CN108126677A - A kind of preparation method of carbon composite for Acid Dye Wastewater processing - Google Patents
A kind of preparation method of carbon composite for Acid Dye Wastewater processing Download PDFInfo
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- CN108126677A CN108126677A CN201711452924.5A CN201711452924A CN108126677A CN 108126677 A CN108126677 A CN 108126677A CN 201711452924 A CN201711452924 A CN 201711452924A CN 108126677 A CN108126677 A CN 108126677A
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- carbon composite
- porous charcoal
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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
- B01J20/26—Synthetic macromolecular compounds
- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
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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
- B01J20/28—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
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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
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
-
- 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 discloses a kind of preparation methods of the carbon composite for Acid Dye Wastewater processing, belong to technical field of carbon material preparation.For this method first using coal tar pitch as carbon source, nano magnesia is template, and after potassium hydroxide prepares the porous charcoal with a large amount of central hole structures for activator, acidification is carried out to porous carbon surface using concentrated nitric acid；Simultaneously using ethylenediamine, methyl acrylate and methanol as raw material, the polyamide-amine dendrimer in 2.0 generations is prepared using " one kettle way ", finally by the porous charcoal after acidification and daiamid obtained with mass ratio 4：1 to 6：Carbon composite of the drying to obtain mesoporous carbon surface rich in daiamid after several hours is mixed in 1 ratio in 35 DEG C of aqueous solutions.Carbon composite prepared by the present invention is raw materials used cheap, derives from a wealth of sources, and has the characteristics that simple for process, and the carbon composite shows the acid dyes in waste water excellent adsorbing and removing performance.
Description
Technical field
The invention belongs to technical field of sewage, and in particular to a kind of compound raw material of wood-charcoal for Acid Dye Wastewater processing
The preparation method of material,
Background technology
According to statistics, still there are nearly 100,000 kinds of different dyestuffs in China by production application every year, is often close on 1600000 tons of dyestuff quilt
It produces and uses, 10%~15% amount cannot be utilized completely to be directly discharged in rivers and lakes, often discharges 1t waste water from dyestuff, just
20t water bodys can be polluted.Waste water from dyestuff has become one of major polluting sources of water system environment.If this kind of waste water cannot have in time
The processing of effect, high causing toxicity dyestuff contaminant will enter body of groundwater, not only ecological environment and human health be generated bad
It influences, directly endangers the health of the mankind, seriously destroy water body, soil and ecological environment；Therefore, with the environmental consciousness of people
How constantly enhancing, effectively administer waste water from dyestuff, receive more and more attention in recent years.Processing waste water from dyestuff is commonly used both at home and abroad
Method have Physical, chemical method and bioanalysis.Absorption method due to easy to operate, have can at normal temperatures and pressures efficient concentration it is low
The excellent performance of concentration pollutant is also used widely in waste water from dyestuff improvement.Adsorbent is the core of adsorption technology,
The adsorbent for being studied for waste water from dyestuff improvement at present includes activated carbon, polymer, nano-metal-oxide, molecular sieve etc.,
But the defects of presence or adsorption efficiency are low, capacity is small or the scope of application is small, reproducibility is poor, of high cost, it is therefore necessary to develop high property
Can adsorbent with meet waste water from dyestuff improvement needs.
Invention content
To overcome the shortcomings of existing adsorbent, the object of the present invention is to provide a kind of high-performance at Acid Dye Wastewater
The preparation method of the carbon composite of reason, to solve the prior art to waste water from dyestuff, particularly Acid Dye Wastewater decoloration is tired
Difficulty is unable to reach the technical barriers such as discharge standard.
The purpose of the present invention is what is be achieved by the following technical programs.
Of the invention to provide a kind of preparation method of the carbon composite for Acid Dye Wastewater processing, this method, which is directed to, divides
The larger-size acid dyes molecule of son, is made the porous charcoal containing a large amount of mesoporous, then gathers in porous charcoal surface graft first
Amide amine (PAMAM), finally obtained acid dyes adsorbent, is as follows：
(1) pretreatment of reactant：Coal tar pitch is put into mortar, nano magnesia is added in and is uniformly mixed, add and ground
To the potassium hydroxide of powder, three is uniformly mixed to obtain reactant.
Wherein：The mass ratio of the coal tar pitch and nano magnesia is between 1/10~2/1；The coal tar pitch and potassium hydroxide
Mass ratio between 1/2~1/4.
(2) preparation of porous charcoal：Reactant obtained by step (1) is put into corundum porcelain boat, and corundum porcelain boat is placed in
In tube furnace, the air in the tube furnace is emptied with the ventilation of the argon gas of flowing, then with the heating rate of 3 DEG C/min by tube furnace
200 DEG C, constant temperature 30min are warming up to, continues that tube furnace is warming up to 800~900 DEG C with the heating rate of 3 DEG C/min, it is warm herein
Room temperature is naturally cooling to after the lower constant temperature 60min of degree；After finally obtained product is taken out, ground, through chlorohydric acid pickling, distillation
Water is washed and obtains porous charcoal after dry.
(3) the surface acidification of porous charcoal：By the dense of the porous charcoal obtained by 1g steps (2) and 9mL mass concentrations 68%
Nitric acid, 6mL distilled water are placed in conical flask, and 3 hours of magnetic agitation, filter out solution, use distilled water under conditions of 60 DEG C
Porous charcoal after washing process, until neutrality is presented in solution, the porous charcoal after washing obtains the porous of surface acidification after drying
Charcoal.
The preparation of (4) 2.0 generation daiamids：First by 0.01 mole of ethylenediamine and 0.1 mole of absolute methanol successively
It adds in the three-necked flask of 250mL, 0.04 mole of methyl acrylate is slowly added dropwise under agitation, in 20 DEG C of reaction temperature
Under degree, 12h is reacted；Then 0.04 mole of ethylenediamine is directly added dropwise again and carries out amidation process, while add in 0.02 mole
Absolute methanol, under 20 DEG C of reaction temperature, reaction obtains the absolute methanol solution of 1.0 generation PAMAM for 24 hours, under agitation,
0.08 mole of methyl acrylate is slowly added dropwise, under 20 DEG C of reaction temperature, reacts 12h；Then 0.08 mole is added dropwise again
Ethylenediamine carries out amidation process, while adds in 0.04 mole of absolute methanol, under 30 DEG C of reaction temperature, reacts 12h, most
Vacuum distillation removes absolute methanol afterwards, obtains 2.0 generation polyamide-amine dendrimers.
(5) preparation of carbon composite：By the porous charcoal that the surface of gained in step (3) is acidified and gained in step (4)
The mixing of 2.0 generation daiamids, add in the deionized water of 40mL, cleaned after ultrasonic disperse, be dried to obtain carbon composite；It is described
The porous charcoal of surface acidification and the mass ratio of 2.0 generation daiamids are 4/1~6/1.
Further, in step (1), the quality of the coal tar pitch is 2g, and the quality of the nano magnesia is 19g,
The quality of the potassium hydroxide is 6g；In step (2), the diamond heating final temperature is 850 DEG C.
Further, in step (3), the drying is freeze-day with constant temperature.
Further, in step (5), the drying is vacuum drying.
Compared with prior art, the present invention has following technique effect：
1. using coal tar pitch as carbon source, carbon material abundance is cheap.
2. the porous charcoal prepared is conducive to the diffusion and suction of the larger dye molecule of molecular dimension rich in a large amount of mesoporous
It is attached.
It, can effective and acid dyes molecule shape 3. a large amount of polyamide-amine dendrimer is contained on carbon composite surface
Into chemisorbed, excellent absorption property is shown to acid dyes.
4. the porous charcoal of acidification can be mixed directly with the less PAMAM of dosage can be prepared by carbon composite, there is work
Skill is simple, it is at low cost the advantages that.
Description of the drawings
Fig. 1 is the nitrogen Adsorption and desorption isotherms figure of carbon composite prepared by the embodiment of the present invention 1,2,3.
Fig. 2 is the graph of pore diameter distribution of carbon composite prepared by the embodiment of the present invention 1,2,3.
Fig. 3 is the adsorption isotherm that carbon composite prepared by the embodiment of the present invention 1,2,3 adsorbs acid orange.
Specific embodiment
The present invention is described in detail, but the present invention is not limited to following embodiments below in conjunction with specific embodiment.
Embodiment 1
The specific preparation process of carbon composite PC4 is as follows：
(1) pretreatment of reactant：It weighs 6g potassium hydroxide and is put into mortar and be ground to powdered, weigh 19g nano oxygens
Change magnesium, weigh 2g coal tar pitch and mixed with potassium hydroxide, be uniformly mixed, obtain reactant.
(2) preparation of porous charcoal：The reactant pre-processed in step (1) is put into corundum porcelain boat, then by Corundum Ceramics
Boat is put into tube furnace, and leading to argon gas 20min in advance with the air velocity of 120ml/min drains air in tube furnace, Ran Hou
Under the argon gas atmosphere of 20ml/min, with the heating rate of 3 DEG C/min by diamond heating to 200 DEG C, constant temperature 30min continues with 3
DEG C/heating rate of min continues tube furnace to be heated to 850 DEG C, constant temperature 60min is naturally cooling to room temperature later.By obtained by
Product take out, product is placed in mortar after grinding and poured into beaker, prepare 2M hydrochloric acid pour into beaker, ultrasonic vibration
2h, then carried out pickling with magnetic stirrer 12h, standing 12h, then washed with hot distilled water to neutrality, clean charcoal is put
Enter drying in air dry oven and grind sieving for 24 hours, after taking-up, obtain porous charcoal.
(3) the surface acidification of porous charcoal：By the porous charcoal and concentrated nitric acid, the 6mL of 9mL68% obtained by 1g steps (2)
Distilled water is placed in conical flask, and 3 hours of magnetic agitation, filter out solution under conditions of 60 DEG C, with distilled water washing process
Porous charcoal afterwards, until neutrality is presented in solution, the porous charcoal after washing is 36 hours dry in constant temperature (110 DEG C) case, obtains table
The porous charcoal of face acidification.
The preparation of (4) 2.0 generation PAMAM：0.01 mole of ethylenediamine and 0.1 mole of absolute methanol are sequentially added first
In the three-necked flask of 250ml, 0.04 mole of methyl acrylate is slowly added dropwise under agitation, in 20 DEG C of reaction temperature
Under, react 12h；Then the ethylenediamine that molar ratio is 0.04 mole is directly added dropwise again and carries out amidation process, while addition mole
Than the absolute methanol for 0.02 mole, under 20 DEG C of reaction temperature, the absolute methanol that reaction obtains 1.0 generation PAMAM for 24 hours is molten
Under agitation, 0.08 mole of methyl acrylate is slowly added dropwise in liquid, under 20 DEG C of reaction temperature, reacts 12h；Then
0.08 mole of ethylenediamine is added dropwise again and carries out amidation process, while add in 0.04 mole of absolute methanol, in 30 DEG C of reaction
At a temperature of, 12h is reacted, finally vacuum distillation removes absolute methanol, obtains the polyamide-amine dendrimer (PAMAM) in 2.0 generations.
(5) preparation of carbon composite：The porous charcoal of gained in step (3) and the PAMAM of gained in step (4) are pressed into matter
Amount is than being 4：1 mixing adds in the deionized water of 40mL, ultrasonic disperse.12h is stirred at 35 DEG C, distilled water cleans 3 times, 60 DEG C
Carbon composite is obtained after vacuum drying.The carbon composite of gained is denoted as PC4.Acid orange is adsorbed with the material, in pH
Be worth be 3.2 under the conditions of, when equilibrium concentration be 30mg/L when, equilibrium adsorption capacity is up to 388mg/g.
Embodiment 2
The specific preparation process of carbon composite PC5 is as follows：
(1), the step of (2), (3), (4) step are with (1-4) in example 1,
The difference lies in:
(5) by the porous charcoal after acidification and PAMAM mass ratioes according to 5：1 mixing.The carbon composite of gained is denoted as PC5.
Acid orange is adsorbed with the material, under the conditions of pH value is 3.2, when acid orange equilibrium concentration is 25mg/L, adsorbance reaches
To 202mg/g.
Embodiment 3
The specific preparation process of carbon composite PC6 is as follows：
(1), the step of (2), (3), (4) step are with (1-4) in example 1,
The difference lies in:
(5) by the porous charcoal after acidification and PAMAM mass ratioes according to 6：1 mixing.The carbon composite of gained is denoted as PC6.
Acid orange is adsorbed with the material, under the conditions of pH value is 3.2, when acid orange equilibrium concentration is 45mg/L, adsorbance reaches
To 285mg/g.
Claims (4)
- A kind of 1. preparation method of carbon composite for Acid Dye Wastewater processing, it is characterised in that this method specific steps It is as follows：(1) pretreatment of reactant：Coal tar pitch is put into mortar, nano magnesia is added in and is uniformly mixed, add and be milled to powder The potassium hydroxide at end, three are uniformly mixed to obtain reactant；Wherein：The mass ratio of the coal tar pitch and nano magnesia is between 1/10~2/1；The matter of the coal tar pitch and potassium hydroxide Ratio is measured between 1/2~1/4；(2) preparation of porous charcoal：Reactant obtained by step (1) is put into corundum porcelain boat, and corundum porcelain boat is placed in tubular type In stove, the air in the tube furnace is emptied with the argon gas ventilation of flowing, then tube furnace heats up with the heating rate of 3 DEG C/min To 200 DEG C, constant temperature 30min, continue that tube furnace is warming up to 800~900 DEG C with the heating rate of 3 DEG C/min, at this temperature Room temperature is naturally cooling to after constant temperature 60min；After finally obtained product is taken out, ground, through chlorohydric acid pickling, distilled water water It washes and obtains porous charcoal after drying；(3) the surface acidification of porous charcoal：By the porous charcoal obtained by 1g steps (2) and the concentrated nitric acid of 9mL mass concentrations 68%, 6mL distilled water is placed in conical flask, and 3 hours of magnetic agitation, filter out solution under conditions of 60 DEG C, at distilled water washing Porous charcoal after reason, until neutrality is presented in solution, the porous charcoal after washing obtains the porous charcoal of surface acidification after drying；The preparation of (4) 2.0 generation daiamids：0.01 mole of ethylenediamine and 0.1 mole of absolute methanol are sequentially added first In the three-necked flask of 250mL, 0.04 mole of methyl acrylate is slowly added dropwise under agitation, in 20 DEG C of reaction temperature Under, react 12h；Then 0.04 mole of ethylenediamine is directly added dropwise again and carries out amidation process, while add in 0.02 mole of nothing Water methanol, under 20 DEG C of reaction temperature, reaction obtains the absolute methanol solution of 1.0 generation PAMAM for 24 hours, under agitation, delays The slow methyl acrylate for being added dropwise 0.08 mole under 20 DEG C of reaction temperature, reacts 12h；Then 0.08 mole of second is added dropwise again Diamines carries out amidation process, while adds in 0.04 mole of absolute methanol, under 30 DEG C of reaction temperature, reacts 12h, finally Vacuum distillation removes absolute methanol, obtains 2.0 generation polyamide-amine dendrimers；(5) preparation of carbon composite：By the porous charcoal that the surface of gained in step (3) is acidified and 2.0 of gained in step (4) It is mixed for daiamid, adds in the deionized water of 40mL, cleaned after ultrasonic disperse, be dried to obtain carbon composite；The surface The mass ratio of the porous charcoal of acidification and 2.0 generation daiamids is 4/1~6/1.
- 2. a kind of preparation method of carbon composite for Acid Dye Wastewater processing as described in claim 1, feature It is, in step (1), the quality of the coal tar pitch is 2g, and the quality of nano magnesia is 19g, and the quality of potassium hydroxide is 6g；In step (2), diamond heating final temperature is 850 DEG C.
- 3. a kind of preparation method of carbon composite for Acid Dye Wastewater processing as described in claim 1, feature It is, in step (3), the drying is freeze-day with constant temperature.
- 4. a kind of preparation method of carbon composite for Acid Dye Wastewater processing as described in claim 1, feature It is, in step (5), the drying is vacuum drying.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110075803A (en) * | 2019-06-03 | 2019-08-02 | 许皖 | A kind of preparation method of N doping Alkaline porous charcoal |
| CN112062127A (en) * | 2020-09-18 | 2020-12-11 | 华侨大学 | Coal-based nano porous carbon and preparation method thereof |
| CN113184847A (en) * | 2021-04-15 | 2021-07-30 | 安徽工业大学 | Porous carbon material and preparation method and application thereof |
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| CN113184847A (en) * | 2021-04-15 | 2021-07-30 | 安徽工业大学 | Porous carbon material and preparation method and application thereof |
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Application publication date: 20180608 |