CN106622132A - Muyu stone adsorbent with pili nut shell and chestnut shell and preparation method thereof - Google Patents
Muyu stone adsorbent with pili nut shell and chestnut shell and preparation method thereof Download PDFInfo
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- CN106622132A CN106622132A CN201611201178.8A CN201611201178A CN106622132A CN 106622132 A CN106622132 A CN 106622132A CN 201611201178 A CN201611201178 A CN 201611201178A CN 106622132 A CN106622132 A CN 106622132A
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- 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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- 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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- C02F1/00—Treatment of water, waste water, or sewage
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- 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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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
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Abstract
A preparation method of pili nut shell and chestnut shell biochar comprises the steps of crushing pili nut shell and chestnut shell, mixing, adding catalyst solution, sealing and standing, placing in a sample boat, introducing nitrogen, sealing for pyrolysis, cooling to room temperature after reaction is finished, removing, mixing with H2O2, vibrating in a vibrator, washing with distilled water, and drying to obtain high-adsorption biochar. The pili nut shell and chestnut shell are mixed to obtain biochar, the adsorbing property of the prepared biochar can be ensured, and the purifying effect of the biochar can be improved. Purification test results indicate that the biochar is up to 80.1%, 82.7% and 85.2% respectively for chromium, lead and methylene blue in water; the results of test on the specific surface area and pore size of the prepared biochar by SA3100 specific surface area and pore size analyzer show that the biochar has excellent related parameters; the biochar prepared herein is up to 251.7 m<2>/g, 0.1301 cm<3>/g and 0.2972 cm<3>/g respectively in specific surface area, micropore size and total pore size.
Description
Technical field
The invention belongs to water treatment field, and in particular to a kind of thunderbolt shell, chestnut shell/limonite adsorbent and its preparation
Method.
Background technology
As industrialization, urbanization process are accelerated, facing mankind increasingly severe shortage of water resources and pollution problem.
According to data, there is the urban water shortage of half or so in more than 600 city of China, the feature water shortage that water pollution is caused more makes water
Shortage of resources makes the matter worse.According to statistics, the lake in the whole nation 75% occurs in that different degrees of eutrophication；90% urban waters are dirty
Dye is serious, and the 60%---70% of the total water deficit in Shelter in South China Cities is caused due to water pollution.Water pollution reduces the use work(of water body
Can, shortage of water resources is exacerbated, have a strong impact on China's economy, the strategy of sustainable development of environment.
Charcoal is that biological material is pyrolyzed under anoxic or limited oxygen condition, is removed oily gentle rear remaining in biomass
Solid matter.Correlative study shows that charcoal has huge surface area and internal voids, with negative electrical charge is more, ion exchange
The features such as ability is strong, absorption property is excellent, can not only directly adsorb polluter, and soil physical chemistry can be also improved after being manured into soil
Matter, reduction nutrient loss, promotion plant growth, absorption fixing soil polluter, and carbon base in soil can be increased, reduce greenhouse gas
Body is discharged.Charcoal research on utilization has become one of focus of environment and field of agricultural sciences research.Prepare the original of charcoal
Material source is quite varied, and farmland discarded object, house refuse, excrement of animals etc. can be as the raw materials for preparing charcoal but different
Charcoal architectural difference prepared by biomass material and pyrolysis temperature is larger, also different to the absorption property of polluter,
This be also in recent years related scholar also continuing to be engaged in biological carbon prepare, the key reason of modified aspect research.Additionally, existing life
It is many in thing carbon preparation research that biological carbon is prepared with single raw material, it is less with the research that mixed material prepares biological carbon, especially lack
Purposive research biomass material being optimized in terms of combining to prepare high absorption property biological carbon.
The content of the invention
First purpose of the present invention is to provide a kind of thunderbolt shell, the preparation method of chestnut shell biological carbon.
Second object of the present invention is to provide a kind of thunderbolt shell, the preparation method of chestnut shell/limonite adsorbent.
The purpose of the present invention is realized by following technical measures：
A kind of thunderbolt shell, the preparation method of chestnut shell biological carbon, it is characterised in that the charcoal is by thunderbolt shell and plate
Chestnut shell is obtained as follows：（1）Take thunderbolt shell, chestnut shell and crush 20～200 mesh sieves respectively, it is standby；（2）By above-mentioned powder
Thunderbolt shell, chestnut shell after broken is 1～10 in mass ratio：1 mixing, adds mixed catalytic agent solution, and mixed catalyst is molten
The compound method of liquid is the mass ratio Co (NO for taking thunderbolt shell, chestnut shell powder gross mass 1%3)2·6H2O: Zr(NO3)4·
3H2O=5:3 mixed catalyst, the water dissolves for adding 10 times of amounts of mixed catalyst are obtained mixed catalytic agent solution, sealing and standing
24h；（3）Above-mentioned biomass are placed in example boat, being passed through nitrogen makes example boat air pressure in tubular type Muffle furnace reach 0-3MPa, close
Pyrolysis is closed, question response terminates to be cooled to room temperature taking-up；The pyrolysis is divided into two processes of low temperature pyrogenation and high temperature pyrolysis, Low Temperature Thermal
Solution preocess is first temperature to be increased into 100-300 DEG C, is pyrolyzed 30-120min, and high temperature pyrolysis process is to continue with being warming up to 300-800
DEG C, 60-200min is pyrolyzed, programming rate is 5-15 DEG C/min；（4）By the biological carbon of above-mentioned preparation and 5 times of biological carbon quality
Volumetric concentration is 1 ~ 20% H2O2Mix, mass volume ratio is biological carbon：H2O2=1:5,12h is shaken in an oscillator to be taken out, use
Distilled water cleans post-drying, that is, obtain high absorption property biological carbon.
Further, in order to improve the absorption property of biological carbon so that the stability of biological carbon more preferably, gap structure more preferably,
A kind of thunderbolt shell, the preparation method of chestnut shell biological carbon, it is characterised in that the thunderbolt shell, walnut shell mass ratio are excellent
Elect 1 as：2, thunderbolt shell, chestnut shell pulverize and sieve mesh number and are preferably 100 mesh, and the nitrogen that is passed through makes sample in tubular type Muffle furnace
Boat air pressure is preferably 1.5MPa, and the low temperature pyrogenation temperature is preferably 150 DEG C, and pyrolysis time is 60min, the high temperature pyrolysis temperature
Preferably 600 DEG C of degree, pyrolysis time are preferably 120min, the H2O2Volumetric concentration is preferably 10%.
The preparation method of a kind of thunderbolt shell, chestnut shell/limonite adsorbent, it is characterised in that it is to follow these steps to
It is obtained：
A. limonite is processed：
A1. the limonite of collection was crushed into 20～500 mesh sieves；
A2. by the salpeter solution immersion 12h that the wooden fish stone powder concentration after crushing is 0.1-10.0mol/L, mass volume ratio is
Wooden fish stone powder：Salpeter solution=1:10, take out；
A3. above-mentioned pretreated wooden fish stone powder is put into tubular type Muffle furnace, 2h is calcined under the conditions of 800 DEG C, taken out standby；
B. prepared by thunderbolt shell, chestnut shell/limonite adsorbent：
B1. by thunderbolt shell, chestnut shell biological carbon and the limonite powder mixing for standby use through pretreatment；
B2. polyvinyl alcohol and sodium alginate are mixed, 10 ~ 25min of heating makes dissolving, wooden fish stone powder and the thunderclap for preparing is added immediately
Thunderbolt shell, chestnut shell biological carbon are stirred into suspension, the sodium alginate：Polyvinyl alcohol：Limonite：Thunderbolt shell, plate
Chestnut shell biological carbon mass ratio is 1:1~10:1~12:1 ~ 20, continuously will with constant flow rate with constant flow pump after 10～60min of cooling
Hanging drop to weight/mass percentage composition is 1 ~ 10%CaCl2BAS in solidify, mass volume ratio is suspension：CaCl2's
Saturation BAS=1:10, hardening time be 5 ~ 40 h, after leach prepared complex microsphere, dry after being rinsed well with water standby；
B3. the complex microsphere of above-mentioned preparation is placed in tubular type Muffle furnace, it is 1 ~ 3MPa's to arrange temperature for 50 ~ 600 DEG C, pressure
The min of calcination 30 ~ 120 under environment, takes out, that is, obtain thunderbolt shell, chestnut shell/limonite adsorbent.
In order that above-mentioned adsorbent in water suspendability more preferably, be more evenly distributed, a kind of thunderbolt shell, chestnut shell/
The preparation method of limonite adsorbent, it is characterised in that：Limonite pulverizes and sieves and be further optimized for 100 mesh sieves in A1 steps；
Concentration of nitric acid is more preferably 3mol/L described in A2 steps；Add thermosol after polyvinyl alcohol and sodium alginate mixing in B2 steps
The solution time is more preferably 15min, sodium alginate：Polyvinyl alcohol：Limonite：Thunderbolt shell, chestnut shell biological carbon mass ratio
To be preferably 1：6：8：15, it is more preferably 30min, CaCl to make cool time after suspension2BAS quality
Percentage composition is more preferably 2%, and hardening time is more preferably 15h.
Further, temperature is set in B3 steps in tubular type Muffle furnace and is preferably 150 DEG C, pressure is preferably 1.5 MPa, calcination
Time is preferably 60min.
The present invention has following beneficial effect：
The present invention prepares the biological carbon of high absorption property using thunderbolt shell, chestnut shell mixed pyrolysis, and here is prepared on basis
Thunderbolt shell, chestnut shell/limonite complex microsphere, can further promote the recycling of waste material, realize the treatment of wastes with processes of wastes against one another
Purpose.Thunderbolt shell, chestnut shell are mixed with into biological carbon, it can be ensured that the absorption property of the biological carbon of preparation, improve biological
The clean-up effect of carbon.Purification test result indicate that, biological carbon to chromium in water, lead, methylene blue clearance may be up to 80.1%,
82.7%th, 85.2%, adsorbent may be up to 85.2,83.4%, 86.1% to the clearance of chromium in water, lead, methylene blue.Utilize
SA3100 types specific surface area and Porosimetry are tested the specific surface area and aperture that prepare biological carbon, and test result shows
Charcoal relevant parameter is excellent, and charcoal specific surface area, micro pore volume and total pore volume prepared by the present invention is reachable respectively
251.7m2/g、0.1301cm3/g、0.2972cm3/g。
Specific embodiment
The present invention is specifically described below by embodiment, it is necessary to it is pointed out here that be that following examples are only used
In being further described to the present invention, it is impossible to be interpreted as limiting the scope of the invention, person skilled in art can
So that some nonessential modifications and adaptations are made to the present invention according to foregoing invention content.
Embodiment 1
First, a kind of thunderbolt shell, chestnut shell/limonite adsorbent and preparation method thereof, is obtained as follows：
1st, biomass material pretreatment
By the thunderbolt shell of collection, broken 20 mesh sieves that sieve of chestnut shell.
2nd, preparation method
（1）Thunderbolt fruit shell after above-mentioned crushing, chestnut shell are pressed into quality 1：1 ratio is mixed（Thunderbolt fruit shell 100g, chestnut shell
100g）, add mass ratio Co (NO3)2·6H2O: Zr(NO3)4·3H2O=5:3 mixed catalytic agent solution（Take mixed catalytic
Agent 2g, adds 20ml water dissolves that mixed catalytic agent solution is obtained）, sealing and standing 24h.
（2）The example boat that the above-mentioned biomass material for processing is placed in tubular type Muffle furnace, being passed through nitrogen makes example boat
Middle atmospheric pressure reaches 1.5MPa, is pyrolyzed 60min under the conditions of being warming up to 200 DEG C with the programming rate of 10 DEG C/min, then is warming up to 600
120min is pyrolyzed under the conditions of DEG C.After pyrolytic reaction terminates, it is cooled to be taken out after room temperature.
（3）By the H that the biological carbon of above-mentioned preparation and concentration are 10%2O2Mix（Mass volume ratio is biological carbon：H2O2=1:
5）, taken out with 400r/min speed concussion 24h in an oscillator, clean drying with distilled water, that is, obtain high absorption property biological
Carbon.
（4）The nitric acid dousing 12 hours of the limonite of 20 mesh sieves 3mol/L will be crushed（Limonite 100g, nitric acid
1000ml）, take out and be placed in tubular type Muffle furnace, 2h is calcined under the conditions of 800 DEG C, take out standby.
（5）Polyvinyl alcohol and sodium alginate are mixed（Polyvinyl alcohol 10g, sodium alginate 10g）, heating for dissolving 15min, with
Wooden fish stone powder and the biological carbon of preparation is added to stir, the sodium alginate：Polyvinyl alcohol：Limonite：Charcoal quality
Than for 1：1：1：1, constant flow pump is used after cooling 10min with constant flow rate continuously by hanging drop to containing 2%（Contained with quality percentage
Gauge）CaCl2Saturation BAS in solidify（Mass volume ratio suspension：CaCl2Saturation BAS=1:10）Gu,
The change time is 5h, is taken out, and is dried after being rinsed well with water standby；
（6）The complex microsphere of above-mentioned preparation is placed in into tubular type Muffle furnace the min of calcination 60 under 150 DEG C, 1.5MPa, is prepared into
Thunderbolt shell, chestnut shell/limonite adsorbent.
By obtained thunderbolt shell, chestnut shell biological carbon SA3100 types specific surface area and Porosimetry contrast surface area
Tested with aperture, test result shows that charcoal specific surface area, micro pore volume and total pore volume are reachable respectively
241.7m2/g、0.1291cm3/g、0.2872cm3/g。
2nd, by thunderbolt shell obtained above, chestnut shell biological carbon and thunderbolt shell, chestnut shell/limonite adsorbent point
Purifying waste water processing is not carried out
Take 100mL concentration be 100.0mg/L self-control chromate waste water in 250ml beakers, add 1.0114g homemade thunderbolt
Fruit shell, chestnut shell biological carbon（It is 6 to adjust the initial pH of solution, back-ground electolyte NaNO3Concentration 0.01mol/L）, in 20 DEG C of bars
3h is shaken with 200r/min under part, taking-up is centrifuged 20min with 4000r/min, determines the content of chromium in water, can be obtained by calculating
Go out thunderbolt fruit shell, clearance of the chestnut shell biological carbon to chromium in waste water, separately take from thunderbolt shell processed, chestnut shell/limonite and inhale
Attached dose of 1.0241g, tests with method, and chromium in thunderbolt shell, chestnut shell/limonite Adsorbent For Removal of Heavy can be drawn by calculating
Clearance, experimental result is attached.
Take 100mL concentration be 100.0mg/L self-control lead waste water in 250ml beakers, add 1.01120g self-control
Thunderbolt fruit shell, chestnut shell biological carbon（It is 6 to adjust the initial pH of solution, back-ground electolyte NaNO3Concentration 0.01mol/L）,
3h is shaken with 200r/min under the conditions of 20 DEG C, is taken out and 20min is centrifuged with 4000r/min, determine the content of lead in water, by calculating
Thunderbolt fruit shell, clearance of the chestnut shell biological carbon to Pb In Exhausted Water can be drawn, separately take from thunderbolt shell processed, chestnut shell/wood
Fish stone adsorbent 1.0347g, tests with method, and thunderbolt shell, chestnut shell/limonite Adsorbent For Removal of Heavy can be drawn by calculating
The clearance of middle lead, experimental result is attached.
Take the self-control methylene blue waste water that 100mL concentration is 100.0mg/L adds 1.0226g to make by oneself in 250ml beakers
Thunderbolt fruit shell, chestnut shell biological carbon（It is 6 to adjust the initial pH of solution, back-ground electolyte NaNO3Concentration 0.01mol/L）,
3h is shaken with 200r/min under the conditions of 20 DEG C, is taken out and 20min is centrifuged with 4000r/min, determine water Methylene Blue content, passed through
Calculating can draw thunderbolt fruit shell, clearance of the chestnut shell biological carbon to water Methylene Blue.Separately take from thunderbolt shell processed, plate
Chestnut shell/limonite adsorbent 1.1018g, tests with method, and by calculating thunderbolt shell, chestnut shell/limonite absorption can be drawn
Clearance of the agent to methylene blue in waste, experimental result is attached.
3rd, experimental result
1st, to the removal of chromium
Thunderbolt fruit shell, chestnut shell biological carbon are 79.5% to the clearance of chromium, thunderbolt shell, chestnut shell/limonite adsorbent pair
The removal rate of chromium is 83.2%.
2nd, to the removal of lead
Thunderbolt fruit shell, chestnut shell biological carbon are 80.6% to the clearance of lead, thunderbolt shell, chestnut shell/limonite adsorbent pair
The removal rate of lead is 81.7%.
3rd, to the removal of methylene blue
Thunderbolt fruit shell, chestnut shell biological carbon are 83.5% to the clearance of methylene blue, and thunderbolt shell, chestnut shell/limonite is inhaled
The attached dose of removal rate to methylene blue is 84.9%.
Embodiment 2
First, a kind of thunderbolt shell, chestnut shell/limonite adsorbent, is obtained as follows：
1st, biomass material pretreatment：By the thunderbolt fruit shell of collection, broken 100 mesh sieves that sieve of chestnut shell.
2nd, preparation method
（1）By the thunderbolt fruit shell after above-mentioned crushing, chestnut shell in mass ratio 1：2 ratios are mixed（Thunderbolt fruit shell 50g, Chinese chestnut
Shell 100g）, add mass ratio Co (NO3)2·6H2O: Zr(NO3)4·3H2O=5:3 mixed catalytic agent solution（Take mixing to urge
Agent 1.5g, adds 15ml water dissolves that mixed catalytic agent solution is obtained）, sealing and standing 24h.
（2）The example boat that the above-mentioned biomass material for processing is placed in tubular type Muffle furnace, being passed through nitrogen makes example boat
Middle atmospheric pressure reaches 1.5MPa, is pyrolyzed 60min under the conditions of being warming up to 150 DEG C with the programming rate of 10 DEG C/min, then is warming up to 600
120min is pyrolyzed under the conditions of DEG C.After pyrolytic reaction terminates, it is cooled to be taken out after room temperature.
（3）By the H that the biological carbon of above-mentioned preparation and concentration are 10%2O2Mix（Mass volume ratio is biological carbon：H2O2=1:
5）, taken out with 400r/min speed concussion 24h in an oscillator, clean drying with distilled water, that is, obtain high absorption property biological
Carbon.
（4）The nitric acid dousing 12 hours of the limonite of 100 mesh sieves 3mol/L will be crushed（Limonite 100g, nitric acid
1000ml）, take out and be placed in tubular type Muffle furnace, 2h is calcined under the conditions of 800 DEG C, take out standby.
（5）Polyvinyl alcohol and sodium alginate are mixed（Polyvinyl alcohol 60g, sodium alginate 10g）, heating for dissolving 15min, with
Wooden fish stone powder and the biological carbon of preparation is added to stir, the sodium alginate：Polyvinyl alcohol：Limonite：Charcoal quality
Than for 1：6：8：15, constant flow pump is used after cooling 60min with constant flow rate continuously by hanging drop to containing 2%（Contained with quality percentage
Gauge）CaCl2Saturation BAS in solidify（Mass volume ratio suspension：CaCl2Saturation BAS=1:10）Gu,
The change time is 40h, is taken out, and is dried after being rinsed well with water standby；
（6）The complex microsphere of above-mentioned preparation is placed in into tubular type Muffle furnace the min of calcination 60 under 150 DEG C, 1.5MPa, is prepared into
Thunderbolt shell, chestnut shell/limonite adsorbent.
By obtained thunderbolt shell, chestnut shell biological carbon SA3100 types specific surface area and Porosimetry contrast surface area
Tested with aperture, test result shows that charcoal specific surface area, micro pore volume and total pore volume are reachable respectively
251.7m2/g、0.1301cm3/g、0.2972cm3/g。
2nd, by thunderbolt shell obtained above, chestnut shell biological carbon and thunderbolt shell, chestnut shell/limonite adsorbent point
Purifying waste water processing is not carried out（Experimental technique is shown in enforcement 1）
3rd, experimental result
1st, to the removal of chromium
Thunderbolt fruit shell, chestnut shell biological carbon consumption be 1.1021g, thunderbolt fruit shell, clearance of the chestnut shell biological carbon to chromium
For 80.1%, thunderbolt shell, chestnut shell/limonite adsorbent amount is 1.0124g, thunderbolt shell, chestnut shell/limonite absorption
Agent is 85.4% to the removal rate of chromium.
2nd, to the removal of lead
Thunderbolt fruit shell, chestnut shell biological carbon consumption be 1.1124g, thunderbolt fruit shell, clearance of the chestnut shell biological carbon to lead
For 82.7%, thunderbolt shell, chestnut shell/limonite adsorbent amount is 1.0157g, thunderbolt shell, chestnut shell/limonite absorption
Agent is 83.4% to the removal rate of lead.
3rd, to the removal of methylene blue
Thunderbolt fruit shell, chestnut shell biological carbon consumption are 1.1101g, and thunderbolt fruit shell, chestnut shell biological carbon are to methylene blue
Clearance is 85.2%, thunderbolt shell, chestnut shell/limonite adsorbent amount be 1.1183g, thunderbolt shell, chestnut shell/wooden fish
Stone adsorbent is 86.1% to the removal rate of methylene blue.
Embodiment 3
First, a kind of thunderbolt shell, chestnut shell/limonite adsorbent, is obtained as follows：
1st, biomass material pretreatment：By the thunderbolt fruit shell of collection, broken 200 mesh sieves that sieve of chestnut shell.
2nd, preparation method
（1）By the thunderbolt fruit shell after above-mentioned crushing, chestnut shell in mass ratio 1：10 ratios are mixed（Thunderbolt fruit shell 10g, Chinese chestnut
Shell 100g）, add mass ratio Co (NO3)2·6H2O: Zr(NO3)4·3H2O=5:3 mixed catalytic agent solution（Take mixing to urge
Agent 1.1g, adds 11ml water dissolves that mixed catalytic agent solution is obtained）, sealing and standing 24h.
（2）The example boat that the above-mentioned biomass material for processing is placed in tubular type Muffle furnace, being passed through nitrogen makes example boat
Middle atmospheric pressure reaches 1.5MPa, is pyrolyzed 60min under the conditions of being warming up to 200 DEG C with the programming rate of 10 DEG C/min, then is warming up to 600
120min is pyrolyzed under the conditions of DEG C.After pyrolytic reaction terminates, it is cooled to be taken out after room temperature.
（3）By the H that the biological carbon of above-mentioned preparation and concentration are 10%2O2Mix（Mass volume ratio is biological carbon：H2O2=1:
5）, taken out with 400r/min speed concussion 24h in an oscillator, clean drying with distilled water, that is, obtain high absorption property biological
Carbon.
（4）The nitric acid dousing 12 hours of the limonite of 100 mesh sieves 3mol/L will be crushed（Limonite 100g, nitric acid
1000ml）, take out and be placed in tubular type Muffle furnace, 2h is calcined under the conditions of 800 DEG C, take out standby.
（5）Polyvinyl alcohol and sodium alginate are mixed（Polyvinyl alcohol 100g, sodium alginate 10g）, heating for dissolving 15min,
Wooden fish stone powder and the biological carbon of preparation is added to stir immediately, the sodium alginate：Polyvinyl alcohol：Limonite：Biological carbonaceous
Amount is than being 1：10：12：20, constant flow pump is used after cooling 30min with constant flow rate continuously by hanging drop to containing 2%（With quality hundred
Divide content meter）CaCl2Saturation BAS in solidify（Mass volume ratio suspension：CaCl2Saturation BAS=1:
10）, hardening time is 15h, is taken out, and is dried after being rinsed well with water standby；
（6）The complex microsphere of above-mentioned preparation is placed in into tubular type Muffle furnace the min of calcination 60 under 150 DEG C, 1.5MPa, is prepared into
Thunderbolt shell, chestnut shell/limonite adsorbent.
By obtained thunderbolt shell, chestnut shell biological carbon SA3100 types specific surface area and Porosimetry contrast surface area
Tested with aperture, test result shows that charcoal specific surface area, micro pore volume and total pore volume are reachable respectively
247.5m2/g、0.1294cm3/g、0.2873cm3/g。
2nd, by thunderbolt shell obtained above, chestnut shell biological carbon and thunderbolt shell, chestnut shell/limonite adsorbent point
Purifying waste water processing is not carried out（Experimental technique is shown in enforcement 1）
3rd, experimental result
1st, to the removal of chromium
Thunderbolt fruit shell, chestnut shell biological carbon consumption be 1.1516g, thunderbolt fruit shell, clearance of the chestnut shell biological carbon to chromium
For 82.1%, thunderbolt shell, chestnut shell/limonite adsorbent amount is 1.1142g, thunderbolt shell, chestnut shell/limonite absorption
Agent is 84.7% to the removal rate of chromium.
2nd, to the removal of lead
Thunderbolt fruit shell, chestnut shell biological carbon consumption be 1.1347g, thunderbolt fruit shell, clearance of the chestnut shell biological carbon to lead
For 82.1%, thunderbolt shell, chestnut shell/limonite adsorbent amount is 1.2117g, thunderbolt shell, chestnut shell/limonite absorption
Agent is 83.1% to the removal rate of lead.
3rd, to the removal of methylene blue
Thunderbolt fruit shell, chestnut shell biological carbon consumption are 1.0009g, and thunderbolt fruit shell, chestnut shell biological carbon are to methylene blue
Clearance is 84.1%, thunderbolt shell, chestnut shell/limonite adsorbent amount be 1.4083g, thunderbolt shell, chestnut shell/wooden fish
Stone adsorbent is 85.6% to the removal rate of methylene blue.
Claims (5)
1. a kind of thunderbolt shell, the preparation method of chestnut shell biological carbon, it is characterised in that the charcoal be by thunderbolt shell and
Chestnut shell is obtained as follows：（1）Take thunderbolt shell, chestnut shell and crush 20～200 mesh sieves respectively, it is standby；（2）Will be above-mentioned
Thunderbolt shell, chestnut shell after crushing in mass ratio about 1～10：1 mixing, adds mixed catalytic agent solution, mixed catalytic
The compound method of agent solution is the mass ratio Co (NO for taking thunderbolt shell, chestnut shell powder gross mass 1%3)2·6H2O: Zr
(NO3)4·3H2O=5:3 mixed catalyst, the water dissolves for adding 10 times of amounts of mixed catalyst are obtained mixed catalytic agent solution, close
Envelope stands 24h；（3）By step（2）Material after middle sealing is static is placed in example boat, and being passed through nitrogen makes sample in tubular type Muffle furnace
Product boat air pressure reaches 0-3MPa, sealed pyrolysis, and question response terminates to be cooled to room temperature taking-up；The pyrolysis is divided into low temperature pyrogenation and height
Warm two processes of solution, Low Temperature Pyrolysis Process is first temperature to be increased into 100-300 DEG C, is pyrolyzed 30-120min, high temperature pyrolysis mistake
Journey is to continue with being warming up to 300-800 DEG C, is pyrolyzed 60-200min, and programming rate is 5-15 DEG C/min；（4）By the life of above-mentioned preparation
Thing carbon and the H that volumetric concentration is 1 ~ 20%2O2Mix, mass volume ratio is biological carbon：H2O2=1:5,12h is shaken in an oscillator
Take out, with distilled water post-drying is cleaned, that is, obtain high absorption property biological carbon.
2. as claimed in claim 1 a kind of thunderbolt shell, the preparation method of chestnut shell biological carbon, it is characterised in that the thunderclap
Thunderbolt shell, walnut shell mass ratio are preferably 1：2, thunderbolt shell, chestnut shell pulverize and sieve mesh number and are preferably 100 mesh, described logical
Entering nitrogen makes example boat air pressure in tubular type Muffle furnace be preferably 1.5MPa, and the low temperature pyrogenation temperature is preferably 150 DEG C, during pyrolysis
Between be 60min, the pyrolysis temperature be preferably 600 DEG C, pyrolysis time be preferably 120min, the H2O2Volumetric concentration is excellent
Elect 10% as.
3. the preparation method of a kind of thunderbolt shell, chestnut shell/limonite adsorbent, it is characterised in that it is to follow these steps to system
：
A. limonite is processed：
A1. the limonite of collection was crushed into 20～500 mesh sieves；
A2. the wooden fish stone powder after crushing is placed in into the salpeter solution immersion 12h that concentration is 0.1-10.0mol/L, mass volume ratio
For wooden fish stone powder：Salpeter solution=1:10, take out；
A3. above-mentioned pretreated wooden fish stone powder is put into tubular type Muffle furnace, 2h is calcined under the conditions of 800 DEG C, taken out standby；
B. prepared by thunderbolt shell, chestnut shell/limonite adsorbent：
B1. by thunderbolt shell, chestnut shell biological carbon and the limonite powder mixing for standby use through pretreatment；
B2. polyvinyl alcohol and sodium alginate are mixed, 10 ~ 25min of heating makes dissolving, wooden fish stone powder and the thunderclap for preparing is added immediately
Thunderbolt shell, chestnut shell biological carbon are stirred into suspension, the sodium alginate：Polyvinyl alcohol：Limonite：Thunderbolt shell, plate
Chestnut shell biological carbon mass ratio is 1:1~10:1~12:1 ~ 20, continuously will with constant flow rate with constant flow pump after 10～60min of cooling
Hanging drop to weight/mass percentage composition is 1 ~ 10%CaCl2BAS in solidify, mass volume ratio is suspension：CaCl2's
Saturation BAS=1:10, hardening time be 5 ~ 40 h, after leach prepared complex microsphere, dry after being rinsed well with water standby；
B3. the complex microsphere of above-mentioned preparation is placed in tubular type Muffle furnace, it is 1 ~ 3MPa's to arrange temperature for 50 ~ 600 DEG C, pressure
The min of calcination 30 ~ 120 under environment, takes out, that is, obtain thunderbolt shell, chestnut shell/limonite adsorbent.
4. as claimed in claim 3 a kind of thunderbolt shell, the preparation method of chestnut shell/limonite adsorbent, it is characterised in that：
Limonite pulverizes and sieves and be further optimized for 100 mesh sieves in A1 steps；Concentration of nitric acid is more preferably described in A2 steps
3mol/L；The heating for dissolving time is more preferably 15min after polyvinyl alcohol and sodium alginate mixing in B2 steps, alginic acid
Sodium：Polyvinyl alcohol：Limonite：Thunderbolt shell, chestnut shell biological carbon mass ratio are preferably 1：6：8：15, make cold after suspension
But the time is more preferably 30min, CaCl2The weight/mass percentage composition of BAS be more preferably 2%, hardening time
More preferably 15h.
5. a kind of thunderbolt shell as described in claim 3 or 4, the preparation method of chestnut shell/limonite adsorbent, its feature exists
In：Temperature is set in the B3 steps in tubular type Muffle furnace and is preferably 150 DEG C, pressure is preferably 1.5 MPa, and calcination time is preferred
For 60min.
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| CN201611201178.8A CN106622132A (en) | 2016-12-22 | 2016-12-22 | Muyu stone adsorbent with pili nut shell and chestnut shell and preparation method thereof |
| CN201710328788.2A CN106944001B (en) | 2016-12-22 | 2017-05-11 | Preparation method of biological carbon adsorbent |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107098329A (en) * | 2016-12-29 | 2017-08-29 | 重庆文理学院 | A kind of preparation method and applications of biological carbon |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107098329A (en) * | 2016-12-29 | 2017-08-29 | 重庆文理学院 | A kind of preparation method and applications of biological carbon |
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