CN106311147A - Illite loaded nanocarbon compound adsorbing material and preparation method thereof - Google Patents
Illite loaded nanocarbon compound adsorbing material and preparation method thereof Download PDFInfo
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- CN106311147A CN106311147A CN201610900682.0A CN201610900682A CN106311147A CN 106311147 A CN106311147 A CN 106311147A CN 201610900682 A CN201610900682 A CN 201610900682A CN 106311147 A CN106311147 A CN 106311147A
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- illite
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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
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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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
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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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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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
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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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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Abstract
The invention relates to an illite loaded nanocarbon compound adsorbing material and a preparation method thereof and belongs to the field of non-metallic mineral material and environmental engineering. According to the invention, illite is taken as a carrier, soluble saccharide is taken as a carbon source and nanocarbon grains are uniformly loaded on the surface of an illite layer, so that the nanocarbon compound adsorbing material taking illite as the carrier is obtained. In the prepared illite loaded nanocarbon compound adsorbing material, the average grain diameter of the nanocarbon grains is 30-50nm, the nanocarbon grains are uniformly and compactly distributed on the surface of the illite layer and the load volume is 30%-70% of the mass of the compound material. According to the material, the illite carrier effect is utilized to increase the adsorbing capturing performance of the compound material to the pollutant and the dispersity of the adsorbent; the obtained raw materials are easily acquired and are low in cost; the preparation technique is simple and the reaction condition is mild; the illite loaded nanocarbon compound adsorbing material has higher application value in the field of wastewater treatment.
Description
Technical field
The present invention relates to a kind of illite load Nano Carbon adsorbing material and preparation method thereof, belong to nonmetallic mineral
Material and field of environment engineering.
Background technology
Society, waste water pollution problem is increasingly severe.In some areas, contaminated wastewater heavy damage ecology
Balance, directly threatens the existence of the mankind.Traditional pollutant effluents treatment technology includes chemical precipitation method, ion exchange, film
Osmosis and coprecipitation etc..But these methods generally also exist, and operating cost is high, treatment effeciency is low and reuses difficulty etc.
Problem, it is impossible to realize industrial applications.Absorption method has the advantages such as operating process is easy, disposal ability is big, can reuse,
It it is a kind of preferably wastewater processing technology.The active charcoal of common sorbent material, biomass, clay mineral and synthetic resin
Deng.Absorbent charcoal material is owing to having excellent absorption property, bigger specific surface area, flourishing space and higher chemically stable
Property, it is a kind of most popular sorbent material.But absorbent charcoal material typically uses chemical gaseous phase deposition and pyrolytic etc.
Prepared by method, there is the shortcomings such as preparation process is complicated, energy consumption is high.The price comparison causing merchandise active carbon is high, and owing to making
The problems such as short, difficult for regeneration with the life-span in operating cost is high, it is impossible to use the most on a large scale.Additionally, pure carbon nano-particle
Particle diameter is less, difficult separation and recycling；Surface can be high, is susceptible to reunite, affects its absorption property.
In order to overcome disadvantage mentioned above, nano carbon particle, with mineral as template vector, is loaded to carrier table by researcher
Face is prepared as mineral loaded Nano Carbon adsorbing material.
Document H.Hadjar, B.Hamdi, C.O.Ania, Adsorption of p-cresol on novel
Diatomite/carbon composites, Journal of hazardous materials, 2011,188:304-310.
With kieselguhr as carrier, Linesless charcoal is carbon source, first the two is mixed, is warmed up to the heating rate of 5 DEG C/min under nitrogen atmosphere
850 DEG C carry out heat treatment 1h；Then heat-treated products use hydrochloric acid carry out chemical treatment；Finally with distilled water, sample is washed
To neutral, at 110 DEG C, it is dried overnight prepared tripolite loading nano carbon composite.Carbon source itself used in this method
It is exactly a kind of chemical products, expensive raw material price；Using 850 DEG C of high temperature to carry out heat treatment, severe reaction conditions, energy consumption is high；System
Also using the hydrochloric acid of high concentration during Bei, operating environment is dangerous, serious to equipment corrosion in commercial production, acid treatment sample
Need to use a large amount of distilled water wash, and the Cl in waste liquid-Being difficult to process, environmental pollution is serious；Whole technological process is complicated,
Severe reaction conditions.
The deficiency existed for above-mentioned mineral loaded Nano Carbon adsorbing material and preparation method thereof, the present patent application carries
Go out a kind of illite with illite as carrier load Nano Carbon adsorbing material and preparation method thereof.Illite is a kind of 2:
The natural layered silicate mineral of 1 type, have ion exchange property and absorbability, its microscopic appearance in the form of sheets, this thin slice
Shape structure has bigger specific surface area, is advantageous to the load of nano carbon particle, it is to avoid the reunion of pure carbon granule, and raising is received
The load capacity of rice carbon granule.And illite source is wide, production cost is low, use process environmentally friendly.Hydrothermal carbonization method is
Mixture is carried out in form of an aqueous solutions in hermetic container, only needs a step Hydrothermal Synthesis, and preparation technology is easy, reaction condition temperature
With.Therefore, this composite adsorbent material has a good application prospect.
Summary of the invention
The technical scheme is that, with illite as carrier, soluble saccharide is carbon source, by hydrothermal carbonization method at her
Profit flag layer area load nano-sized carbon, prepares a kind of illite load Nano Carbon efficient absorption material.
Loading Nano Carbon adsorbing material with the illite prepared by the present invention, nano carbon particle mean diameter is 30-
50nm, distribution uniform in illite sheet surfaces, fine and close, nano carbon particle load capacity is the 30%-70% of composite quality.
Its preparation method and processing step are as follows:
(1) illite and carbon source 1:1-4 in mass ratio being mixed, mixing suspension, suspension are made in the stirring that adds water, dispersion
Concentration is 5%-15%；Described illite is flaky texture, and described carbon source is soluble saccharide, as glucose, sucrose,
Cellulose, starch etc..
(2) gained mixing suspension in step (1) is transitioned in autoclave, at 160-220 DEG C of Water Under
Thermal response 12-24h；
(3) by gained product ethanol in step (2) and water washing and filtering, after at 60 DEG C, be dried 12h；
(4) gained in step (3) is dried product and be ground to 97% by 200 mesh sieves.I.e. obtain described illite to bear
Carry Nano Carbon adsorbing material.
The present invention utilizes illite carrier effect and stronger absorbability to improve composite and catches pollutant absorption
Catch the dispersibility of performance and adsorbent, solve the agglomeration traits of pure carbon granule；Illite sheet-like morphology is utilized to have bigger
Specific surface area, improves the load capacity of nano-sized carbon；And needed raw material is cheap and easy to get, preparation technology is simple, reaction condition is gentle,
In field of waste water treatment, there is bigger using value.
Accompanying drawing explanation
Fig. 1 is laminar illitic SEM figure in the present invention.
Fig. 2 is the SEM of the illite load Nano Carbon adsorbing material in the present invention prepared by with illite as carrier
Figure.
Fig. 3 is the TG of the illite load Nano Carbon adsorbing material in the present invention prepared by with illite as carrier
Figure.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further illustrated.But not limitation of the present invention, all according to
The equivalent of any this area that present invention is done, belongs to protection scope of the present invention.
Embodiment 1:
It is embodied as step as follows:
(1) take 2.5g illite and 2.5g glucose is placed in 50mL water dispersion 30min, configure mixing suspension；
(2) transitioning in autoclave by gained mixing suspension in step (1), under the conditions of 160 DEG C, hydro-thermal is anti-
Answer 24h；
(3) by gained product ethanol in step (2) and water washing and filtering, after at 60 DEG C, be dried 12h；
(4) gained drying product in step (3) is ground to 97% and passes through 200 mesh sieves, obtain illite load nano-sized carbon
Composite adsorbing material.
SEM and the TG figure of the illite load Nano Carbon adsorbing material of embodiment 1 preparation is shown in accompanying drawing 2 and 3.By Fig. 2
Understanding, illite sheet surfaces has loaded nano carbon particle equably, and its mean diameter is 30-50nm；From the figure 3, it may be seen that it is compound
In material, the load capacity of nano-sized carbon is 32.77%.
Embodiment 2:
Identical with step in embodiment 1, difference is: in step (1), sucrose addition is 5.0g, uses 60mL moisture
Dissipate；In step (2), reaction temperature is 180 DEG C, and the response time is 20h；
Embodiment 3:
Identical with step in embodiment 1, difference is: in step (1), starch addition is 7.5g, uses 70mL moisture
Dissipate；In step (2), reaction temperature is 200 DEG C, and the response time is 16h；
Embodiment 4:
Identical with step in embodiment 1, difference is: in step (1), cellulose addition is 10.0g, uses 80mL
Water-dispersible；In step (2), reaction temperature is 220 DEG C, and the response time is 12h；
Method as described below, tests and calculates performance and the parameter of final products in embodiment 1 to 4, gained
The results are shown in Table 1.
The absorption property of effluent containing heavy metal ions Cr (VI) measures: Cr VI (Cr (VI)) is listed in all heavy metal ion
In primary pollutant.Therefore, selected Cr (VI) is as target contaminant, the adsorptivity of test sample heavy metal ion waste water
Energy.Sample is the biggest to the adsorption capacity of Cr (VI) under given conditions, illustrates that its absorption property is the best.This detailed description of the invention
In, the concentration of Cr used (VI) solution is 50mg/L, takes Cr (VI) solution and the 0.025g Product mix of 20ml, in room temperature every time
Under the conditions of stirring reaction 12h.Sample with centrifuge tube after having reacted, after high speed centrifugation, take supernatant on spectrophotometer
Survey absorbance at 258.2nm wavelength, then the clearance computing formula of Cr (VI) solution is: clearance=(C0-Ce)/C0×
100%, C in formula0For the absorbance of initial Cr (VI) solution, CeThe absorbance of Cr (VI) solution during for having reacted.
The absorption property of organic wastewater methylene blue measures: using methylene blue as target contaminant, test sample is to having
The absorption property of machine waste water.In this detailed description of the invention, the absorption property of method and above-mentioned heavy metal ion Cr (VI) measures phase
With.Methylene blue concentration 250mg/L used, surveys absorbance on spectrophotometer at 664nm wavelength.
The load capacity of nano-sized carbon calculates: owing to carbon source added in course of reaction all can not be deposited to her by hydrothermal carbonization
Profit stone sheet surfaces, causes the actual nano-sized carbon load capacity of product to be less than its theoretical value calculated according to the amount adding carbon source.
Therefore, METTLER TGA/DSC 1 SF/1382 thermogravimetric analyzer is used to detect the actual negative carrying capacity of nano-sized carbon in sample.This
In detailed description of the invention, under nitrogen atmosphere, drying sample is increased to 1000 DEG C with the heating rate of 5 DEG C/min from room temperature.
The load capacity of nano-sized carbon is the mass change of 300-600 DEG C of temperature range.
The performance of final products and parameter in table 1 embodiment 1 to 4
Claims (4)
1. an illite load Nano Carbon adsorbing material, i.e. at illite sheet surfaces uniform load nano carbon particle,
It is characterized in that: described nano carbon particle mean diameter is 30-50nm, distribution uniform in illite sheet surfaces, fine and close；Institute
The 30%-70% that nano carbon particle load capacity is composite quality stated.
2. the method preparing a kind of illite load Nano Carbon adsorbing material described in claim 1, with Erie
Stone is carrier, and soluble saccharide is carbon source, loads nano-sized carbon by hydrothermal carbonization method in illite sheet surfaces, including following work
Skill step:
(1) illite and carbon source 1:1-4 in mass ratio being mixed, mixing suspension, suspension concentration are made in the stirring that adds water, dispersion
For 5%-15%；
(2) transitioning in autoclave by gained mixing suspension in step (1), under the conditions of 160-220 DEG C, hydro-thermal is anti-
Answer 12-24h；
(3) by gained product ethanol in step (2) and water washing and filtering, after at 60 DEG C, be dried 12h；
(4) gained drying product in step (3) is ground to 97% and passes through 200 mesh sieves, i.e. obtain illite load nano-sized carbon multiple
Close adsorbing material.
The preparation method of a kind of illite the most according to claim 2 load Nano Carbon adsorbing material, its feature exists
In: described illite is flaky texture.
The preparation method of a kind of illite the most according to claim 2 load Nano Carbon adsorbing material, its feature exists
In: described carbon source is soluble saccharide, such as glucose, sucrose, cellulose, starch etc..
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Cited By (6)
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| CN108423799A (en) * | 2018-03-29 | 2018-08-21 | 上海工程技术大学 | A kind of bio-carrier and preparation method thereof for biofilter |
| CN110496599A (en) * | 2019-07-25 | 2019-11-26 | 南方科技大学 | composite adsorbent and preparation method and application thereof |
| CN110591716A (en) * | 2018-06-13 | 2019-12-20 | 岳西县九方农业有限公司 | Stabilization repair material suitable for heavy metal pollution of tailing waste stone and preparation method |
| CN110665457A (en) * | 2019-09-30 | 2020-01-10 | 广西民族大学 | Sucrose carbide/sepiolite composite material and preparation method thereof |
| CN110665459A (en) * | 2019-09-30 | 2020-01-10 | 广西民族大学 | Starch carbide/sepiolite composite material and preparation method thereof |
| CN110665458A (en) * | 2019-09-30 | 2020-01-10 | 广西民族大学 | Glucose carbide/sepiolite composite material and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108423799A (en) * | 2018-03-29 | 2018-08-21 | 上海工程技术大学 | A kind of bio-carrier and preparation method thereof for biofilter |
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| CN110591716A (en) * | 2018-06-13 | 2019-12-20 | 岳西县九方农业有限公司 | Stabilization repair material suitable for heavy metal pollution of tailing waste stone and preparation method |
| CN110496599A (en) * | 2019-07-25 | 2019-11-26 | 南方科技大学 | composite adsorbent and preparation method and application thereof |
| CN110496599B (en) * | 2019-07-25 | 2022-08-23 | 南方科技大学 | Composite adsorbent and preparation method and application thereof |
| CN110665457A (en) * | 2019-09-30 | 2020-01-10 | 广西民族大学 | Sucrose carbide/sepiolite composite material and preparation method thereof |
| CN110665459A (en) * | 2019-09-30 | 2020-01-10 | 广西民族大学 | Starch carbide/sepiolite composite material and preparation method thereof |
| CN110665458A (en) * | 2019-09-30 | 2020-01-10 | 广西民族大学 | Glucose carbide/sepiolite composite material and preparation method thereof |
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