CN106732369A - A kind of pinenut shell, Fructus Pistaciae Verae shell/limonite adsorbent and preparation method thereof - Google Patents
A kind of pinenut shell, Fructus Pistaciae Verae shell/limonite adsorbent and preparation method thereof Download PDFInfo
- Publication number
- CN106732369A CN106732369A CN201611201425.4A CN201611201425A CN106732369A CN 106732369 A CN106732369 A CN 106732369A CN 201611201425 A CN201611201425 A CN 201611201425A CN 106732369 A CN106732369 A CN 106732369A
- Authority
- CN
- China
- Prior art keywords
- shell
- pinenut
- fructus pistaciae
- pistaciae verae
- biological carbon
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
-
- 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
-
- 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
- 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
-
- 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
-
- 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
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
A kind of pinenut shell, the preparation method of Fructus Pistaciae Verae shell biological carbon follow these steps to be obtained：Take pinenut shell, Fructus Pistaciae Verae shell to crush, mix, add aqueous catalyst solution, be placed in example boat after sealing and standing, be passed through nitrogen sealed pyrolysis, question response terminates to be cooled to room temperature taking-up and H2O2Mix, shaken in oscillator after distilled water is cleaned and dried, that is, obtain high absorption property biological carbon.Pinenut shell, Fructus Pistaciae Verae shell are mixed with biological carbon by the present invention, it can be ensured that the absorption property of the biological carbon of preparation, improve the clean-up effect of biological carbon.Purification test result indicate that, biological carbon may be up to 83.6%, 80.2%, 79.8% to the clearance of chromium in water, lead, methylene blue, the specific surface area and aperture that prepare biological carbon are tested using SA3100 types specific surface area and Porosimetry, test result shows that charcoal relevant parameter is excellent, and charcoal specific surface area, micro pore volume and total pore volume prepared by the present invention is respectively up to 234.1m2/g、0.1221cm3/g、0.2761cm3/g。
Description
Technical field
The invention belongs to water treatment field, and in particular to a kind of pinenut shell, Fructus Pistaciae Verae 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, oily gentle rear remaining in removal 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 turned into 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 used as the raw materials for preparing charcoal, but difference
Charcoal architectural difference prepared by biomass material and pyrolysis temperature is larger, and the absorption property to polluter is also different,
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
The purposive research that combination is optimized to biomass material to prepare in terms of high absorption property biological carbon.
The content of the invention
First purpose of the invention is to provide a kind of pinenut shell, the preparation method of Fructus Pistaciae Verae shell biological carbon.
Second object of the present invention is to provide a kind of pinenut shell, the preparation method of Fructus Pistaciae Verae shell/limonite adsorbent.
The purpose of the present invention is realized by following technical measures：
A kind of pinenut shell, the preparation method of Fructus Pistaciae Verae shell biological carbon, it is characterised in that the charcoal is by pinenut shell and happy
Shell is obtained as follows：（1）Take pinenut shell, Fructus Pistaciae Verae shell and crush 20~200 mesh sieves respectively, it is standby；（2）By above-mentioned powder
Pinenut shell, Fructus Pistaciae Verae shell after broken are 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 pinenut shell, Fructus Pistaciae Verae shell powder gross mass 1%3)2·6H2O: Zr(NO3)4·
3H2O=5:3 mixed catalyst, adds 10 times of water dissolves of amount of mixed catalyst that mixed catalytic agent solution, sealing and standing is obtained
24h；（3）Above-mentioned biomass are placed in example boat, example boat air pressure during nitrogen makes tubular type Muffle furnace are passed through and are reached 0-3MPa, it is 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 that temperature first is 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 is dried after cleaning, 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 pinenut shell, the preparation method of Fructus Pistaciae Verae shell biological carbon, it is characterised in that the pinenut shell, Fructus Pistaciae Verae shell mass ratio are excellent
Elect 1 as：5, pinenut shell, Fructus Pistaciae Verae 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 500 DEG C of degree, pyrolysis time are preferably 120min, the H2O2Volumetric concentration is preferably 10%.
The preparation method of a kind of pinenut shell, Fructus Pistaciae Verae shell/limonite adsorbent, it is characterised in that it is to follow these steps to
It is obtained：
A. limonite treatment：
A1. the limonite of collection was crushed into 20~500 mesh sieves；
A2. the salpeter solution that the wooden fish stone powder concentration after crushing is 0.1-10.0mol/L is soaked into 12h, 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 pinenut shell, Fructus Pistaciae Verae shell/limonite adsorbent：
B1. by pinenut shell, Fructus Pistaciae Verae shell biological carbon and the limonite powder mixing for standby use by pretreatment；
B2. polyvinyl alcohol and sodium alginate are mixed, 10 ~ 25min of heating makes dissolving, wooden fish stone powder and the pine for preparing is added immediately
Benevolence shell, Fructus Pistaciae Verae shell biological carbon are stirred into suspension, the sodium alginate：Polyvinyl alcohol：Limonite：It is pinenut shell, happy
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 be 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, dried after being rinsed well with water standby；
B3. the complex microsphere of above-mentioned preparation is placed in tubular type Muffle furnace, temperature is set for 50 ~ 600 DEG C, pressure are 1 ~ 3MPa's
The min of calcination 30 ~ 120 under environment, takes out, that is, obtain pinenut shell, Fructus Pistaciae Verae shell/limonite adsorbent.
In order that above-mentioned adsorbent in water suspendability more preferably, be more evenly distributed, a kind of pinenut shell, Fructus Pistaciae Verae 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；Polyvinyl alcohol and sodium alginate heat molten in B2 steps after mixing
The solution time is more preferably 15min, sodium alginate：Polyvinyl alcohol：Limonite：Pinenut shell, Fructus Pistaciae Verae shell biological carbon mass ratio
To be preferably 1：5：8：20, it is made cool time more preferably 30min, CaCl 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 pinenut shell, Fructus Pistaciae Verae shell mixed pyrolysis, is prepared on basis herein
Pinenut shell, Fructus Pistaciae Verae 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.Pinenut shell, Fructus Pistaciae Verae shell are mixed with 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 83.6%,
80.2%th, 79.8%, adsorbent may be up to 86.3%, 84.7%, 84.1% 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
234.1m2/g、0.1221cm3/g、0.2761cm3/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
It is further described in the present invention, it is impossible to be interpreted as limiting the scope of the invention, person skilled in art can
Some nonessential modifications and adaptations are made to the present invention with according to foregoing invention content.
Embodiment 1
First, a kind of pinenut shell, Fructus Pistaciae Verae shell/limonite adsorbent and preparation method thereof, is obtained as follows：
1st, biomass material pretreatment
Pinenut shell, Fructus Pistaciae Verae shell 20 mesh sieves of broken sieving that will be collected.
2nd, preparation method
（1）Pinenut shell after above-mentioned crushing, Fructus Pistaciae Verae shell are pressed into quality 1：1 ratio is mixed（Pinenut shell 100g, Fructus Pistaciae Verae 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 above-mentioned treated biomass material is placed in tubular type Muffle furnace, being passed through nitrogen makes example boat
Middle atmospheric pressure reaches 1.5MPa, is warming up to the programming rate of 10 DEG C/min and 60min is pyrolyzed under the conditions of 200 DEG C, then be warming up to 500
120min is pyrolyzed under the conditions of DEG C.After pyrolytic reaction terminates, taken out after being cooled to 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 of the limonite of 20 mesh sieves 3mol/L will be crushed 12 hours（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 being 1：1：1：1, use constant flow pump with constant flow rate continuously by hanging drop to containing 2% after cooling 10min（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 tubular type Muffle furnace in the min of calcination 60 under 150 DEG C, 1.5MPa, is prepared into
Pinenut shell, Fructus Pistaciae Verae shell/limonite adsorbent.
Obtained pinenut shell, Fructus Pistaciae Verae shell biological carbon are contrasted into surface area with SA3100 types specific surface area and Porosimetry
Tested with aperture, test result shows that charcoal specific surface area, micro pore volume and total pore volume are reachable respectively
231.1m2/g、0.1203cm3/g、0.2411cm3/g。
2nd, by pinenut shell obtained above, Fructus Pistaciae Verae shell biological carbon and pinenut shell, Fructus Pistaciae Verae 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 1.0117g homemade pinenut
Shell, Fructus Pistaciae Verae shell biological carbon（The initial pH of regulation solution is 6, back-ground electolyte NaNO3Concentration 0.01mol/L）, in 20 DEG C of conditions
Under 3h is shaken with 200r/min, take out and 20min be centrifuged with 4000r/min, determine the content of chromium in water, can draw by calculating
Pinenut shell, Fructus Pistaciae Verae shell biological carbon separately take from pinenut shell processed, Fructus Pistaciae Verae shell/limonite adsorbent to the clearance of chromium in waste water
1.0107g, is tested with method, and pinenut shell, Fructus Pistaciae Verae shell/removal of the limonite adsorbent to chromium in waste water can be drawn by calculating
Rate, experimental result is attached.
Take 100mL concentration be 100.0mg/L self-control lead waste water in 250ml beakers, add 1.0010g it is homemade
Pinenut shell, Fructus Pistaciae Verae shell biological carbon（The initial pH of regulation solution is 6, 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 in lead content, by calculate
The clearance of pinenut shell, Fructus Pistaciae Verae shell biological carbon to Pb In Exhausted Water is drawn, pinenut shell processed, Fructus Pistaciae Verae shell/limonite is separately taken from and is inhaled
Attached dose of 1.1204g, tests with method, pinenut shell, Fructus Pistaciae Verae shell/limonite adsorbent can be drawn to Pb In Exhausted Water by calculating
Clearance, experimental result is attached.
Take the self-control methylene blue waste water that 100mL concentration is 100.0mg/L adds 1.0127g to make by oneself in 250ml beakers
Pinenut shell, Fructus Pistaciae Verae shell biological carbon（The initial pH of regulation solution is 6, back-ground electolyte NaNO3Concentration 0.01mol/L）, 20
3h is shaken with 200r/min under the conditions of DEG C, is taken out and 20min is centrifuged with 4000r/min, determine water Methylene Blue content, by meter
Calculating can draw the clearance of pinenut shell, Fructus Pistaciae Verae shell biological carbon to water Methylene Blue.Separately take from pinenut shell processed, American pistachios
Shell/limonite adsorbent 1.0071g, is tested with method, and pinenut shell, Fructus Pistaciae Verae shell/limonite adsorbent can be drawn by calculating
To the clearance of methylene blue in waste, experimental result is attached.
3rd, experimental result
1st, to the removal of chromium
Pinenut shell, Fructus Pistaciae Verae shell biological carbon are 82.3% to the clearance of chromium, and pinenut shell, Fructus Pistaciae Verae shell/limonite adsorbent are to chromium
Removal rate be 84.2%.
2nd, to the removal of lead
Pinenut shell, Fructus Pistaciae Verae shell biological carbon are 79.1.9%, pinenut shell, Fructus Pistaciae Verae shell/limonite adsorbent pair to the clearance of lead
The removal rate of lead is 82.9%.
3rd, to the removal of methylene blue
Pinenut shell, Fructus Pistaciae Verae shell biological carbon are 79.2% to the clearance of methylene blue, pinenut shell, Fructus Pistaciae Verae shell/limonite absorption
Agent is 83.1% to the removal rate of methylene blue.
Embodiment 2
First, a kind of pinenut shell, Fructus Pistaciae Verae shell/limonite adsorbent, are obtained as follows：
1st, biomass material pretreatment：Pinenut shell, Fructus Pistaciae Verae shell 100 mesh sieves of broken sieving that will be collected.
2nd, preparation method
（1）By pinenut shell, the Fructus Pistaciae Verae shell in mass ratio 1 after above-mentioned crushing：5 ratios are mixed（Pinenut shell 50g, Fructus Pistaciae Verae shell
100g）, add mass ratio Co (NO3)2·6H2O: Zr(NO3)4·3H2O=5:3 mixed catalytic agent solution（Take mixed catalytic
Agent 1.5g, adds 15ml water dissolves that mixed catalytic agent solution is obtained）, sealing and standing 24h.
（2）The example boat that above-mentioned treated biomass material is placed in tubular type Muffle furnace, being passed through nitrogen makes example boat
Middle atmospheric pressure reaches 1.5MPa, is warming up to the programming rate of 10 DEG C/min and 60min is pyrolyzed under the conditions of 150 DEG C, then be warming up to 500
120min is pyrolyzed under the conditions of DEG C.After pyrolytic reaction terminates, taken out after being cooled to 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 of the limonite of 100 mesh sieves 3mol/L will be crushed 12 hours（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 being 1：5：8：20, use constant flow pump with constant flow rate continuously by hanging drop to containing 2% after cooling 60min（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 tubular type Muffle furnace in the min of calcination 60 under 150 DEG C, 1.5MPa, is prepared into
Pinenut shell, Fructus Pistaciae Verae shell/limonite adsorbent.
Obtained pinenut shell, Fructus Pistaciae Verae shell biological carbon are contrasted into surface area with SA3100 types specific surface area and Porosimetry
Tested with aperture, test result shows that charcoal specific surface area, micro pore volume and total pore volume are reachable respectively
234.1m2/g、0.1221cm3/g、0.2761cm3/g。
2nd, by pinenut shell obtained above, Fructus Pistaciae Verae shell biological carbon and pinenut shell, Fructus Pistaciae Verae shell/limonite adsorbent point
Purifying waste water processing is not carried out（Experimental technique is shown in implementation 1）
3rd, experimental result
1st, to the removal of chromium
Pinenut shell, Fructus Pistaciae Verae shell biological carbon consumption are 1.0006g, and pinenut shell, Fructus Pistaciae Verae shell biological carbon are to the clearance of chromium
83.6%, pinenut shell, Fructus Pistaciae Verae shell/limonite adsorbent amount are 1.0121g, pinenut shell, Fructus Pistaciae Verae shell/limonite adsorbent
Removal rate to chromium is 86.3%.
2nd, to the removal of lead
Pinenut shell, Fructus Pistaciae Verae shell biological carbon consumption are 1.0124g, and pinenut shell, Fructus Pistaciae Verae shell biological carbon are to the clearance of lead
80.2%, pinenut shell, Fructus Pistaciae Verae shell/limonite adsorbent amount are 1.0017g, pinenut shell, Fructus Pistaciae Verae shell/limonite adsorbent
Removal rate to lead is 84.7%.
3rd, to the removal of methylene blue
Pinenut shell, Fructus Pistaciae Verae shell biological carbon consumption are 1.0024g, the removal of pinenut shell, Fructus Pistaciae Verae shell biological carbon to methylene blue
Rate is 79.8%, and pinenut shell, Fructus Pistaciae Verae shell/limonite adsorbent amount are 1.0111g, and pinenut shell, Fructus Pistaciae Verae shell/limonite are inhaled
The attached dose of removal rate to methylene blue is 84.1%.
Embodiment 3
First, a kind of pinenut shell, Fructus Pistaciae Verae shell/limonite adsorbent, are obtained as follows：
1st, biomass material pretreatment：Pinenut shell, Fructus Pistaciae Verae shell 200 mesh sieves of broken sieving that will be collected.
2nd, preparation method
（1）By pinenut shell, the Fructus Pistaciae Verae shell in mass ratio 1 after above-mentioned crushing：10 ratios are mixed（Pinenut shell 10g, Fructus Pistaciae Verae shell
100g）, add mass ratio Co (NO3)2·6H2O: Zr(NO3)4·3H2O=5:3 mixed catalytic agent solution（Take mixed catalytic
Agent 1.1g, adds 11ml water dissolves that mixed catalytic agent solution is obtained）, sealing and standing 24h.
（2）The example boat that above-mentioned treated biomass material is placed in tubular type Muffle furnace, being passed through nitrogen makes example boat
Middle atmospheric pressure reaches 1.5MPa, is warming up to the programming rate of 10 DEG C/min and 60min is pyrolyzed under the conditions of 200 DEG C, then be warming up to 600
120min is pyrolyzed under the conditions of DEG C.After pyrolytic reaction terminates, taken out after being cooled to 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 of the limonite of 100 mesh sieves 3mol/L will be crushed 12 hours（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 1：5：12：20, use constant flow pump with constant flow rate continuously by hanging drop to containing 2% after cooling 30min（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 tubular type Muffle furnace in the min of calcination 60 under 150 DEG C, 1.5MPa, is prepared into
Pinenut shell, Fructus Pistaciae Verae shell/limonite adsorbent.
Obtained pinenut shell, Fructus Pistaciae Verae shell biological carbon are contrasted into surface area with SA3100 types specific surface area and Porosimetry
Tested with aperture, test result shows that charcoal specific surface area, micro pore volume and total pore volume are reachable respectively
226.1m2/g、0.1126cm3/g、0.2541cm3/g。
2nd, by pinenut shell obtained above, Fructus Pistaciae Verae shell biological carbon and pinenut shell, Fructus Pistaciae Verae shell/limonite adsorbent point
Purifying waste water processing is not carried out（Experimental technique is shown in implementation 1）
3rd, experimental result
1st, to the removal of chromium
Pinenut shell, Fructus Pistaciae Verae shell biological carbon consumption are 1.0006g, and pinenut shell, Fructus Pistaciae Verae shell biological carbon are to the clearance of chromium
81.7%, pinenut shell, Fructus Pistaciae Verae shell/limonite adsorbent amount are 1.1002g, pinenut shell, Fructus Pistaciae Verae shell/limonite adsorbent
Removal rate to chromium is 83.5%.
2nd, to the removal of lead
Pinenut shell, Fructus Pistaciae Verae shell biological carbon consumption are 1.0106g, and pinenut shell, Fructus Pistaciae Verae shell biological carbon are to the clearance of lead
80.5%, pinenut shell, Fructus Pistaciae Verae shell/limonite adsorbent amount are 1.0040g, pinenut shell, Fructus Pistaciae Verae shell/limonite adsorbent
Removal rate to lead is 82.2%.
3rd, to the removal of methylene blue
Pinenut shell, Fructus Pistaciae Verae shell biological carbon consumption are 1.0017g, the removal of pinenut shell, Fructus Pistaciae Verae shell biological carbon to methylene blue
Rate is 78.1%, and pinenut shell, Fructus Pistaciae Verae shell/limonite adsorbent amount are 1.0123g, and pinenut shell, Fructus Pistaciae Verae shell/limonite are inhaled
The attached dose of removal rate to methylene blue is 82.5%.
Claims (5)
1. a kind of pinenut shell, the preparation method of Fructus Pistaciae Verae shell biological carbon, it is characterised in that the charcoal is by pinenut shell and opens
Heart shell is obtained as follows：（1）Take pinenut shell, Fructus Pistaciae Verae shell and crush 20~200 mesh sieves respectively, it is standby；（2）Will be above-mentioned
Pinenut shell, Fructus Pistaciae Verae shell in mass ratio about 1~10 after crushing：1 mixing, adds mixed catalytic agent solution, mixed catalytic
The compound method of agent solution is the mass ratio Co (NO for taking pinenut shell, Fructus Pistaciae Verae shell powder gross mass 1%3)2·6H2O: Zr
(NO3)4·3H2O=5:3 mixed catalyst, adds 10 times of water dissolves of amount of mixed catalyst that mixed catalytic agent solution is obtained, 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 that temperature first is 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, dried after being cleaned with distilled water, that is, obtain high absorption property biological carbon.
2. as claimed in claim 1 a kind of pinenut shell, the preparation method of Fructus Pistaciae Verae shell biological carbon, it is characterised in that the pine
Benevolence shell, Fructus Pistaciae Verae shell mass ratio are preferably 1：5, pinenut shell, Fructus Pistaciae Verae shell pulverize and sieve mesh number and are preferably 100 mesh, described logical
Entering nitrogen makes example boat air pressure preferably 1.5MPa in tubular type Muffle furnace, and the low temperature pyrogenation temperature is preferably 150 DEG C, during pyrolysis
Between be 60min, the pyrolysis temperature is preferably 500 DEG C, pyrolysis time preferably 120min, the H2O2Volumetric concentration is excellent
Elect 10% as.
3. the preparation method of a kind of pinenut shell, Fructus Pistaciae Verae shell/limonite adsorbent, it is characterised in that it is to follow these steps to system
：
A. limonite treatment：
A1. the limonite of collection was crushed into 20~500 mesh sieves；
A2. the wooden fish stone powder after crushing is placed in the salpeter solution that concentration is 0.1-10.0mol/L and soaks 12h, mass volume ratio
It 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 pinenut shell, Fructus Pistaciae Verae shell/limonite adsorbent：
B1. by pinenut shell, Fructus Pistaciae Verae shell biological carbon and the limonite powder mixing for standby use by pretreatment；
B2. polyvinyl alcohol and sodium alginate are mixed, 10 ~ 25min of heating makes dissolving, wooden fish stone powder and the pine for preparing is added immediately
Benevolence shell, Fructus Pistaciae Verae shell biological carbon are stirred into suspension, the sodium alginate：Polyvinyl alcohol：Limonite：It is pinenut shell, happy
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 be 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, dried after being rinsed well with water standby；
B3. the complex microsphere of above-mentioned preparation is placed in tubular type Muffle furnace, temperature is set for 50 ~ 600 DEG C, pressure are 1 ~ 3MPa's
The min of calcination 30 ~ 120 under environment, takes out, that is, obtain pinenut shell, Fructus Pistaciae Verae shell/limonite adsorbent.
4. as claimed in claim 3 a kind of pinenut shell, the preparation method of Fructus Pistaciae Verae 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, alginic acid after polyvinyl alcohol and sodium alginate mix in B2 steps
Sodium：Polyvinyl alcohol：Limonite：Pinenut shell, Fructus Pistaciae Verae shell biological carbon mass ratio are preferably 1：5：8：20, it is made 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 pinenut shell as described in claim 3 or 4, the preparation method of Fructus Pistaciae Verae shell/limonite adsorbent, its feature exist
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
It is 60min.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611201425.4A CN106732369A (en) | 2016-12-22 | 2016-12-22 | A kind of pinenut shell, Fructus Pistaciae Verae shell/limonite adsorbent and preparation method thereof |
| CN201710328788.2A CN106944001B (en) | 2016-12-22 | 2017-05-11 | Preparation method of biological carbon adsorbent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611201425.4A CN106732369A (en) | 2016-12-22 | 2016-12-22 | A kind of pinenut shell, Fructus Pistaciae Verae shell/limonite adsorbent and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106732369A true CN106732369A (en) | 2017-05-31 |
Family
ID=58897358
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611201425.4A Pending CN106732369A (en) | 2016-12-22 | 2016-12-22 | A kind of pinenut shell, Fructus Pistaciae Verae shell/limonite adsorbent and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106732369A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107098329A (en) * | 2016-12-29 | 2017-08-29 | 重庆文理学院 | A kind of preparation method and applications of biological carbon |
-
2016
- 2016-12-22 CN CN201611201425.4A patent/CN106732369A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107098329A (en) * | 2016-12-29 | 2017-08-29 | 重庆文理学院 | A kind of preparation method and applications of biological carbon |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105921110A (en) | Preparation method and application of cow dung biological carbon | |
| CN109603749B (en) | Preparation method and application of modified straw stalk biochar | |
| CN107262037B (en) | A kind of preparation and application of sepiolite FeOOH active carbon compound adsorbent | |
| CN107096500A (en) | A kind of utilization Chinese medicine slag prepares the method for magnetic bio charcoal, magnetic bio charcoal and application | |
| CN101829545B (en) | Heavy metal biological adsorbent using eggshell membrane as matrix and preparation method thereof | |
| CN104651347B (en) | A kind of sulfate reduction bacteria immobilized particle and its preparation and application | |
| CN106179216A (en) | The preparation method of a kind of Magnetic Activated hydro-thermal charcoal and application | |
| CN102078791A (en) | Sludge activated carbon and preparation method thereof | |
| CN104084126A (en) | Preparation method of biomass-based ferroaluminium complex spherical carbon | |
| CN106732438A (en) | A kind of natural biomass adsorbent and preparation method and application | |
| CN105148856B (en) | Can be except material for air purification of formaldehyde, acetaldehyde, acetic acid and ammonia and preparation method thereof | |
| CN105692585B (en) | The carbon nanomaterial and its preparation method of a kind of graphene-containing structure and application | |
| CN109317099A (en) | A kind of preparation method and application of load iron pig manure charcoal | |
| CN106732365A (en) | A kind of thunderbolt shell, pinenut shell/limonite adsorbent and preparation method thereof | |
| CN106622135A (en) | Composite adsorbent and preparation method thereof | |
| CN110252247A (en) | A kind of spherical shape microballon shape walnut shell Quito hole carbon adsorbing material and its preparation method and application | |
| CN106582528A (en) | High-adsorptivity biochar/tourmaline adsorbent and preparation method thereof | |
| CN106944001A (en) | A kind of preparation method of biological carbon adsorbent | |
| CN106744949A (en) | A kind of method for preparing activated carbon as raw material with sesame stalk | |
| CN106732369A (en) | A kind of pinenut shell, Fructus Pistaciae Verae shell/limonite adsorbent and preparation method thereof | |
| CN103830965B (en) | Toughness reinforcing composite ceramic filter core of a kind of monkey grass and preparation method thereof | |
| CN106732370A (en) | A kind of hazelnut shell, Fructus Pistaciae Verae shell/limonite adsorbent and preparation method thereof | |
| CN108993393A (en) | A kind of preparation based on fish-bone biomass carbon greasy dirt adsorbent material | |
| CN106622132A (en) | Muyu stone adsorbent with pili nut shell and chestnut shell and preparation method thereof | |
| CN106622133A (en) | Pili nut shell and hazelnut shell/limonite adsorbent and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170531 |
|
| WD01 | Invention patent application deemed withdrawn after publication |