CN106698425A - Preparation method of CO2-adsorbing shrimp-shell-base nitrogenous activated carbon - Google Patents
Preparation method of CO2-adsorbing shrimp-shell-base nitrogenous activated carbon Download PDFInfo
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Abstract
The invention discloses a preparation method of CO2-adsorbing shrimp-shell-base nitrogenous activated carbon. The method comprises the following steps: (1) pulverizing cleaned and dried waste shrimp shells into 100-140 meshes, soaking in excessive 1 mol/L hydrochloric acid for 12 hours, filtering the soaked product, washing with distilled water to a neutral state, and drying to obtain the shrimp shell powder; (2) uniformly mixing the shrimp shell powder and potassium oxalate in a grinder in a certain mass ratio to obtain a mixture; (3) carbonizing the mixture in an N2 atmosphere to obtain a carbonized material; and (4) repeatedly washing the carbonized material with 1 mol/L hydrochloric acid and distilled water to a neutral state, and drying to obtain the shrimp-shell-base nitrogenous activated carbon. Carbonization and activation are completed within one step to substitute the traditional post-activation process; the required raw materials are environmentally friendly and renewable, and the preparation technique is simple; the method can implement in-situ nitrogen doping; and the prepared nitrogen-doped activated carbon has excellent adsorbability and stable cyclic regeneration adsorbability for CO2 under the conditions of room temperature and atmospheric pressure.
Description
Technical field
The present invention relates to a kind of preparation method of nitrogenous activated carbon, specifically a kind of efficient absorption CO2Shrimp shell base it is nitrogenous
The preparation method of activated carbon.
Background technology
Since the industrial revolution, especially since nineteen fifty, fossil feedstock combustion zone comes with CO2Based on a large amount of greenhouse gas
The discharge of body, causes substantial amounts of arid, big flood, sea level rise, and many uncertain disasters.Therefore, CO is implemented2's
Capture and enrichment have important theoretical and practical significance.At present, CO is trapped2Main method have liquid phase scrubbing method, solid-state inhale
Attached method and membrane separation process etc..Wherein liquid phase scrubbing method has severe corrosive, absorbent regeneration energy consumption big to equipment and is easily oxidized, easily
Degraded；Membrane separation process there are problems that separative efficiency it is relatively low, limit its application.By contrast, solid absorption method behaviour
Make relatively easy, the corrosivity to equipment is small, be a kind of CO of great promotion prospect2Trapping recovery technology.
China is shrimp aquaculture big country, and the shrimp shell that peeled shrimp accounts for shrimp gross mass 30~40% in process is removed.Shrimp shell
In contain rich in protein, chitin and chitosan, astaxanthin, unrighted acid and essential amino acid, with wide
Exploitation prospect.But due to the limitation of technical conditions, most of shrimp shell be used to produce feed, and value drops significantly
It is low, and a large amount of soils are taken, cause environmental pollution.Have carbon, nitrogen content high in view of shrimp shell, be easy to get extensively and with low cost
Advantage, can be as the preferable presoma for preparing activated carbon.
The nitrogenous absorbent charcoal material of shrimp shell base not only active charcoal specific surface area high, abundant pore structure, good steady
The advantages of qualitative and alkaline high temperature-resistant acid-resistant, while the introducing of nitrogen-atoms causes that absorbent charcoal material is provided with certain alkalescence, shrimp
The nitrogenous charcoal absorption CO of shell base2Because of its cheap cost, high-adsorption-capacity, adsorptive selectivity high, adsorption dynamics adsorption kinetics faster,
Excellent circular regeneration performance is solid material capture CO2In one of most promising material.Therefore, prepared from shrimp shell nitrogenous
Activated carbon can both reduce the quantity of house refuse, and the new application of shrimp shell can be developed again.Chinese patent literature
CN105271171A discloses a kind of preparation method of the N doping multi-stage porous carbon materials with shrimp shell as carbon source, it is characterised in that with
Nontoxic, cheap shrimp shell is carbon source, in N2Protective effect under, through high-temperature calcination, processed with watery hydrochloric acid, then with ethanol and distillation
The mixed solution of water is cleaned repeatedly, drying to constant weight, obtains the multi-stage porous shrimp shell Carbon Materials of N doping；Again with potassium hydroxide with not
Mix in proportion, in N2Protection under calcine, then by hot distilled water process, watery hydrochloric acid treatment, remove course of reaction in produce
The impurity such as potassium carbonate；Rinsed repeatedly by distilled water again, filtering drying to constant weight, obtain the porous carbon materials of N doping.This is more
Hole carbon material has been successfully applied to the removal of sulfamethazine and chloramphenicol in water environment, and with excellent reproducibility
Energy.But the method needs charing process and activation process, the observable index that this is processed twice is larger, and activation of potassium hydroxide agent is easily dirty
The shortcomings of dye environment.Chinese patent literature CN104310396A discloses a kind of efficient absorption CO2Activated carbon preparation method,
Para-aminophenol, back flow reaction 4h is added to cool to room temperature, be subsequently adding F127 or P123 after being reacted with melamine and formaldehyde
Methanol solution, be segmented at 100-120,130-160,170-190,210-230 and 240-260 DEG C respectively and solidify respectively and must contain
Nitrogen prepolymer；Carbonize again, carbonized material mixes post activation 0.5-2.0h with KOH；Most afterwards through deionized water cyclic washing to neutrality, do
Product is obtained after dry.Activated carbon prepared by the invention has high-specific surface area, high nitrogen-containing and CO high2The advantage of absorption property.
But the method use a large amount of expensive and poisonous organic matters as predecessor, the KOH activators of use have moderate toxicity and
Extremely strong corrosivity, and first carbonize again with KOH admixture activations, complex process, this advocates nontoxic, harmless material with Green Chemistry
Theory be not inconsistent.
To sum up, based on relatively friendly activator, a kind of CO of Cheap highly effective is developed2Sorbing material has important science
Value and good application prospect.
The content of the invention
The technical problems to be solved by the invention are：There is provided a kind of raw material cheap, carbonized and activation system in situ using a step
The method of standby nitrogenous activated carbon, the prepared nitrogenous activated carbon of shrimp shell base is at room temperature to main greenhouse gas CO2With excellent
Absorption property with stabilization circular regeneration absorption property.
The present invention solves its technical problem and uses following technical scheme：
The CO absorption that the present invention is provided2The nitrogenous activated carbon of shrimp shell base preparation method, comprise the following steps：
(1) by clean, dried discarded shrimp shell into powder to 100-140 mesh, then with excessive 1mol/L salt acid soaks
12h, shrimp shell powder is obtained after being washed to neutrality, dry through filtering, distillation；
(2) shrimp shell powder and activator are pressed into certain mass ratio to be well mixed in grinder, obtains mixture；
(3) mixture is placed in the N of 50ml/min2In atmosphere, carbonized material is obtained after charing；
(4) carbonized material after drying 12h at 110 DEG C, is inhaled through 1mol/L hydrochloric acid and distilled water cyclic washing to neutrality
Attached CO2The nitrogenous activated carbon of shrimp shell base.
The activator used in described step (2) is potassium oxalate.
Described step (2) mesoxalic acid potassium is 1 with the mass ratio of shrimp shell powder:1~5:1.
In described step (3), charring process is：Carbonization temperature is 650~750 DEG C, and heating rate is 5 DEG C/min, charcoal
The change time is 2h.
Total specific surface area of the nitrogenous activated carbon of shrimp shell base is 1253-2995m2/g。
The micropore specific area of the nitrogenous activated carbon of shrimp shell base is 1116-2257m2/g。
The nitrogenous activated carbon CO of shrimp shell base2Adsorbance is 2.55~4.51mmol/g, and its circular regeneration number of times is up to 15
It is secondary.
The present invention has the advantages that following main compared with prior art：
(1) with shrimp shell as raw material, its carbon, nitrogen content are high, cheap and wide material sources, it is to avoid using expensive and have
The organic matter of poison；
(2) potassium oxalate is both carbon source and activator；
(3) using a step charing with activation method original position prepare nitrogenous activated carbon, enormously simplify conventional first charing, after
The technological process of activation and the modified process of rear nitrogen, greatly reduce energy consumption and reaction time；
(4) the charcoal absorption CO prepared by2After can regenerate at a lower temperature, by CO absorption2Sample afterwards is in american wheat
In being deaerated under 200 DEG C, vacuum condition on the type Sorption Analyzer degassers of TriStar of new generation II 3020 of gram company production
4h, you can complete regeneration tests, and its circular regeneration absorption property is excellent.
Brief description of the drawings
Fig. 1 is nitrogenous activated carbon, commercial activated carbons (sample A0) prepared by embodiment 1~9 at normal temperatures and pressures to CO2's
Adsorption curve.
Fig. 2 is the scanning electron microscopic picture of nitrogenous activated carbon prepared by embodiment 5.
In Fig. 3, a, b, c figure are respectively the N of nitrogenous activated carbon prepared by embodiment 1~3,4~6,7~92Adsorption-desorption
Thermoisopleth.
In Fig. 4, a, b, c, d figure are respectively the X-ray of the surface N element of nitrogenous activated carbon prepared by embodiment 2,5,6,7
Photoelectron spectroscopy figure.
Nitrogenous activated carbons of the Fig. 5 prepared by embodiment 5 is at normal temperatures and pressures to CO2The circulation absorption thermoisopleth of absorption.
Specific embodiment
With reference to embodiment and accompanying drawing, the invention will be further described, and these embodiments are only preferable to the present invention
The description of implementation method, but it is not limited to the following content.
Embodiment 1：
To clean first, 110 DEG C of discarded shrimp shells dried after 12h into powder to 100-140 mesh, then with the 1mol/L of excess
Salt acid soak 12h, shrimp shell powder is obtained after drying 12h at being washed to neutrality, 110 DEG C through filtering, distillation；Again by 2g shrimp shell meals
(mass ratio of potassium oxalate and shrimp shell powder is 1 for end, 2g potassium oxalates:1) it is well mixed in grinder, obtains mixture；Then
Mixture is placed in N2The lower 650 DEG C of charings 2h of atmosphere (50ml/min) (heating rate is 5 DEG C/min), obtains carbonized material；Finally
Carbonized material through 1mol/L hydrochloric acid and distilled water cyclic washing to neutrality, 110 DEG C dry 12h after obtain activated carbon, it is normal in normal temperature
The CO of pressure2Adsorbance is 3.64mmol/g (see curve A1 in Fig. 1), and nitrogen element content is 4.99wt%.
Embodiment 2：To clean first, 110 DEG C of discarded shrimp shells dried after 12h use excessive into powder to 100-140 mesh, then
1mol/L salt acid soak 12h, through filtering, distillation be washed to it is neutral, dry 12h at 110 DEG C after obtain shrimp shell powder；Then will
(mass ratio of potassium oxalate and shrimp shell powder is 3 for 2g shrimp shells powder, 6g potassium oxalates:1) it is well mixed in grinder, is mixed
Thing；Secondly mixture is placed in N2The lower 650 DEG C of charings 2h of atmosphere (50ml/min) (heating rate is 5 DEG C/min), obtains carbonized material；
Last carbonized material through 1mol/L hydrochloric acid and distilled water cyclic washing to neutrality, 110 DEG C dry 12h after obtain activated carbon, it is normal
CO under normal temperature and pressure2Adsorbance is 4.09mmol/g (see curve A2 in Fig. 1), and nitrogen element content is 6.38wt%.
Embodiment 3：To clean first, 110 DEG C of discarded shrimp shells dried after 12h use excessive into powder to 100-140 mesh, then
1mol/L salt acid soak 12h, through filtering, distillation be washed to it is neutral, dry 12h at 110 DEG C after obtain shrimp shell powder；Then will
(mass ratio of potassium oxalate and shrimp shell powder is 5 for 2g shrimp shells powder, 10g potassium oxalates:1) it is well mixed in grinder, is mixed
Compound；Secondly mixture is placed in N2The lower 650 DEG C of charings 2h of atmosphere (50ml/min) (heating rate is 5 DEG C/min) is carbonized
Material；Last carbonized material through 1mol/L hydrochloric acid and distilled water cyclic washing to neutrality, 110 DEG C dry 12h after obtain activated carbon, its
CO under normal temperature and pressure2Adsorbance is 3.91mmol/g (see curve A3 in Fig. 1), and nitrogen element content is 6.45wt%.
Embodiment 4：To clean first, 110 DEG C of discarded shrimp shells dried after 12h use excessive into powder to 100-140 mesh, then
1mol/L salt acid soak 12h, through filtering, distillation be washed to it is neutral, dry 12h at 110 DEG C after obtain shrimp shell powder；Then will
(mass ratio of potassium oxalate and shrimp shell powder is 1 for 2g shrimp shells powder, 2g potassium oxalates:1) it is well mixed in grinder, is mixed
Thing；Secondly mixture is placed in N2The lower 700 DEG C of charings 2h of atmosphere (50ml/min) (heating rate is 5 DEG C/min) obtains carbonized material；
Last carbonized material through 1mol/L hydrochloric acid and distilled water cyclic washing to neutrality, 110 DEG C dry 12h after obtain activated carbon, it is normal
CO under normal temperature and pressure2Adsorbance is 3.44mmol/g (see curve A4 in Fig. 1), and nitrogen element content is 4.86wt%.
Embodiment 5:To clean first, 110 DEG C of discarded shrimp shells dried after 12h use excessive into powder to 100-140 mesh, then
1mol/L salt acid soak 12h, through filtering, distillation be washed to it is neutral, dry 12h at 110 DEG C after obtain shrimp shell powder；Then will
(mass ratio of potassium oxalate and shrimp shell powder is 3 for 2g shrimp shells powder, 6g potassium oxalates:1) it is well mixed in grinder, is mixed
Thing；Secondly mixture is placed in N2The lower 700 DEG C of charings 2h of atmosphere (50ml/min) (heating rate is 5 DEG C/min), obtains carbonized material；
Last carbonized material, to neutrality, activated carbon is obtained after 12h is dried at 110 DEG C through 1mol/L hydrochloric acid and distilled water cyclic washing, its
CO under normal temperature and pressure2Adsorbance is 4.51mmol/g (see curve A5 in Fig. 1), and nitrogen element content is 3.48wt%.
Embodiment 6：To clean first, 110 DEG C of discarded shrimp shells dried after 12h use excessive into powder to 100-140 mesh, then
1mol/L salt acid soak 12h, through filtering, distillation be washed to it is neutral, dry 12h at 110 DEG C after obtain shrimp shell powder；Then will
(mass ratio of potassium oxalate and shrimp shell powder is 5 for 2g shrimp shells powder, 10g potassium oxalates:1) it is well mixed in grinder, is mixed
Compound；Secondly mixture is placed in N2The lower 700 DEG C of charings 2h of atmosphere (50ml/min) (heating rate is 5 DEG C/min), is carbonized
Material；Last carbonized material, to neutrality, activated carbon is obtained after 12h is dried at 110 DEG C through 1mol/L hydrochloric acid and distilled water cyclic washing, its
CO at normal temperatures and pressures2Adsorbance is 3.65mmol/g (see curve A6 in Fig. 1), and nitrogen element content is 3.36wt%.
Embodiment 7：To clean first, 110 DEG C of discarded shrimp shells dried after 12h use excessive into powder to 100-140 mesh, then
1mol/L salt acid soak 12h, through filtering, distillation be washed to it is neutral, dry 12h at 110 DEG C after obtain shrimp shell powder；Then will
(mass ratio of potassium oxalate and shrimp shell powder is 1 for 2g shrimp shells powder, 2g potassium oxalates:1) it is well mixed in grinder, is mixed
Thing；Secondly mixture is placed in N2The lower 750 DEG C of charings 2h of atmosphere (50ml/min) (heating rate is 5 DEG C/min), obtains carbonized material；
Last carbonized material, to neutrality, activated carbon is obtained after 12h is dried at 110 DEG C through 1mol/L hydrochloric acid and distilled water cyclic washing, its
CO under normal temperature and pressure2Adsorbance is 3.88mmol/g (see curve A7 in Fig. 1), and nitrogen element content is 1.39wt%.
Embodiment 8：To clean first, 110 DEG C of discarded shrimp shells dried after 12h use excessive into powder to 100-140 mesh, then
1mol/L salt acid soak 12h, through filtering, distillation be washed to it is neutral, dry 12h at 110 DEG C after obtain shrimp shell powder；Then will
(mass ratio of potassium oxalate and shrimp shell powder is 3 for 2g shrimp shells powder, 6g potassium oxalates:1) it is well mixed in grinder, is mixed
Thing；Secondly mixture is placed in N2The lower 750 DEG C of charings 2h of atmosphere (50ml/min) (heating rate is 5 DEG C/min), obtains carbonized material；
Last carbonized material, to neutrality, activated carbon is obtained after 12h is dried at 110 DEG C through 1mol/L hydrochloric acid and distilled water cyclic washing, its
CO under normal temperature and pressure2Adsorbance is 2.55mmol/g (see curve A8 in Fig. 1), and nitrogen element content is 1.25wt%.
Embodiment 9：To clean first, 110 DEG C of discarded shrimp shells dried after 12h use excessive into powder to 100-140 mesh, then
1mol/L salt acid soak 12h, through filtering, distillation be washed to it is neutral, dry 12h at 110 DEG C after obtain shrimp shell powder；Then will
(mass ratio of potassium oxalate and shrimp shell powder is 5 for 2g shrimp shells powder, 10g potassium oxalates:1) it is well mixed in grinder, is mixed
Compound；Secondly mixture is placed in N2The lower 750 DEG C of charings 2h of atmosphere (50ml/min) (heating rate is 5 DEG C/min), is carbonized
Material；Last carbonized material, to neutrality, activated carbon is obtained after 12h is dried at 110 DEG C through 1mol/L hydrochloric acid and distilled water cyclic washing, its
CO at normal temperatures and pressures2Adsorbance is 2.62mmol/g (see curve A9 in Fig. 1), and nitrogen element content is 1.12wt%.
The sample of embodiment 1-9 is contrasted using the type Sorption Analyzers of TriStar II 2020 that Merck ＆ Co., Inc of the U.S. produces
Surface area and hole are analyzed, and total specific surface area is measured using Brunauer-Emmett-Teller (BET) method, and total pore volume exists
Relative pressure P/P00~0.995 is calculated by the adsorbance of liquid nitrogen, and micropore specific area is obtained with Micropore volume by t-plot methods
Arrive.Design parameter is shown in Table one, by table one as can be seen that the present invention does the activated carbon for preparing has total specific surface area very high and total
Pore volume, highest is respectively up to 2995m2/ g, 1.51cm3/ g, and micropore specific area and Micropore volume product account for ratio very high
Example, and CO2A diameter of 0.33nm of molecule, this is to CO2The absorption of gas plays a very important role.
The XPS figures of prepared nitrogenous activated carbon are it can be seen that its nitrogen is in material surface according to embodiments of the present invention
To there is Fig. 4 a, 4b, 4c contain N-6 (pyridine) to existence form, and N-5 (pyrroles), N-Q (quaternary nitrogen), Fig. 4 d then comprise only N-5
(pyrroles), N-Q (quaternary nitrogen) show with temperature raises its nitrogen existence form also can respective change.
The mass ratio of the shrimp shell powder after potassium oxalate and HCl treatment is to CO absorption2Nitrogenous shrimp shell matrix activated carbon adsorptivity
The influence of energy：When fixed activation temperature is 700 DEG C, CO2Adsorbance and potassium oxalate and HCl treatment after shrimp shell powder matter
Amount first rises the relation for declining afterwards than presenting, to CO2Adsorbance highest be embodiment 5 prepare, the potassium oxalate of use and
The mass ratio of the shrimp shell powder after HCl treatment is 1:3.
The mass ratio of the shrimp shell powder after fixed potassium oxalate and HCl treatment is 1:3, activation temperature is to CO absorption2It is nitrogenous
The influence of shrimp shell matrix activated carbon absorption property：The mass ratio of the shrimp shell powder after fixed potassium oxalate and HCl treatment is 1:When 3,
CO2Adsorbance and activation temperature the relation for first rising and declining afterwards is presented, to CO2Adsorbance highest is prepared by embodiment 5
, the activation temperature for using is 700 DEG C.
By CO absorption2The type Sorption Analyzers of TriStar of new generation II 3020 that sample afterwards is produced in Merck ＆ Co., Inc of the U.S.
Degasser in the 4h that deaerated under 200 DEG C, vacuum condition.Then the sample after degassing is circulated adsorption experiment, is circulated
13 times, its room temperature CO2Adsorbance substantially remains in 4.51mmol/g, is slightly decreased at the 14th time and the 15th time, shows excellent
Different circular regeneration uses ability (see Fig. 5).
In above-described embodiment, former occupation 400Y type small electric flour mills can be used, peanut shell after drying is ground
Mill.
The Main Texture nature parameters and nitrogen element content data of nitrogenous activated carbon prepared by the embodiment 1~9 of table 1
Claims (9)
1. a kind of CO absorption2The nitrogenous activated carbon of shrimp shell base preparation method, it is characterised in that comprise the following steps：
(1) by clean, dried discarded shrimp shell into powder to 100-140 mesh, then with excessive 1mol/L salt acid soak 12h,
Shrimp shell powder is obtained after being washed to neutrality, dry through filtering, distillation；
(2) shrimp shell powder and activator are pressed into certain mass ratio to be well mixed in grinder, obtains mixture；
(3) mixture is placed in the N of 50ml/min2In atmosphere, carbonized material is obtained after charing；
(4) carbonized material after drying 12h at 110 DEG C, obtains CO absorption through 1mol/L hydrochloric acid and distilled water cyclic washing to neutrality2
The nitrogenous activated carbon of shrimp shell base.
2. preparation method according to claim 1, it is characterised in that in step (2), described activator is potassium oxalate.
3. preparation method according to claim 2, it is characterised in that in step (2), the quality of potassium oxalate and shrimp shell powder
Than being 1:1~5:1.
4. preparation method according to claim 1, it is characterised in that in step (3), charring process is：Carbonization temperature is
650~750 DEG C, heating rate is 5 DEG C/min, carbonization time 2h.
5. the CO absorption that in Claims 1-4 prepared by any methods described2The nitrogenous activated carbon of shrimp shell base, it is characterized in that its always than
Surface area is 1253-2995m2/g。
6. CO absorption according to claim 52The nitrogenous activated carbon of shrimp shell base, it is characterized in that its micropore specific area is
1077-2257m2/g。
7. CO absorption according to claim 52The nitrogenous activated carbon of shrimp shell base, it is characterized in that its CO under normal temperature and pressure2Absorption
It is 2.55~4.51mmol/g to measure.
8. CO absorption according to claim 52The nitrogenous activated carbon of shrimp shell base, it is characterized in that it is in 25 DEG C of CO absorptions2Afterwards,
It is desorbed at 200 DEG C again and realizes regeneration, as the adsorbent for recycling.
9. CO absorption according to claim 82The nitrogenous activated carbon of shrimp shell base, it is characterized in that circular regeneration number of times >=15 time.
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| CN108002360A (en) * | 2017-11-30 | 2018-05-08 | 浙江海洋大学 | A kind of preparation based on shrimp and crab shells biomass carbon electrode material for super capacitor |
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