CN107954424A - A kind of preparation method of wide spectrum superelevation adsorbance absorbent charcoal material - Google Patents
A kind of preparation method of wide spectrum superelevation adsorbance absorbent charcoal material Download PDFInfo
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- CN107954424A CN107954424A CN201810026961.8A CN201810026961A CN107954424A CN 107954424 A CN107954424 A CN 107954424A CN 201810026961 A CN201810026961 A CN 201810026961A CN 107954424 A CN107954424 A CN 107954424A
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- 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
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- 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
Abstract
A kind of preparation method of wide spectrum superelevation adsorbance absorbent charcoal material is to include the following steps to be made：First by quinoa shell carry out high temperature cabonization then sieved, then sieve powder and alkali mix and then the quinoa shell carbon being uniformly mixed with alkali is carried out to sequentially adding after the completion of high-temperature activation, activation sour and distilled water is washed, finally dried, to obtain the final product.Its raw material sources of the invention provide a kind of absorbent charcoal material of high adsorption capacity in agricultural wastes quinoa shell, the adsorption capacity to pluralities of fuel greatly improved in the absorbent charcoal material, for toxic dye methylene blue, rose-red, malachite green, the adsorption capacity of crystal violet etc. improves 2 to 7 times, the activated carbon products rate of recovery of the present invention is up to 95%, with dye separation rate up to 98%, and the activated carbon products may be reused, during reuse, dyestuff removal rate is up to 50%, preparation method is simple and practicable, is worth marketing application.
Description
Technical field
The present invention relates to carbon material field, and in particular to a kind of preparation method of wide spectrum superelevation adsorbance absorbent charcoal material.
Background technology
Absorbent charcoal material is by the amorphous carbon obtained by working process, has very big specific surface area, to gas, solution
In inorganic or organic substance and colloidal solid etc. have good adsorption capacity.Absorbent charcoal material mainly includes activated carbon
（Activated Carbon , A C ）And activated carbon fibre（Activated Carbon Fibers, ACF ）Deng.Activated carbon
Material has unique absorption surface architectural characteristic and surface chemistry mainly due to it as a kind of adsorbent of function admirable
What performance was determined.The chemical property of absorbent charcoal material is stablized, and high mechanical strength is acidproof, alkaline-resisting, heat-resisting, not soluble in water with having
Solvent, can regenerate use, have been widely used for chemical industry, environmental protection, food processing, metallurgy, medicine refine, military chemistry
The every field such as protection.At present, modified active Carbon Materials are widely used in the fields such as sewage disposal, prevention and control of air pollution, are controlling
Its tempting rosy prospect is increasingly shown in terms of reason environmental pollution.
Activated carbon is a kind of very strong Functional carbon material of adsorption capacity.It is with special microstructure, hole is flourishing,
Specific surface area is huge, therefore by as excellent adsorbent, has the double grading of physical absorption and chemisorbed, can there is choosing
Various materials in the absorption liquid and gas selected, to reach the purpose of decolorizing and refining, disinfecting, deodorizing and decontamination purify, extensively
Side applied to production and living such as food, beverage, medicine, water process, fertilizer coating, chemical industry, smelting, national defence, agriculturals
Aspect face.In recent years, stepping up with economic continuous development and people's living standard, people to food, medicine, drink
The living environments such as the security of water, degree of purity propose requirements at the higher level, and the market demand of activated carbon constantly expands.
Current market sales of merchandise active carbon production cost is higher, and selling price is expensive, and adsorption effect is not enough managed
Think, it is not ideal especially for toxic dye such as methylene blue, rose-red, malachite green, crystal violet etc..
The content of the invention
It is an object of the invention to provide a kind of preparation method of wide spectrum superelevation adsorbance absorbent charcoal material.
The purpose of the present invention is what is realized by following technical measures：
A kind of preparation method of wide spectrum superelevation adsorbance absorbent charcoal material, it is characterised in that it is to include the following steps to be made：It is first
First by quinoa shell carry out high temperature cabonization then carry out sieving processing, then sieving powder is mixed with alkali and then will mixed with alkali
Even quinoa shell carbon carries out sequentially adding acid after the completion of high-temperature activation, activation and distilled water is washed, finally dried,
To obtain the final product.
Further, a kind of preparation method of wide spectrum superelevation adsorbance absorbent charcoal material, it is characterised in that the high temperature cabonization
Step is that will clean quinoa shell distilled water, 12 ~ 15 hours is dried in 70 ~ 80 DEG C of thermostatic drying chamber to constant weight, then
Under nitrogen protection, quinoa shell is placed in horizontal pipe furnace, sets heating rate as 5 DEG C/min, temperature rises to 500 DEG C ~ 550
DEG C, take out, cool down after constant temperature 90mins ~ 120min, it is spare.
Further, a kind of preparation method of wide spectrum superelevation adsorbance absorbent charcoal material, it is characterised in that the sieving processing
It is that the quinoa shell charcoal of gained after high-temperature activation is crossed into 80 ~ 120 mesh sieves, collects sieving quinoa shell carbon powder, it is spare.
Further, a kind of preparation method of wide spectrum superelevation adsorbance absorbent charcoal material, it is characterised in that the sieving powder
The alkali charcoal mass ratio mixed with alkali is 2 ~ 4:1, the alkali is KOH and NaOH in mass ratio 1:1 ~ 3 is obtained by mixing.
Further, a kind of preparation method of wide spectrum superelevation adsorbance absorbent charcoal material, it is characterised in that the high-temperature activation
Temperature is 600 ~ 700 DEG C, and the high-temperature activation time is 30 ~ 150min, and the acid added after the activation is that the hydrochloric acid of 0.1mol/L is molten
Liquid, it is 4-6 to wash to the pH of cleaning solution, is then being washed with distilled water to pH=6-8 of cleaning solution, to obtain the final product.
Further, a kind of preparation method of wide spectrum superelevation adsorbance absorbent charcoal material, it is characterised in that it is described drying be by
Product after washing is put into thermostatic drying chamber, and set temperature is 70 ~ 80 DEG C, and drying to constant weight, to obtain the final product.
The beneficial effects of the present invention are：
A kind of preparation method of wide spectrum superelevation adsorbance absorbent charcoal material of the present invention, its raw material sources is in agricultural wastes quinoa
Shell, raw material is simple and easy to get, turns waste into wealth, and can not only solve the problems, such as that quinoa shell waste is handled, and additionally provides a kind of high absorption
The adsorption capacity to pluralities of fuel greatly improved in the absorbent charcoal material of amount, the absorbent charcoal material, for toxic dye methylene
The adsorption capacity of indigo plant, rose-red, malachite green, crystal violet etc. improves 2 to 7 times, its equilibrium adsorption capacities to methylene blue
For 648mg/g, to rose-red（Rhodamine b）Equilibrium adsorption capacities be 759mg/g, the equilibrium adsorption capacities to crystal violet are
601mg/g, the equilibrium adsorption capacities to malachite green are 1365mg/g；The activated carbon products rate of recovery of the present invention is up to 95%, with dye
Separation rate is expected up to 98%, and the activated carbon products may be reused, and during reuse, dyestuff removal rate is prepared up to 50%
Method is simple and practicable, is worth marketing application.
Brief description of the drawings
Fig. 1 is the electron microscope that quinoa shell carbonizes sample.
Fig. 2 is quinoa based active carbon electron microscope.
Fig. 3 is quinoa shell absorbent charcoal material nitrogen adsorption figure.
Fig. 4 is quinoa shell absorbent charcoal material pore size distribution figure.
Embodiment
The present invention is specifically described below by embodiment, it is necessary to which indicated herein is that following embodiments are only used
It is further described in the present invention, it is impossible to limiting the scope of the invention is interpreted as, without departing substantially from spirit of the invention
In the case of essence, the modifications or substitutions made to the method for the present invention, step or condition belong to the scope of the present invention.
Embodiment 1
Take 5g quinoa shells（Discarded after Jilin Agriculture University's quinoa experimental plot stripping seed）It will be cleaned with distilled water, in 70 DEG C of constant temperature
15 hours are dried in drying box to constant weight, then under nitrogen protection, quinoa shell is placed in horizontal pipe furnace, setting heating speed
Rate is 5 DEG C/min, and temperature rises to 500 DEG C, taken out after constant temperature 120min（Quinoa shell charcoal sample is taken to carry out electron microscopic observation, the result is shown in
Fig. 1）, after cooling cross 80 mesh sieves, collect sieving after quinoa shell carbon powder, add 3 times of quinoa shell carbon powder quality KOH with
The mixed base of NaOH, KOH are 1 with NaOH mass ratioes:1, it is uniformly mixed, carries out high-temperature activation, high-temperature activation temperature is 700 DEG C,
The high-temperature activation time is 30min, and activation terminates（The sample after activation is taken to carry out electron microscopic observation, the result is shown in Fig. 2）, add
The hydrochloric acid of 0.1mol/L is washed, and it is 4 to wash to cleaning solution pH, then in pH=7 for being washed with distilled water to cleaning solution, so
After be placed in thermostatic drying chamber, 80 DEG C of set temperature, drying to constant weight, to obtain the final product.Observed from Fig. 1, Fig. 2, quinoa shell
In irregular shape, porous surface after charing and activation.
Experiment one：Sample made from Example 1 carries out nitrogen adsorption experiment
0.1g samples are taken, are positioned in Mike's ASAP2460 instruments, by measuring its cryogenic absorption nitrogen mass, sample is calculated
Product specific surface area, experimental result are shown in Fig. 3, Fig. 4.
Nitrogen adsorption experimental result：N2Adsorption experiment shows that the BET specific surface area of product is 1701.8517m2/ g,
Langmuir specific surface areas are 3020.1627 m2/ g, the duct of product are mainly the micropore that aperture is less than 5nm, average pore size
2.898 nm。
Experiment two：Sample made from Example 1 carries out methylene blue, rose-red, malachite green, the experiment of crystal violet adsorption capacity
0.015g samples are taken, it is parallel to sample 4 parts, it is respectively put into the methylene blue for the 200mg/L for being respectively provided with 100ml, rose
It is rare red, malachite green, in the triangular flask of Crystal Violet Dye solution, with 2%KOH solution or 1%HCl solution（It is mass concentration）Adjust
PH to 7 is saved, is sealed triangular flask with sealed membrane, absorption system is put in the constant-temperature table of 30 DEG C of 150rpm, when its absorption 2 is small
Afterwards, its highest adsorptive value at 663nm, 554nm, 618nm, and 590nm respectively is measured with ultraviolet specrophotometer, can be calculated
Adsorption capacity of the sample to various dyestuffs.
Experimental result：1 sample of embodiment is 648mg/g to the equilibrium adsorption capacities of methylene blue, to rose-red（Rhodamine
b）Equilibrium adsorption capacities be 759mg/g, the equilibrium adsorption capacities to crystal violet are 601mg/g, and the balance of malachite green is inhaled
Attached capacity is 1365mg/g.
Embodiment 2
Take 5g quinoa shells（Discarded after Jilin Agriculture University's quinoa experimental plot stripping seed）It will be cleaned with distilled water, in 80 DEG C of constant temperature
12 hours are dried in drying box to constant weight, then under nitrogen protection, quinoa shell is placed in horizontal pipe furnace, setting heating speed
Rate is 5 DEG C/min, and temperature rises to 500 DEG C DEG C, taken out after constant temperature 120min, and 120 mesh sieves are crossed after cooling, collects the quinoa after sieving
Shell carbon powder, adds the mixed base of the KOH and NaOH of 3 times of quinoa shell carbon powder quality, and KOH is 1 with NaOH mass ratioes:3, mixing
Uniformly, high-temperature activation is carried out, high-temperature activation temperature is 600 DEG C, and the high-temperature activation time is 150min, and activation terminates, and is added
The hydrochloric acid of 0.1mol/L is washed, and it is 6 to wash to cleaning solution pH, then in pH=8 for being washed with distilled water to cleaning solution, so
After be placed in thermostatic drying chamber, 80 DEG C of set temperature, drying to constant weight, to obtain the final product.
By the experimental method of embodiment 1, nitrogen adsorption experiment, methylene blue, rose-red, malachite green, knot are carried out respectively
Crystalviolet adsorption capacity is tested, test result indicates that, in irregular shape, porous surface after the charing of quinoa shell and activation, finished product ratio
Surface area is big, and aperture is small, it is respectively provided with methylene blue, rose-red, malachite green, crystal violet very strong adsorption capacity.
Embodiment 3
Take 5g quinoa shells（Discarded after Jilin Agriculture University's quinoa experimental plot stripping seed）It will be cleaned with distilled water, in 75 DEG C of constant temperature
13 hours are dried in drying box to constant weight, then under nitrogen protection, quinoa shell is placed in horizontal pipe furnace, setting heating speed
Rate is 5 DEG C/min, and temperature rises to 530 DEG C, taken out after constant temperature 110min, and 100 mesh sieves are crossed after cooling, collects the quinoa shell after sieving
Carbon powder, adds the mixed base of the KOH and NaOH of 3 times of quinoa shell carbon powder quality, and KOH is 1 with NaOH mass ratioes:2, mixing is equal
It is even, high-temperature activation is carried out, high-temperature activation temperature is 650 DEG C, and the high-temperature activation time is 60min, and activation terminates, and adds 0.1mol/L
Hydrochloric acid washed, wash to cleaning solution pH be 5, then in pH=7 for being washed with distilled water to cleaning solution, then put
In thermostatic drying chamber, 75 DEG C of set temperature, drying to constant weight, to obtain the final product.
By the experimental method of embodiment 1, nitrogen adsorption experiment, methylene blue, rose-red, malachite green, knot are carried out respectively
Crystalviolet adsorption capacity is tested, test result indicates that, in irregular shape, porous surface after the charing of quinoa shell and activation, finished product ratio
Surface area is big, and aperture is small, it is respectively provided with methylene blue, rose-red, malachite green, crystal violet very strong adsorption capacity.
Claims (6)
1. a kind of preparation method of wide spectrum superelevation adsorbance absorbent charcoal material, it is characterised in that it is to include the following steps to be made：
First by quinoa shell carry out high temperature cabonization then carry out sieving processing, then sieving powder is mixed with alkali and then will mixed with alkali
Acid is sequentially added after the completion of uniform quinoa shell carbon progress high-temperature activation, activation and distilled water is washed, finally dried
It is dry, to obtain the final product.
2. a kind of preparation method of wide spectrum superelevation adsorbance absorbent charcoal material as claimed in claim 1, it is characterised in that described
High temperature cabonization step is that will clean quinoa shell distilled water, and 12 ~ 15 hours are dried in 70 ~ 80 DEG C of thermostatic drying chamber to perseverance
Weight, then under nitrogen protection, quinoa shell is placed in horizontal pipe furnace, heating rate is set and is risen to as 5 DEG C/min, temperature
500 DEG C ~ 550 DEG C, take out after constant temperature 90mins ~ 120min, cool down, it is spare.
3. a kind of preparation method of wide spectrum superelevation adsorbance absorbent charcoal material as claimed in claim 1, it is characterised in that described
Sieving processing is that the quinoa shell charcoal of gained after high-temperature activation is crossed 80 ~ 120 mesh sieves, collects sieving quinoa shell carbon powder, spare.
4. a kind of preparation method of wide spectrum superelevation adsorbance absorbent charcoal material as claimed in claim 1, it is characterised in that described
The alkali charcoal mass ratio that sieving powder is mixed with alkali is 2 ~ 4:1, the alkali is KOH and NaOH in mass ratio 1:1 ~ 3 is obtained by mixing.
5. a kind of preparation method of wide spectrum superelevation adsorbance absorbent charcoal material as claimed in claim 1, it is characterised in that described
High-temperature activation temperature is 600 ~ 700 DEG C, and the high-temperature activation time is 30 ~ 150min, and the acid added after the activation is 0.1mol/L
Hydrochloric acid solution, it is 4-6 to wash to the pH of cleaning solution, is then being washed with distilled water to pH=6-8 of cleaning solution, to obtain the final product.
6. a kind of preparation method of wide spectrum superelevation adsorbance absorbent charcoal material as claimed in claim 1, it is characterised in that described
Drying is that the product after washing is put into thermostatic drying chamber, and set temperature is 70 ~ 80 DEG C, and drying to constant weight, to obtain the final product.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111318254A (en) * | 2020-02-17 | 2020-06-23 | 吉林农业大学 | Preparation method of high-efficiency regenerated activated carbon |
| CN115041137A (en) * | 2022-06-27 | 2022-09-13 | 吉林农业大学 | Preparation and application of recyclable humic acid biomass carbon material |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106744950A (en) * | 2017-03-13 | 2017-05-31 | 东北农业大学 | Pine nut based active carbon and its preparation method and application |
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2018
- 2018-01-11 CN CN201810026961.8A patent/CN107954424A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106744950A (en) * | 2017-03-13 | 2017-05-31 | 东北农业大学 | Pine nut based active carbon and its preparation method and application |
Non-Patent Citations (1)
| Title |
|---|
| 赵松林: "《椰子综合加工技术》", 30 June 2007, 中国农业出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111318254A (en) * | 2020-02-17 | 2020-06-23 | 吉林农业大学 | Preparation method of high-efficiency regenerated activated carbon |
| CN111318254B (en) * | 2020-02-17 | 2022-02-11 | 吉林农业大学 | Preparation method of high-efficiency regenerated activated carbon |
| CN115041137A (en) * | 2022-06-27 | 2022-09-13 | 吉林农业大学 | Preparation and application of recyclable humic acid biomass carbon material |
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Application publication date: 20180424 |