CN105944681A - Preparation method and application of potassium carboxylate base porous carbon material - Google Patents

Preparation method and application of potassium carboxylate base porous carbon material Download PDF

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Publication number
CN105944681A
CN105944681A CN201610356886.2A CN201610356886A CN105944681A CN 105944681 A CN105944681 A CN 105944681A CN 201610356886 A CN201610356886 A CN 201610356886A CN 105944681 A CN105944681 A CN 105944681A
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porous carbon
base porous
carboxylic acid
carbon materials
acid potassium
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CN105944681B (en
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戴江栋
田苏君
何劲松
谢阿田
孙骏
常忠帅
李春香
闫永胜
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Jiangsu University
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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
    • B01J20/22—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
    • 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
    • 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
    • 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
    • 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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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Hydrology & Water Resources (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention provides a preparation method and application of a potassium carboxylate base porous carbon material. The method is performed according to the following steps: weighing potassium acetate, potassium citrate or potassium tartrate crystals, putting into a mortar, sufficiently grinding, then putting into a tube furnace, introducing inert gas, calcining, naturally cooling, then taking out a product in the tube furnace, washing by using hydrochloric acid to remove impurities, performing decompression suction filtration, washing by using deionized water, and drying to obtain the potassium carboxylate base porous carbon material. The obtained potassium carboxylate base porous carbon material is relatively high in yield, has a greater specific surface area and microporosity, can quickly and efficiently adsorb antibiotics and dyes in water, and is relatively stable in physico-chemical property.

Description

A kind of preparation method and its usage of carboxylic acid potassium salt's base porous carbon materials
Technical field
The invention belongs to technical field of environment function material preparation, refer in particular to a kind of carboxylic acid potassium salt's base porous carbon materials preparation method and Purposes.
Background technology
In recent years, the Wastewater Pollutant of some such as dyestuff and medicine antibiotic has been subjected to the extensive concern of people.Many waste water Below standard standard is just discharged in natural environment, and ecological environment and human health cause threat greatly, big in usual waste water The chloromycetin content of amount is detected.Chloromycetin (Chloramphenicol, CAP), as a kind of broad-spectrum antibiotics, is by committee The antibiotic that auspicious slide fastener silk bacterium produces, belongs to biocidal property broad ectrum antibiotic, has stronger to gram negative bacteria and gram positive bacteria Inhibitory action, the growth being widely used in the prevention of human and animal's infectious disease and treatment and animal for a long time promotees Enter agent.Substantial amounts of research shows, can not be completely degraded in the chloromycetin short time, and taking in internal antibiotic can not be complete by organism Hypersorption, major part is got rid of external with original shape or metabolite, is finally flowed into water body.Owing to the cost ratio of chloromycetin is relatively low, the most such as The present, the most still there are many countries at illegal use chloromycetin.A large amount of uses of chloromycetin not only can make bacterial resistance occurred, And the imbalance of animal body normal flora, resistance reduction, the various disease of easy infection can be caused.Accordingly, it would be desirable to research is a kind of fast The cost-effective method of speed removes chloromycetin series antibiotics in environment.
Currently, the method processing water pollutant mainly has absorption method, light degradation method, biodegradation etc., and wherein absorption method is one Plant the effective ways removing water pollutant of low energy consumption and clean and effective.The most industrial mainly using activated carbon as adsorbent Removing pollutant, and activated carbon structure, specific surface area, the character such as surface functional group all can affect the removal efficiency of pollutant. And regenerating active carbon is poor, mechanical strength is low, to solve this problem it is necessary to find a kind of novel, and functional height Adsorbent go solve pollutant removal problem.
Porous carbon materials is the carbon element functional material that a kind of pore structure is flourishing, possesses that specific surface area is big, chemical stability is high, machine Tool performance is catalyzed by force that activity is high and pore passage structure and the excellent properties such as aperture size is adjustable, has electric conductivity, heat conductivity concurrently simultaneously And the advantage such as its preparation cost is cheap, process is easy, it is widely used in ultracapacitor, fuel cell, Water warfare, Gas separates and pollutant absorption etc..The characteristic of these excellences makes porous carbon materials be expected to as adsorbent and is applied to water pollution process In.
Summary of the invention
This experiment is with potassium acetate, potassium citrate or Soluble tartar. as carbon source, and direct high-temperature calcination, same under nitrogen or argon Step carbonization and activation, then remove impurity with hydrochloric acid, and reduce pressure sucking filtration, is had to neutrality with deionized water or hot wash Carboxylic acid potassium salt's base porous carbon materials of high-specific surface area；And utilize multiple characterization method, investigate pattern and the hole of composite The parameters such as road distribution, by adsorption experiment research carboxylic acid potassium salt's base porous carbon materials to the removal capacity of chloromycetin in water environment.
The technical solution used in the present invention is:
The preparation method of a kind of carboxylic acid potassium salt's base porous carbon materials, is carried out as steps described below:
Weigh potassium acetate, potassium citrate or Rochelle salt to put in mortar and be fully ground, be subsequently placed in tube furnace, be passed through Noble gas, calcines, and after natural cooling, is taken out by the product in tube furnace, removes impurity, decompression with salt acid elution Sucking filtration, is washed with deionized, and dries, and prepares carboxylic acid potassium salt's base porous carbon materials.
The quality of described potassium acetate, potassium citrate or Rochelle salt is 10g.
Described noble gas is nitrogen or argon.
Described calcining manners is 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 dimensions Hold 1.0～4.0h.
Concentration of hydrochloric acid used is 1.0～12mol L-1。
Prepared carboxylic acid potassium salt's base porous carbon materials is for adsorbing the chloromycetin in water.
The technological merit of the present invention:
(1) carbon source potassium acetate, potassium citrate or Soluble tartar. used by, abundance, cheap, economic and environment-friendly.
(2) gained carboxylic acid potassium salt base porous carbon productivity is higher, and has higher specific surface area and microporosity, can be rapidly and efficiently Absorption water in antibiotic and dyestuff, physico-chemical property is relatively stable.
(3) operational approach of the present invention is simple, synchronize carbonization and activation, and flow process is shorter, easy controlled operation, is suitable to popularization and makes With.
Accompanying drawing explanation
Fig. 1 is the Electronic Speculum figure of the material prepared by embodiment 2, and wherein (a) is scanning electron microscope (SEM) photograph, and (b) is transmission electron microscope picture；
Fig. 2 is nitrogen adsorption-desorption isothermal line and the graph of pore diameter distribution of the material prepared by embodiment 2；
Fig. 3 is that the material prepared by embodiment 2 is to the adsorption isotherm line chart of chloromycetin in water environment；
Fig. 4 is that the material prepared by embodiment 2 is to the adsorption dynamics adsorption kinetics figure of chloromycetin in water environment.
Detailed description of the invention
Below in conjunction with the accompanying drawings and the present invention is described further by specific embodiment.
Embodiment 1:
Being fully ground by 10g potassium citrate, put under nitrogen protection in tube furnace and calcine, temperature is 700 DEG C, and heating rate is 3℃ min-1, maintain 1.0h；By prepared product 1mol L-1HCl washing go the removal of impurity, repeatedly wash with deionized water to Neutrality, is dried and both obtains carboxylic acid potassium salt's base porous carbon materials.
Staticadsorption experiment is utilized to complete；The chloromycetin solution of 10mL variable concentrations is joined in centrifuge tube, adds the most wherein Enter 2.0mg carboxylic acid potassium salt's base porous carbon materials, water bath with thermostatic control stands, has investigated solution ph, time of contact, temperature ion The impact that chloromycetin is adsorbed by intensity；Absorption reach saturated after, 0.22um membrane filtration collect the supernatant, use ultraviolet-visible The chloromycetin molecular concentration that photometer is not to be adsorbed in 278nm records test solution, is calculated adsorption capacity (Qe)。
Q e = ( C 0 - C e ) V m
Wherein C0(mg L-1) and Ce(mg L-1) it is initial and equilibrium concentration respectively, m (mg) is adsorbent amount, and V (mL) is Liquor capacity.
Take 10mL initial concentration and be respectively 30～170mg L-1Chloromycetin solution join in centrifuge tube, be separately added into 2.0mg Carboxylic acid potassium salt's base porous carbon materials, after test fluid is placed in 298K water-bath standing 24h, collects the supernatant, not to be adsorbed Chloromycetin molecular concentration ultraviolet-uisible spectrophotometer measures, and calculates adsorption capacity, last equilibrium adsorption capacity according to result For 389.9mg g-1。
Taking 10mL initial concentration is 150mg L-1Chloromycetin solution join in centrifuge tube, be separately added into 2.0mg carboxylic acid potassium salt Base porous carbon materials, is placed on test fluid in the water-bath of 298K and stands 5.0～330min respectively.After standing completes, collect upper strata clear Liquid, chloromycetin molecular concentration ultraviolet-uisible spectrophotometer not to be adsorbed measures, and calculates adsorption capacity according to result； Result shows: initial concentration is 150mg L-1, when temperature is 298K, about 300min reaches adsorption equilibrium.
Embodiment 2:
Being fully ground by 10g potassium acetate, put under nitrogen protection in tube furnace and calcine, temperature is 850 DEG C, and heating rate is 5 DEG C min-1, maintain 2.0h；By prepared product 5mol L-1HCl washing go the removal of impurity, repeatedly wash to neutrality with deionized water, It is dried and both obtains carboxylic acid potassium salt's base porous carbon materials.By embodiment 1 step operation, gained equilibrium adsorption capacity is 509.8mg g-1.Just Beginning concentration is 150mg L-1, when temperature is 298K, about 250min reaches adsorption equilibrium.
Fig. 1 is the Electronic Speculum figure of the material prepared by embodiment 2, and wherein (a) is scanning electron microscope (SEM) photograph, and (b) is transmission electron microscope picture； Can be seen that this carboxylic acid potassium salt's base porous carbon materials is fibre-like structure from 1a, and reunite together mutually, surface is somewhat coarse； From Fig. 1 b it can be clearly seen that carbon material surface is uniform-distribution with nano-pore, the beneficially attachment of contaminant molecule.
Fig. 2 is nitrogen adsorption-desorption isothermal line and the graph of pore diameter distribution of the material prepared by embodiment 2；Wherein (a) is nitrogen Aspiration is attached-desorption isothermal line, and (b) is graph of pore diameter distribution；As can be seen from the figure the absorption of porous carbon materials belongs to I type (root Classify according to IUPAC), low pressure when, absorption ratio is very fast；Fig. 2 b we it appeared that bore dia less than 2nm, shows to inhale Attached dose has substantial amounts of micropore.
Fig. 3 is that the material prepared by embodiment 2 is to the adsorption isotherm line chart of chloromycetin in water environment；As shown in Figure 3: along with just The rising of beginning concentration, adsorbance increases therewith, and during 298K, equilibrium adsorption capacity is 509.8mg g-1。
Fig. 4 is that the material prepared by embodiment 2 is to the adsorption dynamics adsorption kinetics figure of chloromycetin in water environment.As shown in Figure 4, along with contact The increase of time, adsorbance increases sharply, and at front 70min, adsorbance increases very fast, and about 250min slowly tends to balance, Show adsorption equilibrium faster.
Embodiment 3:
Being fully ground by 10g Soluble tartar., put in tube furnace and calcine under argon shield, temperature is 900 DEG C, heating rate It is 10 DEG C of min-1, maintain 4.0h；By prepared product 12mol L-1HCl washing go the removal of impurity, many with deionized water Secondary washing, to neutral, be dried and both obtain carboxylic acid potassium salt's base porous carbon materials.By embodiment 1 step operation, gained equilibrium adsorption capacity is 435.3mg g-1.It is 150mg L at initial concentration-1, when temperature is 298K, about 270min reaches adsorption equilibrium.

Claims (6)

1. the preparation method of carboxylic acid potassium salt's base porous carbon materials, it is characterised in that carry out as steps described below:
Weigh potassium acetate, potassium citrate or Rochelle salt to put in mortar and be fully ground, be subsequently placed in tube furnace, be passed through Noble gas, calcines, and after natural cooling, is taken out by the product in tube furnace, removes impurity, decompression with salt acid elution Sucking filtration, is washed with deionized, and dries, and prepares carboxylic acid potassium salt's base porous carbon materials.
The preparation method of a kind of carboxylic acid potassium salt's base porous carbon materials the most according to claim 1, it is characterised in that described second The quality of acid potassium, potassium citrate or Rochelle salt is 10g.
The preparation method of a kind of carboxylic acid potassium salt's base porous carbon materials the most according to claim 1, it is characterised in that described Noble gas is nitrogen or argon.
The preparation method of a kind of carboxylic acid potassium salt's base porous carbon materials the most according to claim 1, it is characterised in that described Calcining manners is as follows: heating rate is 3.0～10 DEG C of min-1, rise to 700～900 DEG C and maintain 1.0～4.0h at 700～900 DEG C.
The preparation method of a kind of carboxylic acid potassium salt's base porous carbon materials the most according to claim 1, it is characterised in that used Concentration of hydrochloric acid is 1.0～12mol L-1。
6. the purposes of carboxylic acid potassium salt's base porous carbon materials that prepared by the method described in Claims 1 to 5 any one, it is characterised in that Prepared carboxylic acid potassium salt's base porous carbon materials is for adsorbing the chloromycetin in water.
CN201610356886.2A 2016-05-26 2016-05-26 A kind of preparation method and its usage of carboxylic acid potassium salt's base porous carbon materials Expired - Fee Related CN105944681B (en)

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Cited By (5)

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CN107175090A (en) * 2017-05-31 2017-09-19 中国科学院南京土壤研究所 A kind of porous carbon solid-phase micro-extraction coating and its preparation method and application
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
CN115231550A (en) * 2022-08-05 2022-10-25 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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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107175090A (en) * 2017-05-31 2017-09-19 中国科学院南京土壤研究所 A kind of porous carbon solid-phase micro-extraction coating and its preparation method and application
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
CN115231550A (en) * 2022-08-05 2022-10-25 中国新型建材设计研究院有限公司 Preparation method and application of porous carbon material
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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