CN107115843A - A kind of preparation method and applications for coming from peanut shell modified activated carbon - Google Patents
A kind of preparation method and applications for coming from peanut shell modified activated carbon Download PDFInfo
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- CN107115843A CN107115843A CN201710367917.9A CN201710367917A CN107115843A CN 107115843 A CN107115843 A CN 107115843A CN 201710367917 A CN201710367917 A CN 201710367917A CN 107115843 A CN107115843 A CN 107115843A
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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
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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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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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
Abstract
Prepared the invention belongs to material and pollutant process field, disclose a kind of preparation method and applications for coming from peanut shell modified activated carbon.The activated carbon is, using peanut shell as raw material, using chemical activation, and to be prepared with Nitric Acid Modified.By the peanut shell powder after clean, crushing, sieving, in the activator solution for immersing 5~20%, water-bath, activator is fully infiltrated into peanut shell fibrous inside, then drying, grinding；The lower high-temperature activation of nitrogen protection, 400~800 DEG C of 30~120min of activation after cooling, with chlorohydric acid pickling, then are washed to neutrality, are modified using nitric acid high-temperature oxydation, washing drying obtains modified Activated Carbon Made from Peanut Shells.The modified activated carbon is homogeneous, hole is flourishing, and specific surface area is up to 1807m2/ g, pore volume is 0.725cm3/g.Peanut shell is a kind of sufficient, cheap and easy to get wastes of crops of originating, and the present invention not only reduces the manufacturing cost of activated carbon, solves the problems, such as the sublimity that peanut shell processing is brought not in time, also handles its modified water pollution that is used for.
Description
Technical field
Prepared the invention belongs to material and pollutant process field, be related to a kind of preparation for coming from peanut shell modified activated carbon
Method and its application.
Background technology
With industry develop rapidly and dyeing waste water unreasonable discharge, the pollution of dyeing waste water in China's water body environment
It is increasingly severe, cause the extensive concern of people.The features such as dyeing waste water has bio-toxicity, persistence and easily accumulated, influence
The growth and breeding of animals and plants in water body, destroy ecological environment, and the harm mankind's is healthy.At present, dyeing waste water is handled
Major technique includes：Chemical precipitation, ion exchange, UF membrane and absorption etc..Wherein, because absorption method has simple to operate, material
The advantages of material is cheap and has a wide range of application, it is had been widely used in treatment of dyeing wastewater.
Activated carbon has abundant pore structure, huge specific surface area and a variety of functional groups, makes it have efficient suction
Attached effect, therefore, it has a wide range of applications as adsorbent in industrial circle.Raw material prepared by conventional carbon is mainly wood
Material and coal, but be due to the enhancing in short supply and people's environmental consciousness of coal resources, seek cheap and abundant renewable
The problem of raw material are current activated carbon preparation field urgent need to resolve.In recent years, with coconut husk, walnut, corncob, stalk Isoquant
Agriculture and forestry organic waste material that is big and being easy to get turns into the focus in terms of activated carbon raw material exploitation for activated carbon prepared by raw material.Peanut is China
Important oil crops, peanut shell is as a kind of agricultural wastes, without any industrial utility value, if located not in time
Reason, can also cause certain environmental pollution.However, peanut shell material have very low content of ashes, small apparent density and
High porosity etc., these properties cause peanut shell to be a kind of preferable activated carbon raw material.Therefore, activity is prepared using peanut shell
Charcoal can not only reduce the production cost of activated carbon, moreover it is possible to effective to solve the problem of environmental pollution that peanut shell is brought.
Activated carbon as a kind of adsorbent of high-quality, its adsorption capacity be mainly derived from its surface chemical functional group and
Loose structure.In order to further improve absorption property of the activated carbon to object, researcher is directed to developing and improves activity
The activation of charcoal and method of modifying.In recent years, activated carbon research emphasis is concentrated on ruthenium ammonia synthesis catalyst, and it is broadly divided into sour place
Reason, alkali process, microwave treatment and ozone processing etc..Research shows, by the surface modification treatment to activated carbon, can improve pair
The Adsorption effect of Pollutants in Wastewater.The activated carbon that this patent is modified using peanut shell as raw material and with nitric acid oxidation is absorption
Agent is used to adsorb the organic dyestuff and heavy metal ion in water, not only solves peanut shell handling problems, also effectively raises
Absorption property of the activated carbon to dyeing waste water.
The content of the invention
The purpose of the present invention is, using peanut shell as raw material, using analysis for preparation of activated carbon by chemical activation material, and to use concentrated nitric acid
It is modified, is reapplied in organic dyestuff and the research of the adsorption experiment of heavy metal ion at high temperature.The adsorbent is compared to biography
System activated carbon has the advantages that preparing raw material wide material sources, cheap, renewable and high to the clearance of object, absorption
Capacity is big.
The present invention is achieved through the following technical solutions：
A kind of preparation method for coming from peanut shell modified activated carbon, comprises the following steps：
Step 1, peanut shell washed, after drying, recycle pulverizer grinding and sieving, peanut shell powder is made；
Step 2, by the material that step 1 is obtained be added in activator solution stir, heating water bath, and carry out vacuum do
Dry, milled processed obtains peanut shell activated feedstock；
The high-temperature calcination under nitrogen protection in tube furnace of step 3, the peanut shell activated feedstock for obtaining step 2, is carried out high
Warm priming reaction, is cooled to after room temperature, then washs, and dries；
Step 4, the material that step 3 is obtained is added in hydrochloric acid solution, obtains mixed liquor A, mixed liquor A is heated to reflux
Stirring, is washed after cooling to neutral and dry；
Step 5, the material obtained in step 4 is added in salpeter solution, obtains mixed liquid B, mixed liquid B is heated back
Stream stirring, cooling after scrubbed and vacuum drying, obtains modified Activated Carbon Made from Peanut Shells.
In step 1, peanut shell drying temperature be 100~120 DEG C, the time be 12~24h, sieved after crushing be 40~
60 mesh.
In step 2, activator used is any of phosphoric acid, potassium hydroxide or zinc chloride.Peanut shell and activator
Mass ratio be 1:1~4, the concentration of the aqueous solution of activator is 5%~20%, and the temperature of heating water bath is 50~70 DEG C, plus
The hot time is 1~3h；Vacuum drying temperature is 100~120 DEG C, and the time is 12~24h.
In step 3, nitrogen flow rate is 50mL/min in tube furnace, and the temperature of heating is 400~800 DEG C, heating and continuous
Time is 30~120min, and heating rate is 3 DEG C/min.
In step 4, the concentration of hydrochloric acid is 2~5mol/L in mixed liquor A, and heating-up temperature is 60~80 DEG C, the time of heating
For 2~4h, the mass ratio of sample and hydrochloric acid is 1:2~10.
In step 5, in mixed liquid B the concentration of nitric acid be 5~10mol/L, heating-up temperature be 80~100 DEG C, heating when
Between be 12~24h, the mass ratio of sample and nitric acid is 1:5~60.
The method that above-mentioned peanut shell modified activated carbon is applied to organic dyestuff or heavy metal ion in adsorption aqueous solution, according to
Following step is carried out：
Staticadsorption experiment：
The organic dye molecule of 20mL concentration knowns or heavy metal ion solution are added in colorimetric cylinder, thermostatted water is placed on
Stood in bath, investigate the shadow to activated carbon adsorptive capacity such as initial concentration, solution ph, temperature, adsorption time of adsorbent solution
Ring.After the completion of absorption, by being centrifugally separating to obtain supernatant liquor, ultraviolet specrophotometer is recycled to for organic dye molecule
Concentration is measured；Detected using the concentration of ICP heavy metal ions, and adsorption capacity is calculated according to result.
Organic dyestuff of the present invention includes：Cationic blue, Congo red, methylene blue, rhodamine B, gentian violet, she
Red, sarranine；Heavy metal ion of the present invention includes：Lead, chromium, cadmium, copper.
The beneficial effects of the present invention are：
A kind of peanut shell modified activated carbon that comes from prepared by the present invention makes discarded peanut shell using discarded peanut shell as raw material
Recycling, solves the discarded environmental problem brought of peanut shell, the cost of reduction production activated carbon.Utilize the place of hydrochloric acid and nitric acid
Reason is modified, and is added the pore structure of activated carbon and the functional group on surface, has been obviously improved processing energy of the activated carbon for waste water
Power.
Brief description of the drawings
Fig. 1：For the infrared figure of peanut shell modified activated carbon, activated carbon is infrared before and after the two lines difference Nitric Acid Modified in figure
Absorb collection of illustrative plates；
Fig. 2：(a) it is the scanning electron microscope (SEM) photograph of peanut shell powder, (b) is the scanning electron microscope (SEM) photograph of peanut shell modified activated carbon.
Embodiment
With reference to Figure of description and specific implementation example, the present invention will be further described.
Embodiment 1：
1. the preparation of peanut shell modified activated carbon
(1) peanut shell is washed, 24h is dried at 100 DEG C, 60 mesh sieves are crossed after crushing, peanut shell powder is obtained.
(2) 5.0g peanut shell powder is weighed, is added in the liquor zinci chloridi that 100mL concentration is 5%, the water at 50 DEG C
Bath heating 3h, is most dried in vacuo 24h after 100 DEG C, and then grinding obtains peanut shell activated feedstock.
(3) take 5.0g peanut shell activated feedstocks to be placed in tube furnace, be passed through nitrogen 10min to arrange with 50mL/min speed
Except the air in pipe.Then 800 DEG C are warming up to 3 DEG C/min speed under nitrogen protection, and keep 30min, stop heating
It is continually fed into nitrogen and is cooled to room temperature, then washs drying.
(4) material obtained in 2.0g steps (3) is taken to be added in the hydrochloric acid solution that 100mL concentration is 2mol/L, and
4h is heated in 60 DEG C of water-bath, centrifuge washing to neutrality is simultaneously dried.
(5) material obtained in 1.0g steps (4) is taken to be added in the salpeter solution that 100mL concentration is 5mol/L, and
24h is heated at reflux in 80 DEG C of water-bath, centrifuge washing to neutrality is simultaneously dried.
2. adsorption test
The cationic blue solution for taking 20mL initial concentrations to be respectively 5~400mg/L is added in 25mL colorimetric cylinders, uses dilute salt
It is 7 that acid or dilute sodium hydroxide, which adjust pH value, is separately added into 10mg peanut shell modified activated carbon absorbents, and three groups of test fluids are distinguished
It is placed in 25, stands 8h in 35,45 DEG C of water-bath, centrifuges, take supernatant and determined after diluting using ultraviolet specrophotometer
The concentration of remaining attached cationic blue, adsorption capacity is calculated according to result.As a result show, peanut shell modified activated carbon is at 45 DEG C
The saturated extent of adsorption of cationic blue is 639mg/g.
Embodiment 2：
1. the preparation of peanut shell modified activated carbon
(1) peanut shell is washed, 12h is dried at 120 DEG C, 60 mesh sieves are crossed after crushing, peanut shell powder is obtained.
(2) 5.0g peanut shell powder is weighed, is added in the liquor zinci chloridi that 100mL concentration is 20%, at 70 DEG C
Heating water bath 1h, is most dried in vacuo 12h after 120 DEG C, and then grinding obtains peanut shell activated feedstock.
(3) take 5.0g peanut shell activated feedstocks to be placed in tube furnace, be passed through nitrogen 10min to arrange with 50mL/min speed
Except the air in pipe.Then 600 DEG C are warming up to 3 DEG C/min speed under nitrogen protection, and keep 120min, stop heating
It is continually fed into nitrogen and is cooled to room temperature, then washs drying.
(4) material obtained in 2.0g steps (3) is taken to be added in the hydrochloric acid solution that 100mL concentration is 5mol/L, and
2h is heated in 80 DEG C of water-bath, centrifuge washing to neutrality is simultaneously dried.
(5) material obtained in 1.0g steps (4) is taken to be added in the salpeter solution that 100mL concentration is 8mol/L, and
12h is heated at reflux in 100 DEG C of water-bath, centrifuge washing to neutrality is simultaneously dried.
2. adsorption test
The Congo red solution for taking 20mL initial concentrations to be respectively 5~400mg/L is added in 25mL colorimetric cylinders, uses watery hydrochloric acid
Or dilute sodium hydroxide regulation pH value is 2, is separately added into 10mg peanut shell modified activated carbon absorbents, three groups of test fluids are put respectively
8h is stood in 25, in 35,45 DEG C of water-bath, centrifuges, determines surplus using ultraviolet specrophotometer after taking supernatant and diluting
Remaining attached Congo red concentration, adsorption capacity is calculated according to result.As a result show, peanut shell modified activated carbon is in the 45 DEG CXia the Congo
Red saturated extent of adsorption is 421mg/g.
Embodiment 3：
1. the preparation of peanut shell modified activated carbon
(1) peanut shell is washed, 24h is dried at 100 DEG C, 60 mesh sieves are crossed after crushing, peanut shell powder is obtained
(2) 5.0g peanut shell powder is weighed, is added in the potassium hydroxide solution that 100mL concentration is 5%, at 50 DEG C
Heating water bath 3h, is most dried in vacuo 24h after 100 DEG C, and then grinding obtains peanut shell activated feedstock.
(3) take 5.0g peanut shell activated feedstocks to be placed in tube furnace, be passed through nitrogen 10min to arrange with 50mL/min speed
Except the air in pipe.Then 800 DEG C are warming up to 3 DEG C/min speed under nitrogen protection, and keep 30min, stop heating
It is continually fed into nitrogen and is cooled to room temperature, and washs drying.
(4) material obtained in 2.0g steps (3) is taken to be added in the hydrochloric acid solution that 100mL concentration is 2mol/L, and
4h is heated in 60 DEG C of water-bath, centrifuge washing to neutrality is simultaneously dried.
(5) material obtained in 1.0g steps (4) is taken to be added in the salpeter solution that 100mL concentration is 5mol/L, and
24h is heated at reflux in 80 DEG C of water-bath, centrifuge washing to neutrality is simultaneously dried.
2. adsorption test
The phenol solution for taking 20mL initial concentrations to be respectively 5~400mg/L is added in 25mL colorimetric cylinders, with watery hydrochloric acid or
Dilute sodium hydroxide regulation pH value is 3, is separately added into 10mg peanut shell modified activated carbon absorbents, three groups of test fluids are respectively placed in
25th, 35 8h, is stood in 45 DEG C of water-bath, is centrifuged, determines remaining using ultraviolet specrophotometer after taking supernatant and diluting
The concentration of phenol, adsorption capacity is calculated according to result.As a result show, the saturation of peanut shell modified activated carbon phenol at 45 DEG C
Adsorbance is 117mg/g.
Embodiment 4：
1. the preparation of peanut shell modified activated carbon
(1) peanut shell is washed, 24h is dried at 100 DEG C, 40 mesh sieves are crossed after crushing, peanut shell powder is obtained.
(2) 5.0g peanut shell powder is weighed, is added in the phosphoric acid solution that 100mL concentration is 5%, the water-bath at 50 DEG C
3h is heated, most 24h is dried in vacuo after 100 DEG C, then grinding obtains peanut shell activated feedstock.
(3) take 5.0g peanut shell activated feedstocks to be placed in tube furnace, be passed through nitrogen 10min to arrange with 50mL/min speed
Except the air in pipe.Then 600 DEG C are warming up to 3 DEG C/min speed under nitrogen protection, and keep 30min, stop heating
It is continually fed into nitrogen and is cooled to room temperature, and washs drying.
(4) material obtained in 2.0g steps (3) is taken to be added in the hydrochloric acid solution that 100mL concentration is 2mol/L, and
4h is heated in 60 DEG C of water-bath, centrifuge washing to neutrality is simultaneously dried.
(5) material obtained in 1.0g steps (4) is taken to be added in the salpeter solution that 100mL concentration is 5mol/L, and
24h is heated at reflux in 80 DEG C of water-bath, centrifuge washing to neutrality is simultaneously dried.
2. adsorption test
Pb (II) solution for taking 20mL initial concentrations to be respectively 5~400mg/L is added in 25mL colorimetric cylinders, uses watery hydrochloric acid
Or weak aqua ammonia regulation pH value is 5, is separately added into 10mg peanut shell modified activated carbon absorbents, three groups of test fluids are respectively placed in
25th, 35 8h, is stood in 45 DEG C of water-bath, is centrifuged, supernatant is taken and determines the dense of residue Pb (II) using ICP after diluting
Degree, adsorption capacity is calculated according to result.As a result show, peanut shell modified activated carbon Pb (II) at 45 DEG C saturated extent of adsorption
For 135mg/g.
Embodiment 5：
1. the preparation of peanut shell modified activated carbon
(1) peanut shell is washed, 12h is dried at 120 DEG C, 60 mesh sieves are crossed after crushing, peanut shell powder is obtained.
(2) 5.0g peanut shell powder is weighed, is added in the phosphoric acid solution that 100mL concentration is 20%, the water at 70 DEG C
Bath heating 1h, is most dried in vacuo 12h after 120 DEG C, and then grinding obtains peanut shell activated feedstock.
(3) take 5.0g peanut shell activated feedstocks to be placed in tube furnace, be passed through nitrogen 10min to arrange with 50mL/min speed
Except the air in pipe.Then 400 DEG C are warming up to 3 DEG C/min speed under nitrogen protection, and keep 120min, stop heating
It is continually fed into nitrogen and is cooled to room temperature, and washs drying.
(4) material obtained in 2.0g steps (3) is taken to be added in the hydrochloric acid solution that 100mL concentration is 5mol/L, and
2h is heated in 80 DEG C of water-bath, centrifuge washing to neutrality is simultaneously dried.
(5) material obtained in 1.0g steps (4) is taken to be added in the salpeter solution that 100mL concentration is 8mol/L, and
12h is heated at reflux in 100 DEG C of water-bath, centrifuge washing to neutrality is simultaneously dried.
2. adsorption test
Cr (VI) solution for taking 20mL initial concentrations to be respectively 5~400mg/L is added in 25mL colorimetric cylinders, uses watery hydrochloric acid
Or weak aqua ammonia regulation pH value is 2, is separately added into 10mg peanut shell modified activated carbon absorbents, three groups of test fluids are respectively placed in
25th, 35 8h, is stood in 45 DEG C of water-bath, is centrifuged, supernatant is taken and determines the dense of residue Cr (VI) using ICP after diluting
Degree, adsorption capacity is calculated according to result.As a result show, peanut shell modified activated carbon Cr (VI) at 45 DEG C saturated extent of adsorption
For 107mg/g.
From Fig. 1, it is clear that after Nitric Acid Modified, activated carbon possesses more abundant functional group, such as carboxyl, hydroxyl
Deng.
From figure 2, it is seen that (b) is more coarse relative to (a) surface, illustrate that activation causes activated carbon to have bigger ratio table
Area and pore structure.
Claims (10)
1. a kind of preparation method for coming from peanut shell modified activated carbon, it is characterised in that comprise the following steps：
Step 1, peanut shell washed, after drying, recycle pulverizer grinding and sieving, peanut shell powder is made；
Step 2, the material that step 1 is obtained is added in activator solution and stirred, heating water bath, and being dried in vacuo is ground
Mill processing, obtains peanut shell activated feedstock；
The high-temperature calcination under nitrogen protection in tube furnace of step 3, the peanut shell activated feedstock for obtaining step 2, progress activates anti-
Should, it is cooled to after room temperature, then wash, dry；
Step 4, the material that step 3 is obtained is added in hydrochloric acid solution, obtains mixed liquor A, mixed liquor A is heated to reflux to stir
Mix, washed after cooling to neutral and dry；
Step 5, the material obtained in step 4 is added in salpeter solution, obtains mixed liquid B, mixed liquid B is heated to reflux to stir
Mix, cool down, after scrubbed and vacuum drying, obtain modified Activated Carbon Made from Peanut Shells.
2. the preparation method of a kind of peanut shell modified activated carbon according to claim 1, it is characterised in that in step 1, institute
The drying temperature for stating peanut shell is 100~120 DEG C, and the time is 12~24h, and grinding and sieving is 40~60 mesh.
3. the preparation method of a kind of peanut shell modified activated carbon according to claim 1, it is characterised in that in step 2, institute
It is any of phosphoric acid, potassium hydroxide or zinc chloride to state activator.
4. the preparation method of a kind of peanut shell modified activated carbon according to claim 1, it is characterised in that in step 2, institute
The mass ratio for stating peanut shell powder and activator is 1:1~4, the concentration of the aqueous solution of activator is 5%~20%.
5. the preparation method of a kind of peanut shell modified activated carbon according to claim 1, it is characterised in that in step 2, flower
Raw shell powder is in activator solution, and the temperature of heating water bath is 50~70 DEG C, and the time is 1~3h, and vacuum drying temperature is 100
~120 DEG C, the time is 12~24h.
6. the preparation method of a kind of peanut shell modified activated carbon according to claim 1, it is characterised in that in step 3, institute
The heating-up temperature stated is 400~800 DEG C, and the heat time is 30~120min, and heating rate is 3 DEG C/min, and nitrogen flow rate is
50mL/min。
7. the preparation method of a kind of peanut shell modified activated carbon according to claim 1, it is characterised in that in step 4, institute
The concentration for stating activator hydrochloric acid is 2~5mol/L, and heating-up temperature is 60~80 DEG C, and the time of heating is 2~4h, sample and hydrochloric acid
Mass ratio be 1:2~10.
8. the preparation method of a kind of peanut shell modified activated carbon according to claim 1, it is characterised in that in step 5, institute
The concentration for stating activator nitric acid is 5~10mol/L, and heating-up temperature is 80~100 DEG C, and time of heating is 12~24h, sample with
The mass ratio of nitric acid is 1:5~60.
9. one kind made from preparation method described in claim 1~8, which comes from peanut shell modified activated carbon, to be used in adsorption aqueous solution
The purposes of organic dyestuff or heavy metal ion.
10. one kind as claimed in claim 9, which comes from peanut shell modified activated carbon, is used for organic dyestuff or again in adsorption aqueous solution
The purposes of metal ion, it is characterised in that the organic dyestuff includes：Cationic blue, Congo red, methylene blue, rhodamine B,
Gentian violet, Yihong, sarranine；Heavy metal ion includes：Lead, chromium, cadmium, copper.
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| CN107459096A (en) * | 2017-09-29 | 2017-12-12 | 长沙理工大学 | A kind of method of gill fungus bacterium matrix activated carbon adsorbent processing cadmium wastewater |
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| CN115140737A (en) * | 2022-06-30 | 2022-10-04 | 潍坊学院 | Process for preparing peanut shell-based activated carbon by one-step activation method and CO 2 Application of trapping |
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