CN105944681B - A kind of preparation method and its usage of carboxylic acid potassium salt's base porous carbon materials - Google Patents
A kind of preparation method and its usage of carboxylic acid potassium salt's base porous carbon materials Download PDFInfo
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- CN105944681B CN105944681B CN201610356886.2A CN201610356886A CN105944681B CN 105944681 B CN105944681 B CN 105944681B CN 201610356886 A CN201610356886 A CN 201610356886A CN 105944681 B CN105944681 B CN 105944681B
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/223—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
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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
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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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
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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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
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
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Abstract
The present invention provides a kind of preparation method and its usage of carboxylic acid potassium salt's base porous carbon materials, the method carries out as steps described below：It weighs potassium acetate, potassium citrate or Rochelle salt and is put into mortar and be fully ground, it is subsequently placed in tube furnace, it is passed through inert gas, is calcined, after natural cooling, product in tube furnace is taken out, impurity is removed with salt acid elution, decompression is filtered, is washed with deionized, carboxylic acid potassium salt's base porous carbon materials are made in drying.Gained carboxylic acid potassium salt's base porous carbon yield is higher, and possesses higher specific surface area and microporosity, antibiotic and dyestuff in absorption water that can be rapidly and efficiently, and physico-chemical property is relatively stable.
Description
Technical field
The invention belongs to technical field of environment function material preparation, refer in particular to a kind of preparation side of carboxylic acid potassium salt's base porous carbon materials
Method and application thereof.
Background technology
In recent years, some such as Wastewater Pollutants of dyestuff and medical antibiotic have got more and more people's extensive concerning.Perhaps
More below standard standards of waste water are just discharged into natural environment, cause great threat to ecological environment and human health, usually
A large amount of chloromycetin content is detected in waste water.Chloramphenicol (Chloramphenicol, CAP) is used as a kind of broad spectrum activity antibiosis
Element is the antibiotic generated by Venezuela Streptothrix, belongs to biocidal property broad-spectrum antibiotic, to Gram-negative bacteria and gram sun
Property bacterium has stronger inhibiting effect, be widely used in for a long time the prevention and treatment of human and animal's communicable disease with
And the growth promoter of animal.Largely studies have shown that cannot be completely degraded in the chloramphenicol short time, internal antibiotic is taken in
It cannot be fully absorbed by organism, it is most of to exclude in vitro, to finally flow into water body with original shape or metabolin.Due to chloramphenicol at
This is relatively low, and nowadays, still there are many countries in the world uses chloramphenicol illegal.A large amount of use of chloramphenicol can not only make carefully
Bacterium develops immunity to drugs, and the imbalance of animal body normal flora, resistance can be caused to reduce, the various diseases of easy infection.Therefore, it needs
A kind of effective method of fast, economical is studied to remove chloromycetin series antibiotics in environment.
Currently, the method for handling water pollutant mainly has absorption method, light degradation method, biodegradation etc., wherein absorption method
It is a kind of effective ways for removing water pollutant of low energy consumption and clean and effective.It is industrial at present mainly using activated carbon as
Adsorbent removes pollutant, and activated carbon structure, specific surface area, the properties such as surface functional group can all influence the removal of pollutant
Efficiency.And regenerating active carbon is poor, and mechanical strength is low, to solve this problem it is necessary to find a kind of novel, function
The high adsorbent of property goes to solve the problems, such as the removal of pollutant.
Porous carbon materials are a kind of carbon functional materials of pore structure prosperity, have large specific surface area, chemical stability
High, the strong catalytic activity of mechanical performance is high and the excellent properties such as pore passage structure and aperture size are adjustable, at the same have both electric conductivity,
The advantages that thermal conductivity and its manufacturing cost are cheap, process is easy is widely used in ultracapacitor, fuel cell, water
Purification, gas separation and pollutant absorption etc..These excellent characteristics make porous carbon materials be expected to be applied to water as adsorbent
In pollution processing.
Invention content
This experiment is using potassium acetate, potassium citrate or potassium tartrate as carbon source, and direct high temperature is forged under nitrogen or argon
It burns, it is synchronous to be carbonized and activate, impurity then is removed with hydrochloric acid, decompression filters, and is washed to neutral and is obtained with deionized water or hot water
To carboxylic acid potassium salt's base porous carbon materials with high-specific surface area；And a variety of characterization methods are utilized, investigate the shape of composite material
The parameters such as looks and pore distribution are studied carboxylic acid potassium salt's base porous carbon materials by adsorption experiment and are gone to chloramphenicol in water environment
Except performance.
The technical solution adopted by the present invention is：
A kind of preparation method of carboxylic acid potassium salt's base porous carbon materials, carries out as steps described below：
It weighs potassium acetate, potassium citrate or Rochelle salt and is put into mortar and be fully ground, be subsequently placed in tube furnace,
It is passed through inert gas, is calcined, after natural cooling, the product in tube furnace is taken out, impurity is removed with salt acid elution, subtracts
Pressure filters, and is washed with deionized, and dries, and carboxylic acid potassium salt's base porous carbon materials are made.
The quality of the potassium acetate, potassium citrate or Rochelle salt is 10g.
The inert gas is nitrogen or argon gas.
The calcining manners are as follows：Heating rate is 3.0~10 DEG C of min-1, rise to 700~900 DEG C and 700~
900 DEG C of 1.0~4.0h of maintenance.
Concentration of hydrochloric acid used is 1.0~12mol L-1。
Prepared carboxylic acid potassium salt's base porous carbon materials are used to adsorb the chloramphenicol in water.
The technological merit of the present invention：
(1) carbon source potassium acetate, potassium citrate or potassium tartrate used in, abundance is cheap, economic and environment-friendly.
(2) gained carboxylic acid potassium salt's base porous carbon yield is higher, and possesses higher specific surface area and microporosity, can be quickly
Antibiotic and dyestuff in efficient absorption water, physico-chemical property are relatively stable.
(3) operating method of the invention is simple and practicable, synchronous carbonization and activation, and flow is shorter, easy controlled operation, is suitable for promoting
It uses.
Description of the drawings
Fig. 1 is the electron microscope of the material prepared by embodiment 2, wherein (a) is scanning electron microscope (SEM) photograph, it is (b) transmission electron microscope picture；
Fig. 2 is the nitrogen adsorption-desorption thermoisopleth and graph of pore diameter distribution of the material prepared by embodiment 2；
Fig. 3 is adsorption isotherm map of the material prepared by embodiment 2 to chloramphenicol in water environment；
Fig. 4 is adsorption dynamics adsorption kinetics figure of the material prepared by embodiment 2 to chloramphenicol in water environment.
Specific implementation mode
Below in conjunction with the accompanying drawings and specific embodiment is described further the present invention.
Embodiment 1：
10g potassium citrates are fully ground, is put into tube furnace calcines under nitrogen protection, temperature is 700 DEG C, heating speed
Rate is 3 DEG C of min-1, maintain 1.0h；By product obtained 1mol L-1HCl washing removal impurity, it is multiple with deionized water
Washing is dried to obtain carboxylic acid potassium salt's base porous carbon materials to neutrality.
It is completed using Staticadsorption experiment；The chloromycetin solution of 10mL various concentrations is added in centrifuge tube, respectively to
2.0mg carboxylic acid potassium salt's base porous carbon materials are wherein added, is stood in water bath with thermostatic control, has investigated solution ph, time of contact, temperature
The influence that ionic strength adsorbs chloramphenicol；Absorption reach saturation after, 0.22um membrane filtrations collect supernatant liquor, with it is ultraviolet can
Light-exposed photometer chloramphenicol molecular concentration not to be adsorbed in 278nm measures test solution, is calculated adsorption capacity (Qe)。
Wherein C0(mg L-1) and Ce(mg L-1) it is initial and equilibrium concentration respectively, m (mg) is adsorbent amount, V (mL)
For liquor capacity.
It is respectively 30~170mg L to take 10mL initial concentrations-1Chloromycetin solution be added in centrifuge tube, be separately added into
2.0mg carboxylic acid potassium salt's base porous carbon materials, are placed on test fluid after being stood for 24 hours in 298K water-baths, collect supernatant liquor, are not inhaled
Attached chloramphenicol molecular concentration is measured with ultraviolet-uisible spectrophotometer, and calculates adsorption capacity according to result, is finally balanced
Adsorbance is 389.9mg g-1。
It is 150mg L to take 10mL initial concentrations-1Chloromycetin solution be added in centrifuge tube, be separately added into 2.0mg carboxylic acids
Sylvite base porous carbon materials, are placed on test fluid in the water-bath of 298K and stand 5.0~330min respectively.After the completion of standing, collect
Supernatant liquor, chloramphenicol molecular concentration not to be adsorbed is measured with ultraviolet-uisible spectrophotometer, and calculates suction according to result
Attached capacity；The result shows that：Initial concentration is 150mg L-1, when temperature is 298K, 300min or so reaches adsorption equilibrium.
Embodiment 2：
10g potassium acetates are fully ground, is put into tube furnace calcines under nitrogen protection, temperature is 850 DEG C, heating rate
For 5 DEG C of min-1, maintain 2.0h；By product obtained 5mol L-1HCl washing removal impurity, repeatedly washed with deionized water
It washs to neutrality, is dried to obtain carboxylic acid potassium salt's base porous carbon materials.By 1 step operation of embodiment, gained equilibrium adsorption capacity is
509.8mg g-1.It is 150mg L in initial concentration-1, when temperature is 298K, 250min or so reaches adsorption equilibrium.
Fig. 1 is the electron microscope of the material prepared by embodiment 2, wherein (a) is scanning electron microscope (SEM) photograph, it is (b) transmission electron microscope picture；
From 1a it can be seen that carboxylic acid potassium salt's base porous carbon materials are fibre-like structure, and reunite together mutually, surface is somewhat thick
It is rough；It can be clearly seen that carbon material surface is uniform-distribution with nano-pore from Fig. 1 b, be conducive to the attachment of contaminant molecule.
Fig. 2 is the nitrogen adsorption-desorption thermoisopleth and graph of pore diameter distribution of the material prepared by embodiment 2；Wherein (a) is
Nitrogen adsorption-desorption thermoisopleth (b) is graph of pore diameter distribution；As can be seen from the figure the absorption of porous carbon materials belongs to I types
(being classified according to IUPAC), absorption is than very fast when low pressure；We can be found that bore dia is less than 2nm to Fig. 2 b, show to adsorb
Agent has a large amount of micropore.
Fig. 3 is adsorption isotherm map of the material prepared by embodiment 2 to chloramphenicol in water environment；As shown in Figure 3：With
The raising of initial concentration, adsorbance increase therewith, and when 298K, equilibrium adsorption capacity is 509.8mg g-1。
Fig. 4 is adsorption dynamics adsorption kinetics figure of the material prepared by embodiment 2 to chloramphenicol in water environment.As shown in Figure 4, with
The increase of time of contact, adsorbance increases sharply, and in preceding 70min, adsorbance increases comparatively fast, and 250min or so slowly tends to be flat
Weighing apparatus, shows adsorption equilibrium faster.
Embodiment 3：
10g potassium tartrates are fully ground, is put into tube furnace calcines under protection of argon gas, temperature is 900 DEG C, heating speed
Rate is 10 DEG C of min-1, maintain 4.0h；By product obtained 12mol L-1HCl washing removal impurity, it is more with deionized water
Secondary washing is dried to obtain carboxylic acid potassium salt's base porous carbon materials to neutrality.By 1 step operation of embodiment, gained equilibrium adsorption capacity is
435.3mg g-1.It is 150mg L in initial concentration-1, when temperature is 298K, 270min or so reaches adsorption equilibrium.
Claims (1)
1. a kind of carboxylic acid potassium salt's base porous carbon materials are used to adsorb the purposes of the chloramphenicol in water, which is characterized in that the carboxylic acid
The preparation method of sylvite base porous carbon materials carries out as steps described below：
It weighs potassium acetate, potassium citrate or Rochelle salt and is put into mortar and be fully ground, potassium acetate, potassium citrate or winestone
The quality of sour potassium crystal is 10g；It is subsequently placed in tube furnace, is passed through nitrogen or argon gas, is calcined, the mode of the calcining
It is as follows：Heating rate is 3.0 ~ 10 DEG C of min-1, rise to 700 ~ 900 DEG C and maintain 1.0 ~ 4.0 h at 700 ~ 900 DEG C；Wait for that nature is cold
But after, the product in tube furnace is taken out, with a concentration of 1.0 ~ 12 mol L-1Salt acid elution remove impurity, decompression filter, use
Deionized water is washed, and carboxylic acid potassium salt's base porous carbon materials are made in drying.
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| CN107175090B (en) * | 2017-05-31 | 2020-04-24 | 中国科学院南京土壤研究所 | Porous carbon solid phase micro-extraction coating and preparation method and application thereof |
| CN107519874A (en) * | 2017-08-22 | 2017-12-29 | 江苏大学 | A kind of preparation method and applications of cobalt doped carboxylic acid potassium salt base combined multi-stage hole carbon material |
| CN107993855A (en) * | 2017-11-16 | 2018-05-04 | 三峡大学 | A kind of preparation method of high voltage sodium ion ultracapacitor |
| CN110252246A (en) * | 2019-07-01 | 2019-09-20 | 河南城建学院 | A kind of coal fly ash hollow micro bead is template potassium salt Quito hole carbon adsorbing material and its preparation method and application |
| CN115231550B (en) * | 2022-08-05 | 2024-02-06 | 中国新型建材设计研究院有限公司 | Preparation method and application of porous carbon material |
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| US9415996B2 (en) * | 2014-08-18 | 2016-08-16 | BlackPak, Inc. | Sorption pumps and storage for gases |
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| A general and facile synthesis strategy towards highly porous carbons: carbonization of organic salts;Marta Sevilla et al.;《J. Mater. Chem. A》;20131014;第1卷;第1378页摘要、Scheme 1，第13739页Table 1，Experimental Section部分 * |
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