CN106185923A - A kind of inorganic salt template auxiliary method preparing porous carbon nano material and application thereof - Google Patents

A kind of inorganic salt template auxiliary method preparing porous carbon nano material and application thereof Download PDF

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Publication number
CN106185923A
CN106185923A CN201610530251.XA CN201610530251A CN106185923A CN 106185923 A CN106185923 A CN 106185923A CN 201610530251 A CN201610530251 A CN 201610530251A CN 106185923 A CN106185923 A CN 106185923A
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porous carbon
nano material
carbon nano
matrix precursor
inorganic salt
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戴江栋
周志平
孙骏
何劲松
谢阿田
张瑞龙
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
    • B01J20/02—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
    • B01J20/205—Carbon nanostructures, e.g. nanotubes, nanohorns, nanocones, nanoballs
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/16—Pore diameter
    • C01P2006/17—Pore diameter distribution
    • 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

Abstract

The invention provides a kind of inorganic salt template auxiliary method preparing porous carbon nano material and application thereof, carry out as steps described below: step 1, the synthesis of carbon matrix precursor: in glucose solids, add solid sodium chloride, after grinding, obtain uniform mixture A；By mixture A under nitrogen protection, it is warming up to 450～500 DEG C and maintains 1h；It is cooled to room temperature after reaction, cleans product, obtain carbon matrix precursor after drying；Step 2, the preparation of porous carbon nano material: in carbon matrix precursor, add potassium hydroxide solid, after grinding, obtain uniform mixture B；By mixture B under nitrogen protection, it is warming up to 800～850 DEG C and maintains 1h；It is cooled to room temperature after reaction, cleans product, obtain porous carbon nano material after drying.The present invention is with glucose as carbon source, and raw material is easy to get, asepsis environment-protecting.

Description

A kind of inorganic salt template auxiliary method preparing porous carbon nano material and application thereof
Technical field
The present invention relates to a kind of inorganic salt template auxiliary method preparing porous carbon nano material and application thereof, belong to ring Border functional material preparing technical field.
Background technology
Methylene blue is a kind of typical high conjugation Cationic organic dyes, is widely used in manufacturing ink and color lake and life Thing, the field such as dyeing of bacterial organisms.But, methylene blue has certain bio-toxicity, enters in environment and can cause water body Pollute simultaneously, can carry out shifting and propagating and produce toxic effect in microorganism.Abuse methylene blue already leads to ecological environment In dangerous residual.Chinese scholars research has been proven that and there is methylene blue residual in soil and water environment, causes The extensive concern of environmental ecology.Therefore, set up and develop effective and economic and practical process means to the methylene removing in environment Base indigo plant residual is the most urgent.
Porous carbon materials refers to the carbon materials with Different Pore Structures, and it has from the nanoscale of equivalent molecules size super Fine holes is to the extensive aperture of the micron order pore being suitable to microorganism reproduction activity.Prepare mainly comprising the following steps of porous carbon materials: (1) material selecting suitably enrichment carbon is that raw material carries out carbonization；(2) carry out carbonized product activating drilling.Porous carbon Material has high-specific surface area and abundant pore volume, high temperature resistant, acid and alkali-resistance and good stability, and has real widely The property used.Porous carbon materials is widely used in the fields such as refined, the separation of gas and liquid, air cleaning.In recent years, more and more Researcher be devoted to the application during porous carbon materials is administered in water environment.
Owing to the preparation of porous carbon tradition uses traditional steam physical activation method, therefore there are some defects, such as: 1, Activation temperature is higher, and the material aperture prepared is undesirable, and absorbability is the highest；2, the productivity of porous carbon materials is low, is unfavorable for work Industry produces.In order to preferably solve the defect of conventional activation method, chemical activation method arises at the historic moment as a kind of new technology, i.e. adopts With activators such as potassium hydroxide, material with carbon element is carried out drilling.Use chemical activation method can reduce activation temperature, improve porous carbon The reference area of material and productivity.But, the method still has many technical barriers: such as corrosive equipment be easily generated chemical reagent Residual pollutes.
Potassium gluconate, as the typical small organic molecule of one, is widely used in the industries such as medicine, food, chemical industry. With glucose as carbon source, sodium chloride is hard mould agent, prepares porous carbon materials by carbonization and activation, and is used for adsorbing methylene Blue, it is achieved by the imagination of pollutant control pollutant, protect environment.
Summary of the invention
The present invention is first with glucose as carbon source, and sodium chloride is hard mould agent, makes glucose carbonization by calcining, after remove impurity Obtain carbonized product；Secondly, with potassium hydroxide as activator, carry out drilling modification on carbonized product surface, obtain many after remove impurity Hole carbon nanomaterial.By parameters such as multiple characterization method, the pattern of announcement material with carbon element and pore-size distributions.Utilize adsorption experiment The research resulting materials selective removal performance to water environment Methylene Blue.
The technical solution used in the present invention is:
A kind of method that inorganic salt template auxiliary prepares porous carbon nano material, is carried out as steps described below:
Step 1, the synthesis of carbon matrix precursor
In glucose solids, add solid sodium chloride, after grinding, obtain uniform mixture A；By mixture A at nitrogen Under protection, it is warming up to 450～500 DEG C and maintains 1h；It is cooled to room temperature after reaction, cleans product, before obtaining carbon after drying Drive body；
Step 2, the preparation of porous carbon nano material
In carbon matrix precursor, add potassium hydroxide solid, after grinding, obtain uniform mixture B；By mixture B at nitrogen Under protection, it is warming up to 800～850 DEG C and maintains 1h；It is cooled to room temperature after reaction, cleans product, obtain porous after drying Carbon nanomaterial, is designated as PCNM.
In step 1, glucose solids and solid sodium chloride mass ratio are 1:1.
In step 2, potassium hydroxide solid and carbon matrix precursor mass ratio are 0～4:1.
In step 1, described heating rate be 5 DEG C per minute, in step 2, described heating rate is 5～10 DEG C every point Clock；Step 1, in 2, the method for described cleaning product is: cleans reaction with 2mol/L hydrochloric acid, second alcohol and water successively and produces Thing；Step 1, in 2, described being dried is at 50～60 DEG C vacuum drying.
Prepared porous carbon nano material methylene blue in adsorbed water body.
Beneficial effect:
(1) present invention is with glucose as carbon source, and raw material is easy to get, asepsis environment-protecting.
(2) present invention is with sodium chloride as hard mould agent, and the porous carbon of preparation has two-dimensional sheet structure, and shape is unique.
(3) porous carbon materials prepared has higher specific surface area and pore volume.
(4) porous carbon materials prepared can efficiently remove the methylene blue in sewage.
(5) preparation method of the present invention is simple, production procedure is shorter, simple operation, easy to spread.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of PCNM；
Fig. 2 is the transmission electron microscope picture of PCNM；
Fig. 3 is nitrogen adsorption desorption figure (figure a) and the graph of pore diameter distribution (figure b) of PCNM；
Fig. 4 is the isollaothermic chart of PCNM absorption methylene blue；
Fig. 5 is the kinetics figure of PCNM absorption methylene blue；
Fig. 6 is the comparison diagram of the methylene blue of the different pH of PCNM absorption.
Detailed description of the invention
Below in conjunction with being embodied as example, the present invention will be further described:
Embodiment 1
(1) synthesis of carbon matrix precursor
In glucose solids, add solid sodium chloride, after grinding, obtain uniform mixture；By said mixture at nitrogen Under gas shielded, rise to 450 DEG C with 5 DEG C of speed per minute and maintain 1h；It is cooled to room temperature after reaction, cleans product, dry Carbon matrix precursor is obtained after dry.
Further, glucose solids and solid sodium chloride mass ratio are 1:1, milling time at least 10min.
Further, cleaning product and refer to clean product successively with dilute hydrochloric acid, second alcohol and water, dilute hydrochloric acid concentration is 2mol/L.It is dried and refers to be vacuum dried at 50-60 DEG C.
(2) preparation of porous carbon nano material
In carbon matrix precursor, add potassium hydroxide solid, after grinding, obtain uniform mixture；By said mixture at nitrogen Under gas shielded, rise to 850 DEG C with 5 DEG C of speed per minute and maintain 1h；It is cooled to room temperature after reaction, cleans product, dry Porous carbon nano material (PCNM) is obtained after dry.
Further, carbon matrix precursor and potassium hydroxide solid masses are than for 1:4, milling time at least 10min.
Further, cleaning product and refer to clean product successively with dilute hydrochloric acid, second alcohol and water, dilute hydrochloric acid concentration is 2mol/L, is dried and refers to be vacuum dried at 50-60 DEG C.
Embodiment 2
(1) synthesis of carbon matrix precursor
In glucose solids, add solid sodium chloride, after grinding, obtain uniform mixture；By said mixture at nitrogen Under gas shielded, rise to 450 DEG C with 5 DEG C of speed per minute and maintain 1h；It is cooled to room temperature after reaction, cleans product, dry Carbon matrix precursor is obtained after dry.
Further, glucose solids and solid sodium chloride mass ratio are 1:1, milling time at least 10min.
Further, cleaning product and refer to clean product successively with dilute hydrochloric acid, second alcohol and water, dilute hydrochloric acid concentration is 2mol/L, is dried and refers to be vacuum dried at 50-60 DEG C.
(2) preparation of porous carbon nano material
In carbon matrix precursor, add potassium hydroxide solid, after grinding, obtain uniform mixture；By said mixture at nitrogen Under gas shielded, rise to 800 DEG C with 10 DEG C of speed per minute and maintain 1h；It is cooled to room temperature after reaction, cleans product, dry Porous carbon nano material (PCNM) is obtained after dry.
Further, carbon matrix precursor and potassium hydroxide solid masses are than for 1:4, milling time at least 10min.
Further, cleaning product and refer to clean product successively with dilute hydrochloric acid, second alcohol and water, dilute hydrochloric acid concentration is 2mol/L, is dried and refers to be vacuum dried at 50-60 DEG C.
Embodiment 3
(1) synthesis of carbon matrix precursor
In glucose solids, add solid sodium chloride, after grinding, obtain uniform mixture；By said mixture at nitrogen Under gas shielded, rise to 450 DEG C with 5 DEG C of speed per minute and maintain 1h；It is cooled to room temperature after reaction, cleans product, dry Carbon matrix precursor is obtained after dry.
Further, glucose solids and solid sodium chloride mass ratio are 1:1, milling time at least 10min.
Further, cleaning product and refer to clean product successively with dilute hydrochloric acid, second alcohol and water, dilute hydrochloric acid concentration is 2mol/L, is dried and refers to be vacuum dried at 50-60 DEG C.
(2) preparation of porous carbon nano material
In carbon matrix precursor, add potassium hydroxide solid, after grinding, obtain uniform mixture；By said mixture at nitrogen Under gas shielded, rise to 850 DEG C with 5 DEG C of speed per minute and maintain 1h；It is cooled to room temperature after reaction, cleans product, dry Porous carbon nano material (PCNM) is obtained after dry.
Further, carbon matrix precursor and potassium hydroxide solid masses are than for 1:x (x=0,1,2,3,4), and milling time is at least 10min。
Further, cleaning product and refer to clean product successively with dilute hydrochloric acid, second alcohol and water, dilute hydrochloric acid concentration is 2mol/L, is dried and refers to be vacuum dried at 50-60 DEG C.
2, below in conjunction with being embodied as example, the present invention will be further described:
In the present invention, in specific embodiments, absorption property evaluation is carried out by the following method: utilize Staticadsorption experiment complete Become.The methylene blue solution of 10mL variable concentrations is joined in centrifuge tube, is added thereto to 3.0mg PCNM (carbonization temperature respectively Spend 500 DEG C, activation temperature 850 DEG C, carbon matrix precursor and potassium hydroxide mass ratio 1:4), water bath with thermostatic control stands, has investigated solution PH value, adsorbent amount, time of contact, the temperature impact on methylene blue adsorption number.Absorption reach saturated after, pass through Magnetic Isolation Collect, obtain clear liquid at the middle and upper levels, record methylene blue molecular concentration not to be adsorbed in test solution with ultraviolet-visible photometer, meter Calculation obtains adsorption capacity (Qe)。
Q e = ( C 0 - C e ) V m
Wherein C0And C (mg/L)e(mg/L) being initial and equilibrium concentration respectively, m (mg) is adsorbent amount, and V (mL) is molten Liquid amasss.
Experimental example 1: take 10ml initial concentration be respectively 50,100,120,150,180,200,250, the methylene of 300mg/L Base indigo plant solution joins in centrifuge tube, is separately added into 3.0mg PCNM (carburizing temperature 500 DEG C, activation temperature 850 DEG C, carbon forerunner Body and potassium hydroxide mass ratio 1:4), after test fluid is placed in 298K water-bath standing 12.0h, it is clear that upper strata is collected in centrifugation Liquid, methylene blue molecular concentration ultraviolet-uisible spectrophotometer not to be adsorbed measures, and calculates absorption appearance according to result Amount.Fig. 4 result shows: along with temperature and the rising of concentration, adsorbance is gradually increased, and is finally reached adsorption equilibrium.
Experimental example 2: take the methylene blue solution that 10ml initial concentration is 50mg/L and join in centrifuge tube, be separately added into 3.0mg PCNM (carburizing temperature 500 DEG C, activation temperature 850 DEG C, carbon matrix precursor and potassium hydroxide mass ratio 1:4), test fluid It is placed in the water-bath of 298K and stands 5,10,20,30,45,60,90,120,150,180,240,300 and 360 minutes respectively.Stand After completing, the centrifugal collection supernatant, methylene blue molecular concentration ultraviolet-uisible spectrophotometer not to be adsorbed measures, and Adsorption capacity is calculated according to result.Fig. 5 result shows, and: PCNM has a preferable adsorption dynamics adsorption kinetics performance to methylene blue, 300 points Adsorption equilibrium is basically reached in clock.
Experimental example 3: selecting dilute hydrochloric acid, sodium hydroxide is solution acid-base modifier.Respectively preparation pH be 2.0,4.0,6.0, 7.0,8.0,10.0,12.0, solubility is the methylene blue solution of 200mg/L.Take the solution that 10ml prepares and join centrifuge tube In, be separately added into 3.0mg PCNM (carburizing temperature 500 DEG C, activation temperature 850 DEG C, carbon matrix precursor and potassium hydroxide mass ratio 1: 4), test fluid is placed in the water-bath of 298K stands 14h respectively.Absorption reach saturated after, centrifugal collect the supernatant, do not inhaled Attached methylene blue concentration Uv-vis measures.Fig. 6 result shows, PCNM to the absorption property of methylene blue neutral and alkaline Under the conditions of comparatively acidic condition the most superior.
Fig. 1 is the scanning electron microscope (SEM) photograph of PCNM.PCNM shows as two-dimensional sheet material as we know from the figure, and rough surface is uneven, Size is relatively uniform.
Fig. 2 is the transmission electron microscope picture of PCNM.As can be seen from the figure PCNM rough surface is uneven, present a series of irregularly Duct, and there is higher specific surface area, be conducive to absorption.
Fig. 3 is nitrogen adsorption desorption figure (figure a) and the graph of pore diameter distribution (figure b) of PCNM.The nitrogen of PCNM is understood from Fig. 3 a Adsorption/desorption curve belongs to I type curve；The duct understanding PCNM from Fig. 3 b is mainly distributed on 1.5-3.5nm, shows in PCNM Duct is made up of micropore.
Fig. 4 is the isollaothermic chart of PCNM absorption methylene blue.It can be seen that along with temperature and the rising of concentration, absorption Amount increases.PCNM shows the separating property good to methylene blue, illustrates that micropore can be good at sub-present in PCNM Methyl blue interaction of molecules.
Fig. 5 is the kinetics figure of PCNM absorption methylene blue.It can be seen that initially, along with the increase of time of contact, inhale Attached amount increases sharply；Balance is slowly reached after 100 minutes.In whole time range, PCNM shows methylene blue Quick adsorption equilibrium.
Fig. 6 is the comparison diagram of the methylene blue of the different pH of PCNM absorption.It can be seen that in neutral and alkaline conditions, PCNM is more than adsorbance in acid condition to the adsorbance of dye of positive ion methylene blue, shows that PCNM is more suitable in neutrality With under the conditions of alkalescence, methylene blue is carried out adsorbing separation.

Claims (5)

1. the method preparing porous carbon nano material by inorganic salt template auxiliary, it is characterised in that enter as steps described below OK:
Step 1, the synthesis of carbon matrix precursor
In glucose solids, add solid sodium chloride, after grinding, obtain uniform mixture A；Mixture A is protected at nitrogen Under, it is warming up to 450～500 DEG C and maintains 1h；It is cooled to room temperature after reaction, cleans product, obtain carbon matrix precursor after drying；
Step 2, the preparation of porous carbon nano material
In carbon matrix precursor, add potassium hydroxide solid, after grinding, obtain uniform mixture B；Mixture B is protected at nitrogen Under, it is warming up to 800～850 DEG C and maintains 1h；It is cooled to room temperature after reaction, cleans product, obtain porous carbon after drying and receive Rice material.
The method that a kind of inorganic salt template auxiliary the most according to claim 1 prepares porous carbon nano material, its feature Being, in step 1, glucose solids and solid sodium chloride mass ratio are 1:1.
The method that a kind of inorganic salt template auxiliary the most according to claim 1 prepares porous carbon nano material, its feature Being, in step 2, potassium hydroxide solid and carbon matrix precursor mass ratio are 0～4:1.
The method that a kind of inorganic salt template auxiliary the most according to claim 1 prepares porous carbon nano material, its feature Be, in step 1, described heating rate be 5 DEG C per minute, in step 2, described heating rate be 5～10 DEG C per minute； Step 1, in 2, the method for described cleaning product is: clean product successively with 2mol/L hydrochloric acid, second alcohol and water；Step In rapid 1,2, described being dried is at 50～60 DEG C vacuum drying.
5. the purposes of the porous carbon nano material that prepared by the method described in Claims 1 to 4 any one, it is characterised in that institute The porous carbon nano material of preparation methylene blue in adsorbed water body.
CN201610530251.XA 2016-07-06 2016-07-06 A kind of inorganic salt template auxiliary method preparing porous carbon nano material and application thereof Pending CN106185923A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107159115A (en) * 2017-05-31 2017-09-15 宁夏大学 A kind of porous carbon prepared by template of sodium chloride for adsorbing methylene blue
CN108529596A (en) * 2018-07-20 2018-09-14 广东工业大学 A kind of preparation method of dimensional thinlayer carbon
CN108649242A (en) * 2018-03-21 2018-10-12 南京师范大学 The preparation method and its resulting materials of a kind of porous Pt nanometer sheets of two dimension and application
CN110078051A (en) * 2019-04-30 2019-08-02 济宁学院 The preparation method of nano cages material
CN114058246A (en) * 2021-12-31 2022-02-18 常州市华菱新材料有限公司 High-strength corrosion-resistant water-based epoxy coating and preparation method thereof

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CN103601185A (en) * 2013-12-05 2014-02-26 天津工业大学 Preparation method of spherical porous carbon for super capacitors
CN103663448A (en) * 2012-09-19 2014-03-26 天津普兰纳米科技有限公司 Preparation method of carbon material, obtained carbon material and application thereof
CN105502386A (en) * 2015-12-17 2016-04-20 中北大学 Preparation method of microporous carbon nanosheets

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Publication number Priority date Publication date Assignee Title
WO2012125839A1 (en) * 2011-03-15 2012-09-20 University Of Kentucky Research Foundation Carbon particles
CN103663448A (en) * 2012-09-19 2014-03-26 天津普兰纳米科技有限公司 Preparation method of carbon material, obtained carbon material and application thereof
CN103601185A (en) * 2013-12-05 2014-02-26 天津工业大学 Preparation method of spherical porous carbon for super capacitors
CN105502386A (en) * 2015-12-17 2016-04-20 中北大学 Preparation method of microporous carbon nanosheets

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107159115A (en) * 2017-05-31 2017-09-15 宁夏大学 A kind of porous carbon prepared by template of sodium chloride for adsorbing methylene blue
CN108649242A (en) * 2018-03-21 2018-10-12 南京师范大学 The preparation method and its resulting materials of a kind of porous Pt nanometer sheets of two dimension and application
CN108529596A (en) * 2018-07-20 2018-09-14 广东工业大学 A kind of preparation method of dimensional thinlayer carbon
CN108529596B (en) * 2018-07-20 2021-11-26 广东工业大学 Preparation method of two-dimensional thin-layer carbon
CN110078051A (en) * 2019-04-30 2019-08-02 济宁学院 The preparation method of nano cages material
WO2020220591A1 (en) * 2019-04-30 2020-11-05 济宁学院 Preparation method for carbon nanocage material
CN114058246A (en) * 2021-12-31 2022-02-18 常州市华菱新材料有限公司 High-strength corrosion-resistant water-based epoxy coating and preparation method thereof

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Application publication date: 20161207