CN106622135A - Composite adsorbent and preparation method thereof - Google Patents
Composite adsorbent and preparation method thereof Download PDFInfo
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- CN106622135A CN106622135A CN201611205195.9A CN201611205195A CN106622135A CN 106622135 A CN106622135 A CN 106622135A CN 201611205195 A CN201611205195 A CN 201611205195A CN 106622135 A CN106622135 A CN 106622135A
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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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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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B53/00—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form
- C10B53/02—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form of cellulose-containing material
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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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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
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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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
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Abstract
The invention provides a preparation method of a composite adsorbent. The preparation method of the composite adsorbent comprises steps as follows: pine nut shells and chestnut shells are taken, smashed and mixed, an aqueous catalyst solution is added, the raw materials are sealed, left to stand and then placed in a sample boat, nitrogen is introduced for closed pyrolysis, after reaction, a product is cooled to the room temperature and then is taken out and uniformly mixed with H2O2, a mixture is oscillated in an oscillator, washed with distilled water and dried, and biochar with high adsorption property is obtained; the composite adsorbent is prepared from the prepared biochar with high adsorption property and pretreated tourmaline through mixing. The prepared adsorbent has better adsorbing and purifying effects. A purification experiment result indicates that removal rate of chromium, lead and methylene blue in water by the prepared composite adsorbent can reach 85.9%, 87.1% and 86.0% respectively.
Description
Technical field
The invention belongs to water treatment field, and in particular to a kind of compound adsorbent and preparation method thereof.
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.
Biological carbon 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 biological carbon 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.Biological carbon research on utilization has become one of focus of environment and field of agricultural sciences research.Prepare the original of biological carbon
Material source is quite varied, and farmland discarded object, house refuse, excrement of animals etc. can be as the raw materials for preparing biological carbon but different
Biological carbon 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 preparation method of biological carbon.
Second object of the present invention is to provide a kind of compound attached dose preparation method.
The purpose of the present invention is realized by following technical measures：
A kind of preparation method of biological carbon, it is characterised in that the biological carbon is made as follows by pinenut shell and chestnut shell
：（1）Take pinenut shell, chestnut shell and crush 20～200 mesh sieves respectively, it is standby；（2）By pinenut shell, Chinese chestnut after above-mentioned crushing
Shell is 1～10 in mass ratio：1 mixing, adds mixed catalytic agent solution, and the compound method of mixed catalytic agent solution is to take pinenut
Mass ratio Co (the NO of shell, chestnut shell powder gross mass 1%3)2·6H2O: Zr(NO3)4·3H2O=5:3 mixed catalyst, plus
The water dissolves for entering 10 times of amounts of mixed catalyst are obtained mixed catalytic agent solution, sealing and standing 24h；（3）Above-mentioned biomass are placed in
In example boat, being passed through nitrogen makes example boat air pressure in tubular type Muffle furnace reach 0-3MPa, sealed pyrolysis, and question response terminates to be cooled to
Room temperature is taken out；The pyrolysis is divided into two processes of low temperature pyrogenation and high temperature pyrolysis, and Low Temperature Pyrolysis Process is first to be increased to temperature
100-300 DEG C, 30-120min is pyrolyzed, high temperature pyrolysis process is to continue with being warming up to 300-800 DEG C, is pyrolyzed 60-200min, heats up
Speed is 5-15 DEG C/min；（4）By the biological carbon of above-mentioned preparation and the H that the volumetric concentration of 5 times of biological carbon quality is 1 ~ 20%2O2It is mixed
Even, mass volume ratio is biological carbon：H2O2=1:5,12h is shaken in an oscillator to be taken out, clean post-drying with distilled water, 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,
The biomass material pinenut shell, shell mass ratio are preferably 1：3, pinenut shell, chestnut shell pulverize and sieve mesh number and are preferably 100
Mesh, the nitrogen that is passed through 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, pyrolysis time is 60min, the pyrolysis temperature be preferably 500 DEG C, pyrolysis time be preferably 120min, the H2O2Body
Product concentration is preferably 10%.
A kind of preparation method of compound adsorbent, it is characterised in that it is to follow these steps to be obtained：
A. tourmaline is processed：
A1. the tourmaline of collection was crushed into 20～500 mesh sieves；
A2. by the salpeter solution immersion 12h that the tourmaline powder concentration after crushing is 0.1-10.0mol/L, mass volume ratio is
Tourmaline powder：Salpeter solution=1:10, take out；
A3. above-mentioned pretreated tourmaline powder is put in tubular type Muffle furnace, 2h is calcined under the conditions of 800 DEG C, taken out standby；
B. prepared by compound adsorbent：
B1. by pinenut shell, chestnut shell biological carbon and the tourmaline powder mixing for standby use through pretreatment；
B2. polyvinyl alcohol and sodium alginate are mixed, 10 ~ 25min of heating makes dissolving, tourmaline powder and the pine for preparing is added immediately
Benevolence shell, chestnut shell biological carbon are stirred into suspension, the sodium alginate：Polyvinyl alcohol：Tourmaline：Pinenut shell, chestnut shell
Biological carbon mass ratio is 1:1~10:1~12:1 ~ 20, continuously will be suspended with constant flow rate with constant flow pump after 10～60min of cooling
Drop to weight/mass percentage composition is 1 ~ 10%CaCl2BAS in solidify, mass volume ratio is suspension：CaCl2Saturation
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 compound adsorbent.
In order that above-mentioned adsorbent in water suspendability more preferably, be more evenly distributed, a kind of preparation of compound adsorbent
Method, it is characterised in that：Tourmaline pulverizes and sieves and be further optimized for 100 mesh sieves in A1 steps；Nitric acid is dense described in A2 steps
Degree is more preferably 3mol/L；The heating for dissolving time is more preferably after polyvinyl alcohol and sodium alginate mix in B2 steps
15min, sodium alginate：Polyvinyl alcohol：Tourmaline：Biological carbon mass ratio is preferably 1：5：8：20, make and cooled down after suspension
Time is more preferably 30min, CaCl2The weight/mass percentage composition of BAS be more preferably 2%, hardening time enters
One step is 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 pinenut shell, chestnut shell mixed pyrolysis, prepares on here basis multiple
Adsorbent is closed, can further promote the recycling of waste material, realize the purpose of the treatment of wastes with processes of wastes against one another.By pinenut shell, chestnut shell
It is mixed with biological carbon, it can be ensured that the absorption property of the biological carbon of preparation, improves the clean-up effect of biological carbon.Purification experimental result
Show, biological carbon may be up to 82.4%, 84.3%, 82.7% to the clearance of chromium in water, lead, methylene blue, and adsorbent is in water
Chromium, lead, the clearance of methylene blue may be up to 85.9%, 87.1%, 86.0%.Using SA3100 types specific surface area and pore analysis
Instrument is tested the specific surface area and aperture that prepare biological carbon, and test result shows that biological carbon relevant parameter is excellent, the present invention
The biological carbon specific surface area of preparation, micro pore volume and total pore volume are respectively up to 253.1m2/g、0.1331cm3/g、
0.2847cm3/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 compound adsorbent and preparation method thereof, is obtained as follows：
1st, biomass material pretreatment
By the pinenut shell of collection, broken 20 mesh sieves that sieve of chestnut shell.
2nd, preparation method
（1）Pinenut shell after above-mentioned crushing, chestnut shell are pressed into quality 1：1 ratio is mixed（Pinenut shell 100g, chestnut shell 100g）, then
Add mass ratio Co (NO3)2·6H2O: Zr(NO3)4·3H2O=5:3 mixed catalytic agent solution（Mixed catalyst 2g is taken, plus
Enter 20ml water dissolves and 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 500
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 tourmaline of 20 mesh sieves 3mol/L will be crushed（Tourmaline 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
Tourmaline powder and the biological carbon of preparation is added to stir, the sodium alginate：Polyvinyl alcohol：Tourmaline：Biological carbon 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 in tubular type Muffle furnace the min of calcination 60 under 150 DEG C, 1.5MPa, is prepared into
Compound adsorbent.
By obtained pinenut shell, chestnut shell biological carbon with SA3100 types specific surface area and Porosimetry contrast surface area and
Aperture is tested, and test result shows biological carbon specific surface area, micro pore volume and total pore volume respectively up to 241.7m2/
g、0.1271cm3/g、0.2531cm3/g。
2nd, pinenut shell obtained above, chestnut shell biological carbon and compound adsorbent are carried out into respectively purifying waste water processing
Take 100mL concentration be 100.0mg/L self-control chromate waste water in 250ml beakers, add 1.0118g homemade pinenut
Shell, chestnut shell biological carbon（It is 6 to adjust the initial pH of solution, back-ground electolyte NaNO3Concentration 0.01mol/L）, under the conditions of 20 DEG C
3h is shaken with 200r/min, is taken out and 20min is centrifuged with 4000r/min, determine the content of chromium in water, pine can be drawn by calculating
The clearance of benevolence shell, chestnut shell biological carbon to chromium in waste water, separately takes from compound adsorbent 1.0121g processed, tests with method, by meter
Calculating can draw clearance of the compound adsorbent to chromium in waste water, and experimental result is attached.
Take 100mL concentration be 100.0mg/L self-control lead waste water in 250ml beakers, add 1.1121g it is homemade
Pinenut 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 lead in water, can be obtained by calculating
Go out the clearance of pinenut shell, chestnut shell biological carbon to Pb In Exhausted Water, separately take from compound adsorbent 1.0143g processed, test with method, lead to
Clearance of the compound adsorbent to Pb In Exhausted Water is drawn by crossing calculating, experimental result is attached.
Take the self-control methylene blue waste water that 100mL concentration is 100.0mg/L adds 1.0012g to make by oneself in 250ml beakers
Pinenut shell, chestnut shell biological carbon（It is 6 to adjust the initial pH of solution, back-ground electolyte NaNO3Concentration 0.01mol/L）, at 20 DEG C
Under the conditions of with 200r/min shake 3h, take out with 4000r/min be centrifuged 20min, determine water Methylene Blue content, by calculate
The clearance of pinenut shell, chestnut shell biological carbon to water Methylene Blue can be drawn.Compound adsorbent 1.0211g processed is separately taken from,
Test with method, clearance of the compound adsorbent to methylene blue in waste can be drawn by calculating, experimental result is attached.
3rd, experimental result
1st, to the removal of chromium
Pinenut shell, chestnut shell biological carbon are 80.2% to the clearance of chromium, and compound adsorbent is 82.7% to the removal rate of chromium.
2nd, to the removal of lead
Pinenut shell, chestnut shell biological carbon are 81.6% to the clearance of lead, and compound adsorbent is 83.6% to the removal rate of lead.
3rd, to the removal of methylene blue
Pinenut shell, chestnut shell biological carbon are 80.1% to the clearance of methylene blue, removal rate of the compound adsorbent to methylene blue
83.1%。
Embodiment 2
First, a kind of compound adsorbent, is obtained as follows：
1st, biomass material pretreatment：By the pinenut shell of collection, broken 100 mesh sieves that sieve of chestnut shell.
2nd, preparation method
（1）By pinenut shell, the chestnut shell in mass ratio 1 after above-mentioned crushing：3 ratios are mixed（Pinenut shell 50g, chestnut shell 100g）,
Add mass ratio Co (NO3)2·6H2O: Zr(NO3)4·3H2O=5:3 mixed catalytic agent solution（Take mixed catalyst
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 500
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 tourmaline of 100 mesh sieves 3mol/L will be crushed（Tourmaline 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
Tourmaline powder and the biological carbon of preparation is added to stir, the sodium alginate：Polyvinyl alcohol：Tourmaline：Biological carbon quality
Than for 1：5：8：20, 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 in tubular type Muffle furnace the min of calcination 60 under 150 DEG C, 1.5MPa, is prepared into
Compound adsorbent.
By obtained pinenut shell, chestnut shell biological carbon with SA3100 types specific surface area and Porosimetry contrast surface area and
Aperture is tested, and test result shows biological carbon specific surface area, micro pore volume and total pore volume respectively up to 253.1m2/
g、0.1331cm3/g、0.2847cm3/g。
2nd, pinenut shell obtained above, chestnut shell biological carbon and compound adsorbent are carried out into respectively purifying waste water processing（It is real
Proved recipe method is shown in enforcement 1）
3rd, experimental result
1st, to the removal of chromium
Pinenut shell, chestnut shell biological carbon consumption are 1.0106g, and pinenut shell, chestnut shell biological carbon are 82.4% to the clearance of chromium,
Compound adsorbent consumption is 1.0012g, and compound adsorbent is 85.9% to the removal rate of chromium.
2nd, to the removal of lead
Pinenut shell, chestnut shell biological carbon consumption are 1.0004g, and pinenut shell, chestnut shell biological carbon are 84.3% to the clearance of lead,
Compound adsorbent consumption is 1.0124g, and compound adsorbent is 87.1% to the removal rate of lead.
3rd, to the removal of methylene blue
Pinenut shell, chestnut shell biological carbon consumption are 1.2024g, and pinenut shell, chestnut shell biological carbon are to the clearance of methylene blue
82.7%, compound adsorbent consumption is 1.0141g, and compound adsorbent is 86.0% to the removal rate of methylene blue.
Embodiment 3
First, a kind of compound adsorbent, is obtained as follows：
1st, biomass material pretreatment：By the pinenut shell of collection, broken 200 mesh sieves that sieve of chestnut shell.
2nd, preparation method
（1）By pinenut shell, the chestnut shell in mass ratio 1 after above-mentioned crushing：10 ratios are mixed（Pinenut shell 10g, chestnut shell 100g）,
Add mass ratio Co (NO3)2·6H2O: Zr(NO3)4·3H2O=5:3 mixed catalytic agent solution（Take mixed catalyst
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 500
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 tourmaline of 100 mesh sieves 3mol/L will be crushed（Tourmaline 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,
Tourmaline powder and the biological carbon of preparation is added to stir immediately, the sodium alginate：Polyvinyl alcohol：Tourmaline：Biological carbon
Amount is than being 1：5：12：20, 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
In Muffle furnace under 150 DEG C, 1.5MPa the min of calcination 60, be prepared into compound adsorbent.
By obtained pinenut shell, chestnut shell biological carbon with SA3100 types specific surface area and Porosimetry contrast surface area and
Aperture is tested, and test result shows biological carbon specific surface area, micro pore volume and total pore volume respectively up to 243.2m2/
g、0.1201cm3/g、0.2349cm3/g。
2nd, pinenut shell obtained above, chestnut shell biological carbon and compound adsorbent are carried out into respectively purifying waste water processing（It is real
Proved recipe method is shown in enforcement 1）
3rd, experimental result
1st, to the removal of chromium
Pinenut shell, chestnut shell biological carbon consumption are 1.0021g, and pinenut shell, chestnut shell biological carbon are 81.1% to the clearance of chromium,
Compound adsorbent consumption is 1.0008g, and compound adsorbent is 82.4% to the removal rate of chromium.
2nd, to the removal of lead
Pinenut shell, chestnut shell biological carbon consumption are 1.0006g, and pinenut shell, chestnut shell biological carbon are 82.5% to the clearance of lead,
Compound adsorbent consumption is 1.0021g, and compound adsorbent is 83.1% to the removal rate of lead.
3rd, to the removal of methylene blue
Pinenut shell, chestnut shell biological carbon consumption are 1.0102g, and pinenut shell, chestnut shell biological carbon are to the clearance of methylene blue
79.2%, compound adsorbent consumption is 1.0004g, and compound adsorbent is 82.1% to the removal rate of methylene blue.
Claims (5)
1. a kind of preparation method of biological carbon, it is characterised in that the biological carbon be by pinenut shell and chestnut shell as follows
It is obtained：（1）Take pinenut shell, chestnut shell and crush 20～200 mesh sieves respectively, it is standby；（2）By pinenut shell, plate after above-mentioned crushing
Chestnut shell in mass ratio about 1～10：1 mixing, adds mixed catalytic agent solution, and the compound method of mixed catalytic agent solution is to take
Mass ratio Co (the NO of pinenut shell, chestnut shell powder gross mass 1%3)2·6H2O: Zr(NO3)4·3H2O=5:3 mixed catalytic
Agent, the water dissolves for adding 10 times of amounts of mixed catalyst are obtained mixed catalytic agent solution, sealing and standing 24h；（3）By step（2）In
Material after sealing is static is placed in example boat, and being passed through nitrogen makes example boat air pressure in tubular type Muffle furnace reach 0-3MPa, closed
Pyrolysis, 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 pyrogenation
Process is first temperature to be increased to 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）It is 1 ~ 20% by the biological carbon of above-mentioned preparation and volumetric concentration
H2O2Mix, mass volume ratio is biological carbon：H2O2=1:5,12h is shaken in an oscillator to be taken out, dry after being cleaned with distilled water
It is dry, that is, obtain high absorption property biological carbon.
2. a kind of preparation method of biological carbon as claimed in claim 1, it is characterised in that the pinenut shell, walnut shell quality
Ratio is preferably 1：3, pinenut shell, chestnut shell pulverize and sieve mesh number and are preferably 100 mesh, and the nitrogen that is passed through is made in tubular type Muffle furnace
Example 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 warm
Solution temperature be preferably 500 DEG C, pyrolysis time be preferably 120min, the H2O2Volumetric concentration is preferably 10%.
3. a kind of preparation method of compound adsorbent adsorbent, it is characterised in that it is to follow these steps to be obtained：
A. tourmaline is processed：
A1. the tourmaline of collection was crushed into 20～500 mesh sieves；
A2. the tourmaline powder after crushing is placed in into the salpeter solution immersion 12h that concentration is 0.1-10.0mol/L, mass volume ratio
For tourmaline powder：Salpeter solution=1:10, take out；
A3. above-mentioned pretreated tourmaline powder is put in tubular type Muffle furnace, 2h is calcined under the conditions of 800 DEG C, taken out standby；
B. prepared by compound adsorbent：
B1. by pinenut shell, chestnut shell biological carbon and the tourmaline powder mixing for standby use through pretreatment；
B2. polyvinyl alcohol and sodium alginate are mixed, 10 ~ 25min of heating makes dissolving, tourmaline powder and the pine for preparing is added immediately
Benevolence shell, chestnut shell biological carbon are stirred into suspension, the sodium alginate：Polyvinyl alcohol：Tourmaline：Pinenut shell, chestnut shell
Biological carbon mass ratio is 1:1~10:1~12:1 ~ 20, continuously will be suspended with constant flow rate with constant flow pump after 10～60min of cooling
Drop to weight/mass percentage composition is 1 ~ 10%CaCl2BAS in solidify, mass volume ratio is suspension：CaCl2Saturation
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 compound adsorbent.
4. the preparation method of compound adsorbent as claimed in claim 3, it is characterised in that：Tourmaline pulverizes and sieves in A1 steps
Further it is optimized for 100 mesh sieves；Concentration of nitric acid is more preferably 3mol/L described in A2 steps；In B2 steps polyvinyl alcohol and
The heating for dissolving time is more preferably 15min after sodium alginate mixing, sodium alginate：Polyvinyl alcohol：Tourmaline：Pinenut shell,
Chestnut shell biological carbon mass ratio is preferably 1：5：8：20, it is more preferably 30min to make cool time after suspension,
CaCl2The weight/mass percentage composition of BAS be more preferably 2%, hardening time is more preferably 15h.
5. the preparation method of a kind of compound adsorbent as described in claim 3 or 4, it is characterised in that：Manage in the B3 steps
Temperature is set in formula Muffle furnace and is preferably 150 DEG C, pressure is preferably 1.5 MPa, and calcination time is preferably 60min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109487895A (en) * | 2018-11-02 | 2019-03-19 | 珠海南德海绵城市建设管理有限公司 | A kind of dedicated water storage sustained release module in sponge city |
| CN113019317A (en) * | 2021-01-20 | 2021-06-25 | 桂林理工大学 | Bimetal-loaded activated carbon high-performance adsorbent and preparation method and application thereof |
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2016
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109487895A (en) * | 2018-11-02 | 2019-03-19 | 珠海南德海绵城市建设管理有限公司 | A kind of dedicated water storage sustained release module in sponge city |
| CN113019317A (en) * | 2021-01-20 | 2021-06-25 | 桂林理工大学 | Bimetal-loaded activated carbon high-performance adsorbent and preparation method and application thereof |
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