being more than 1000 m2/g
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • 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
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid 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
    • B01J20/28069—Pore volume, e.g. total pore volume, mesopore volume, micropore volume
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • 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
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid 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
    • B01J20/28069—Pore volume, e.g. total pore volume, mesopore volume, micropore volume
    • B01J20/28076—Pore volume, e.g. total pore volume, mesopore volume, micropore volume being more than 1.0 ml/g
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • 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
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid 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
    • B01J20/28078—Pore diameter
    • B01J20/2808—Pore diameter being less than 2 nm, i.e. micropores or nanopores
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • 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
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid 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
    • B01J20/28088—Pore-size distribution
    • B01J20/28092—Bimodal, polymodal, different types of pores or different pore size distributions in different parts of the sorbent
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
    • B01J2220/485—Plants or land vegetals, e.g. cereals, wheat, corn, rice, sphagnum, peat moss
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
    • C02F2103/343—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the pharmaceutical industry, e.g. containing antibiotics

Abstract

Belonging to the technical field of environmental protection and repair material preparation, the invention relates to a preparation method of a hierarchical porous carbon material for adsorption of tetracycline antibiotics. The method includes: subjecting two-step prepared hierarchical porous activated carbon with good pore structure to cleaning and drying treatment, then carbonizing the obtained wicker, fully mixing the carbonized wicker with an inorganic base activator in certain proportion by physical method, and grinding the mixture to a uniform state; and by means of the activation effect of the inorganic base, conducting high-temperature calcination (750-850DEG C) to obtain the hierarchical porous activated carbon with high specific surface area and high pore volume. Also, the hierarchical porous activated carbon is used for adsorption separation of tetracycline, and the result shows that the hierarchical porous activated carbon has excellent adsorption properties to tetracycline. In the preparation process, the activation temperature and the activator dosage have enormous influence on the pore structure, and can be used to regulate the pore type structure.

Description

A kind of preparation method of the multi-stage porous carbon material for tetracycline antibiotics absorption
Technical field
The present invention relates to a kind of preparation method of multi-stage porous carbon material for tetracycline antibiotics absorption, belong to environmental conservation and Repair materials preparing technical field.
Background technology
At present, antibiotic is used on human and animal's prevention and treatment of diseases in a large number, in mankind's medical usage amount Account for more than the 6% of prescription drugs total amount, veterinary drug consumption accounts for more than 70% especially.It addition, agriculturally can also be used for rush Enter plant growing.But, antibiotic is by the assimilation effect of human or animal bad, and major part unconverted is decomposed and is directly over Excretory system enters in environment, and scholar has been found that the vestige of antibiotic in surface water, subsoil water, deposit and soil, Ecological environment is caused harm in various degree.Antibiotic is difficult to be decomposed by the microorganisms, and this becomes one in some sense The persistence organic pollutant that class is emerging.
Antibiotic in environment is in addition to causing chemical contamination, it is often more important that may in induced environment resistant microorganism and The generation of resistant gene, and accelerate propagation and the diffusion of antibiotic resistance.These resistant microorganisms can be by directly or indirectly The mode of contact enters human body, strengthens the drug resistance of human body, thus threatens to mankind's publilc health.Increasing card Closely related with the generation of pathogenic bacterium drug resistance according to display, resistant microorganism and resistant gene, and the increase of pathogenic bacterium drug resistance Have become as global disease with diffusion and treat the huge problem faced.
Tetracycline antibiotics be currently used the most extensively, one of the maximum Antibiotics of consumption, its action principle is to pass through Hinder aminoacyl tRNA to suppress tropina to synthesize with the combination of ribosome binding site, and then reach bacteriostasis.Such The microorganism of gram positive bacteria, gram negative bacteria, rickettsia and chlamydia etc can be played a role by antibiotic, tool There are broad spectrum antibacterial and good therapeutic effect.In addition to being widely used in medical treatment, also as veterinary drug and growth promoter for poultry and Culture fishery.Additionally, also add certain antibiotics during CARCASS QUALITY for suppressing the growth of antibacterial. Due to the cheapness of tetracycline antibiotics and broad spectrum activity, it has also become the class antibiotic that in environmental monitoring, recall rate is the highest.
Tetracycline, as one typical antibacterial type medicine, belongs to the Organic substance of difficult degradation, can induce Soil Microorganism drug resistance Property enhancing, and surface water and groundwater can be entered by the approach such as rainwash, leaching, consequently, it is possible to the health to the mankind Produce potential adverse effect, and tetracycline catabolite may produce harm to environmental microorganism and the mankind.Due to such Antibiotic has strong inhibitory action to bioprocess, utilizes conventional processing method to be extremely difficult to preferable effect.
In recent years, porous carbon materials has obtained increasing concern, and relevant report the most persistently increases, and some researcheres are recognized Can be as porous material of future generation for porous carbon materials.On the one hand, the precursor wide variety of porous carbon materials, cost are prepared Inexpensively；On the other hand, material with carbon element typically has a preferable biocompatibility, and chemical stability under anaerobic, Structural stability in low-density, high thermal conductivity, high conductivity and aqueous phase.Use in porous carbon materials Adsorption water body four The research of the antibiotic such as ring element has extremely important potentiality.
Summary of the invention
It is an object of the invention to provide the application of a kind of novel multi-stage porous carbon material, this material uses Salix babylonica L. (Salix Babylonica) current-year branch is as carbon source, utilizes inorganic base to carry out reaming activation and has big specific surface area, hole to obtain The porous carbon materials that footpath is evenly distributed, and it is applied to tetracycline adsorption.
The technical solution used in the present invention is: the preparation method of a kind of porous carbon materials for tetracycline absorption, according to following Step is carried out:
(1) carbonization
Gather the current-year branch of Salix babylonica L. (Salix babylonica), clean, air-dry；Branch is cut to 2-4cm segment, dress Enter magnetic boat, quartz tube furnace is used N2Air-flow protection, is warming up to 450-550 DEG C with 5.0-10.0 DEG C/min, and maintaining should Temperature calcination 1-2h, obtains wicker based biomass carbon.
(2) activation
Wicker based biomass carbon and inorganic base (KOH, NaOH) are mixed with the ratio of 1:1-4 (mass ratio), is placed in Agate mortar is ground to mixing be uniformly dispersed, quartz tube furnace is used N2Air-flow protection, heats up with 4.0-8.0 DEG C/min To 700-850 DEG C, maintain this temperature calcination 1-2h, obtain the multi-stage porous carbon of activation.
The method that porous carbon materials is used for absorption is:
Antibiotic is configured to the aqueous solution of 200mg/L, pipettes 25ml with pipet and put in politef hermetic container, It is subsequently adding the multi-stage porous carbon 5mg of preparation, supersound process 1min, after making activation porous carbon be uniformly dispersed in the solution, will It is placed in 298K water bath with thermostatic control 24h to reach adsorption equilibrium.
Use film changeable needle-based to cross the solution after film device utilizes aqueous phase CN-CA to separate absorption during measurement, obtain without adsorbent Tetracycline absorption residual liquid, uses UV/visible spectrophotometer (Genesys 10UV vis, Thermo Electron Corporation, USA) Measure its concentration.
It is calculated adsorption capacity (Q by formula belowe)。
Q e = V ( C 0 - C e ) M
Wherein CoAnd C (mg/L)e(mg/L) being initial and equilibrium concentration respectively, M (mg) is adsorbent amount, V (mL) For liquor capacity.
The technological merit of the present invention: the adsorbing material that the present invention uses also is a kind of charcoal, belongs to environment-friendly material, and Material is cheap, wide material sources, and willow is the most extensively planted in China, fast growth, it is ensured that this material Extensive supply in the application.Wicker has abundant wood fibre and conveying moisture and the pore passage structure of nutrition, and this is to many Preparing of hole carbon is extremely beneficial.The activated carbon with high-specific surface area and pore volume has been synthesized by carbonization and activation two steps, and And can utilize the activation temperature in building-up process and two important parameters of activator level that its permeability structure is regulated and controled.Should Activated carbon prepared by method possesses good stability and regenerability, is successfully applied to the antibiotic such as tetracycline in water environment Separate absorption.It is possible not only to provide a kind of cycling and reutilization approach for discarded wicker establishment processed goods, is also antibiosis in water body The Adsorption of the organic pollutions such as element provides a kind of cheap, preparation method of effective adsorbing material.
Accompanying drawing explanation
(a, b) with transmission electron microscope picture (c) for the scanning electron microscope (SEM) photograph of the multi-stage porous carbon material that Fig. 1 embodiment 1 prepares；Can from figure Go out, after inorganic base activates, also have substantial amounts of hierarchical porous structure in its surface.
The N of the multi-stage porous carbon material that Fig. 2 embodiment 1 prepares2Adsorption-desorption isothermal (a) and graph of pore diameter distribution (b).Isothermal Line is I type isothermal line, i.e. pore type, and figure (b) further confirms that its microcellular structure.
The infrared spectrogram of the multi-stage porous carbon material that Fig. 3 embodiment 1 prepares.As seen from the figure: 3420cm-1Place's broad peak is that-OH stretches Vibration peak, illustrates containing hydrogen bond；1578cm-1For C=C stretching vibration peak.1440cm-1Weak Absorption peak corresponding to fat The C-H bending vibration of fat hydrocarbon；1040cm-1Absworption peak shake corresponding to the C-O in ether, alcohol and phenolic compound is flexible Dynamic.
Detailed description of the invention
Below in conjunction with being embodied as example, the present invention will be further described:
Embodiment 1
Wicker after processing is placed in Ci Zhou, at N2In the quartz ampoule of protection, the heating rate through 5 DEG C/min rises to 450 After DEG C maintain 2h, take the wicker after carbonization and potassium hydroxide by the quality of 1:1 than mixed grinding uniform after, be placed in nickel crucible In, at N2Gas shield is warming up to 750 DEG C of calcining 2h with 8 DEG C/min in quartz tube furnace, obtains multi-stage porous carbon. This multi-stage porous carbon material BET surface area is 2306.87m2/ g, pore volume is 1.38cm3/ g, according to t-plot method, micro- Aperture surface area is 1716.26m2/ g, micropore volume is 0.91cm3/ g, still falls within hierarchical porous structure, and based on micropore.
Adsorption test result shows: under 298K temperature conditions, and tetracycline is adsorbed by the hole material with carbon element prepared by embodiment 1 Amount is 502.87mg/g.When initial concentration is 150mg L-1Time, adsorption reaction can reach balance in 90min.
Embodiment 2
Wicker after processing is placed in Ci Zhou, at N2In the quartz ampoule of protection, the heating rate through 10 DEG C/min rises to 550 After DEG C maintain 1h, take the wicker after carbonization and potassium hydroxide by the quality of 1:4 than mixed grinding uniform after, be placed in nickel crucible In, at N2Gas shield is warming up to 850 DEG C of calcining 1h with 5 DEG C/min in quartz tube furnace, obtains multi-stage porous carbon. This multi-stage porous carbon material BET (Brunauer-Emmett-Teller) surface area is 3342.96m2/ g, pore volume is 1.91cm3/ g, According to t-plot method, micropore surface amasss as 2855.35m2/ g, micropore volume is 1.49cm3/ g, belongs to hierarchical porous structure, Based on micropore.
Adsorption test result shows: under 298K temperature conditions, and the hole material with carbon element described in embodiment 2 is to tetracycline adsorbance For 942.87mg/g.Further, it is 150mg L when initial concentration-1Time, adsorption reaction can reach balance in 60min, There is the rate of adsorption faster.
Comparative example 1, illustrates that the consumption of inorganic base activator and activation temperature are formed for pore structure and have important effect. Inorganic base activator plays important drilling effect in activation, and pore structure increases along with activator incorporation within the specific limits And enrich；And activation temperature is also an important parameter of regulation and control pore structure, activate with deep activation in certain temperature range Being main, produce a large amount of micropore, exceed certain temperature range and be then mainly width activation, partial pore is converted into mesoporous, big Pore structure.Contrasting hole material with carbon element prepared by a series of different condition, the technological parameter in this embodiment is more excellent parameter.
Embodiment 3
Wicker after processing is placed in Ci Zhou, at N2In the quartz ampoule of protection, the heating rate through 10 DEG C/min rises to 500 After DEG C maintain 1.5h, take the wicker after carbonization and potassium hydroxide (KOH) by the quality of 1:3 than mixed grinding uniform after, put In nickel crucible, at N2Gas shield is warming up to 800 DEG C of calcining 1h with 4 DEG C/min in quartz tube furnace, obtains many Level hole carbon；This multi-stage porous carbon material BET surface area is 2696.07m2/ g, pore volume is 1.70cm3/ g, according to t-plot Method, micropore surface amasss as 2293.75m2/ g, micropore volume is 1.46cm3/ g, still falls within hierarchical porous structure, and with micro- Kong Weizhu.
In adsorption experiment, take respectively initial concentration be respectively 200mg/L ciprofloxacin (Ciprofloxacin, CFX) and Sulfamethazine (Sulfamethazine, SMZ) solution 25ml, in polytetrafluoroethylcontainer container, is sequentially added into 5mg Embodiment 3 preparation multi-stage porous carbon, ultrasonic to fully dispersed after, be placed in 298K water bath with thermostatic control maintenance 24h.Absorption result Show that it is respectively 632.44mg/g and 587.41mg/g to ciprofloxacin and sulfamethazine adsorbance, this method is described The multi-stage porous carbon of preparation has preferable absorption property to most antibiotic.
Each raw material cited by the present invention can realize the present invention, and the bound value of each raw material, interval value can realize The present invention, embodiment numerous to list herein.The technological parameter (activator level, calcining heat and time) of the present invention Bound value, interval value can realize the present invention, embodiment numerous to list herein.Therefore without departing substantially from claim and Under the general concept that equivalency range is limited, the present invention is not limited to specific details and shown here as the legend with description.

Claims (6)

1. the preparation method for the multi-stage porous carbon material of tetracycline antibiotics absorption, it is characterised in that this is multistage Hole material with carbon element is carried out as steps described below:
(1) carbonization
Gather the current-year branch of Salix babylonica L., clean, air-dry；Branch is cut to segment, loads magnetic boat, in quartz tube furnace Use N2Air-flow protection, calcining obtains wicker based biomass carbon；
(2) activation
Wicker based biomass carbon and inorganic base are mixed, is ground to mixing and is uniformly dispersed, quartz tube furnace is used N2Air-flow is protected Protecting, calcining obtains the multi-stage porous carbon of activation；By the calcining heat in building-up process with as the inorganic base consumption pair of activator The pore structure of multi-stage porous carbon regulates and controls.
A kind of preparation method of the multi-stage porous carbon material for tetracycline antibiotics absorption, It is characterized in that: in step (1), a length of 2-4cm of described segment.
A kind of preparation method of the multi-stage porous carbon material for tetracycline antibiotics absorption, It is characterized in that: in step (1), calcining refers to: be warming up to 450-550 DEG C with 5.0-10.0 DEG C/min, maintains this temperature Calcining 1-2h.
A kind of preparation method of the multi-stage porous carbon material for tetracycline antibiotics absorption, It is characterized in that: in step (2), described inorganic base is KOH or NaOH.
A kind of preparation method of the multi-stage porous carbon material for tetracycline antibiotics absorption, It is characterized in that: in step (2), the mass ratio of wicker based biomass carbon and inorganic base is 1:1 4, and calcining refers to 4.0 -8.0 DEG C/min is warming up to 700-850 DEG C, maintains this temperature calcination 1-2h.
A kind of preparation method of the multi-stage porous carbon material for tetracycline antibiotics absorption, its Being characterised by: in step (2), the mass ratio of wicker based biomass carbon and inorganic base is 1:4, and calcining refers to 5 DEG C/min It is warming up to 850 DEG C, maintains this temperature calcination 1h.
CN201610299434.5A 2016-05-06 2016-05-06 Preparation method of hierarchical porous carbon material for adsorption of tetracycline antibiotics Pending CN105944702A (en)

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