CN106582524A - Pine nut shell, pistachio nut shell and wooden fish-like stone adsorbent and preparation method thereof - Google Patents
Pine nut shell, pistachio nut shell and wooden fish-like stone adsorbent and preparation method thereof Download PDFInfo
- Publication number
- CN106582524A CN106582524A CN201611201208.5A CN201611201208A CN106582524A CN 106582524 A CN106582524 A CN 106582524A CN 201611201208 A CN201611201208 A CN 201611201208A CN 106582524 A CN106582524 A CN 106582524A
- Authority
- CN
- China
- Prior art keywords
- shell
- fructus pistaciae
- pistaciae verae
- muyu
- stone
- 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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
-
- 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
-
- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28061—Surface area, e.g. B.E.T specific surface area being in the range 100-500 m2/g
-
- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28069—Pore volume, e.g. total pore volume, mesopore volume, micropore volume
- B01J20/28071—Pore volume, e.g. total pore volume, mesopore volume, micropore volume being less than 0.5 ml/g
-
- 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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- 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
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
-
- 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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (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)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a preparation method for pine nut shell and pistachio nut shell biomedical carbon. The method comprises the following steps of crashing pine nut shells and pistachio nut shells, and mixing the same; adding catalyst aqueous solution, and placing the reactants into a sample boat after sealing and standing; inputting nitrogen into the sample boat and pyrolyzing in a closed condition; after the reaction ends, cooling products to room temperature, taking the products out, and uniformly mixing the products with H2O2; and washing the products by shocking in an oscillator with distilled water and drying, thus acquiring high-adsorption biomedical carbon. According to the method provided by the invention, the pine nut shells and the pistachio nut shells are mixed for preparing the biomedical carbon, adsorption performance of the biomedical carbon can be ensured, and purification effect of the biomedical carbon can be improved. Purification experiment results show that removal rates of the biomedical carbon to chrome, lead and methylene blue in water can be up to 85.3%, 84.9% and 83.1%; the specific surface area and the pore size of the prepared biomedical carbon are tested by using an SA3100 specific surface area and pore size analyzer, a test result shows that the biomedical carbon has excellent related parameters, and the specific surface area, the micropore size and the overall pore size of the biomedical carbon prepared according to the method provided by the invention can respectively be up to 254.9m<2>/g, 0.1425cm<3>/g and 0.3001cm<3>/g.
Description
Technical field
The invention belongs to water treatment field, and in particular to a kind of chestnut shell, Fructus Pistaciae Verae shell/Muyu-Stone 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 hydropenia 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 anoxia or limited oxygen condition, is removed oily gentle rear remaining in biomass
Solid matter.Correlational study shows that charcoal has huge surface area and internal voids, with negative 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 garbage, 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 chestnut shell, the preparation method of Fructus Pistaciae Verae shell biological carbon.
Second object of the present invention is to provide a kind of chestnut shell, the preparation method of Fructus Pistaciae Verae shell/Muyu-Stone adsorbent.
The purpose of the present invention is realized by following technical measures：
The preparation method of a kind of chestnut shell, Fructus Pistaciae Verae shell biological carbon, it is characterised in that the charcoal is by chestnut shell and happy
Shell is obtained as follows：（1）Take chestnut shell, Fructus Pistaciae Verae shell and crush 20～200 mesh sieves respectively, it is standby；（2）By above-mentioned powder
Chestnut shell, Fructus Pistaciae Verae 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 chestnut shell, Fructus Pistaciae Verae shell powder gross mass 1%3)2·6H2O: Zr(NO3)4·
3H2O=5:3 mixed catalyst, the water dissolution for adding 10 times of amounts of mixed catalyst is 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 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）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,
The preparation method of a kind of chestnut shell, Fructus Pistaciae Verae shell biological carbon, it is characterised in that the chestnut shell, Fructus Pistaciae Verae shell mass ratio are excellent
Elect 1 as：1, chestnut 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 600 DEG C of degree, pyrolysis time are preferably 120min, the H2O2Volumetric concentration is preferably 10%.
The preparation method of a kind of chestnut shell, Fructus Pistaciae Verae shell/Muyu-Stone adsorbent, it is characterised in that it is to follow these steps to
It is obtained：
A. Muyu-Stone is processed：
A1. the Muyu-Stone 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 in tubular type Muffle furnace, 2h is calcined under the conditions of 800 DEG C, taken out standby；
B. prepared by chestnut shell, Fructus Pistaciae Verae shell/Muyu-Stone adsorbent：
B1. by chestnut shell, Fructus Pistaciae Verae shell biological carbon and the Muyu-Stone 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 plate for preparing is added immediately
Epicarpium Castaneae, Fructus Pistaciae Verae shell biological carbon are stirred into suspension, the sodium alginate：Polyvinyl alcohol：Muyu-Stone：It is chestnut 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 is 1 ~ 10%CaCl2Boric acid solution in solidify, mass volume ratio is suspension：CaCl2's
Saturation boric acid solution=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 chestnut shell, Fructus Pistaciae Verae shell/Muyu-Stone adsorbent.
In order that above-mentioned adsorbent in water suspendability more preferably, be more evenly distributed, a kind of chestnut shell, Fructus Pistaciae Verae shell/
The preparation method of Muyu-Stone adsorbent, it is characterised in that：Muyu-Stone 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 mixing post-heating are molten in B2 steps
The solution time is more preferably 15min, sodium alginate：Polyvinyl alcohol：Muyu-Stone：Chestnut shell, Fructus Pistaciae Verae shell biological carbon mass ratio
To be preferably 1：5：8：20, it is more preferably 30min, CaCl to make cool time after suspension2Boric acid solution 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 chestnut shell, Fructus Pistaciae Verae shell mixed pyrolysis, and here is prepared on basis
Chestnut shell, Fructus Pistaciae Verae shell/Muyu-Stone complex microsphere, can further promote the recycling of waste material, realize the treatment of wastes with processes of wastes against one another
Purpose.Chestnut shell, Fructus Pistaciae Verae 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 85.3%,
84.9%th, 83.1%, adsorbent may be up to 87.5%, 89.3%, 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
254.9m2/g、0.1425cm3/g、0.3001cm3/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 chestnut shell, Fructus Pistaciae Verae shell/Muyu-Stone adsorbent and preparation method thereof, is obtained as follows：
1st, biomass material pretreatment
By the chestnut shell of collection, broken 20 mesh sieves that sieve of Fructus Pistaciae Verae shell.
2nd, preparation method
（1）Thunderbolt fruit shell after above-mentioned crushing, Fructus Pistaciae Verae shell are pressed into quality 1：2 ratios are mixed（Chestnut 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 dissolutioies 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 Muyu-Stone of 20 mesh sieves 3mol/L will be crushed（Muyu-Stone 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：Muyu-Stone：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 boric acid solution in solidify（Mass volume ratio suspension：CaCl2Saturation boric acid solution=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
Chestnut shell, Fructus Pistaciae Verae shell/Muyu-Stone adsorbent.
By obtained chestnut shell, Fructus Pistaciae Verae 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
241.9m2/g、0.1281cm3/g、0.2712cm3/g。
2nd, by chestnut shell obtained above, Fructus Pistaciae Verae shell biological carbon and chestnut shell, Fructus Pistaciae Verae shell/Muyu-Stone 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 1.001g homemade Semen Castaneae
Shell, Fructus Pistaciae Verae 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 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
The clearance of chestnut shell, Fructus Pistaciae Verae shell biological carbon to chromium in waste water, separately takes from making sheet epicarpium Castaneae, Fructus Pistaciae Verae shell/Muyu-Stone adsorbent
1.0014g, tests with method, by calculating the removal that can draw chromium in chestnut shell, Fructus Pistaciae Verae shell/Muyu-Stone Adsorbent For Removal of Heavy
Rate, experimental result is attached.
Take 100mL concentration be 100.0mg/L self-control lead waste water in 250ml beakers, add 1.0211g it is homemade
Chestnut shell, Fructus Pistaciae Verae 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 in lead content, by calculate
The clearance of chestnut shell, Fructus Pistaciae Verae shell biological carbon to Pb In Exhausted Water is drawn, making sheet epicarpium Castaneae, Fructus Pistaciae Verae shell/Muyu-Stone is separately taken from and is inhaled
Attached dose of 1.1241g, tests with method, and lead in chestnut shell, Fructus Pistaciae Verae shell/Muyu-Stone Adsorbent For Removal of Heavy can be drawn by calculating
Clearance, experimental result is attached.
Take the self-control methylene blue waste water that 100mL concentration is 100.0mg/L adds 1.0027g to make by oneself in 250ml beakers
Chestnut shell, Fructus Pistaciae Verae shell biological carbon（It is 6 to adjust the initial pH of solution, 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 chestnut shell, Fructus Pistaciae Verae shell biological carbon to water Methylene Blue.Separately take from making sheet epicarpium Castaneae, Fructus Pistaciae Verae
Shell/Muyu-Stone adsorbent 1.1011g, tests with method, and chestnut shell, Fructus Pistaciae Verae shell/Muyu-Stone adsorbent can be drawn by calculating
Clearance to methylene blue in waste, experimental result is attached.
3rd, experimental result
1st, to the removal of chromium
Chestnut shell, Fructus Pistaciae Verae shell biological carbon are 82.3% to the clearance of chromium, and chestnut shell, Fructus Pistaciae Verae shell/Muyu-Stone adsorbent is to chromium
Removal rate be 83.7%.
2nd, to the removal of lead
Chestnut shell, Fructus Pistaciae Verae shell biological carbon are 81.9% to the clearance of lead, and chestnut shell, Fructus Pistaciae Verae shell/Muyu-Stone adsorbent is to lead
Removal rate be 86.1%.
3rd, to the removal of methylene blue
Chestnut shell, Fructus Pistaciae Verae shell biological carbon are 81.5% to the clearance of methylene blue, chestnut shell, Fructus Pistaciae Verae shell/Muyu-Stone absorption
Agent is 83.5% to the removal rate of methylene blue.
Embodiment 2
First, a kind of chestnut shell, Fructus Pistaciae Verae shell/Muyu-Stone adsorbent, is obtained as follows：
1st, biomass material pretreatment：By the chestnut shell of collection, broken 100 mesh sieves that sieve of Fructus Pistaciae Verae shell.
2nd, preparation method
（1）By the chestnut shell after above-mentioned crushing, Fructus Pistaciae Verae shell in mass ratio 1：1 ratio is mixed（Chestnut 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 dissolutioies 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 Muyu-Stone of 100 mesh sieves 3mol/L will be crushed（Muyu-Stone 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：Muyu-Stone：Charcoal 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 boric acid solution in solidify（Mass volume ratio suspension：CaCl2Saturation boric acid solution=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
Chestnut shell, Fructus Pistaciae Verae shell/Muyu-Stone adsorbent.
By obtained chestnut shell, Fructus Pistaciae Verae 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
254.9m2/g、0.1425cm3/g、0.3001cm3/g。
2nd, by chestnut shell obtained above, Fructus Pistaciae Verae shell biological carbon and chestnut shell, Fructus Pistaciae Verae shell/Muyu-Stone 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
Chestnut shell, Fructus Pistaciae Verae shell biological carbon consumption are 1.1101g, and chestnut shell, Fructus Pistaciae Verae shell biological carbon are to the clearance of chromium
85.3%, chestnut shell, Fructus Pistaciae Verae shell/Muyu-Stone adsorbent amount be 1.1011g, chestnut shell, Fructus Pistaciae Verae shell/Muyu-Stone adsorbent
It is 87.5% to the removal rate of chromium.
2nd, to the removal of lead
Chestnut shell, Fructus Pistaciae Verae shell biological carbon consumption are 1.1001g, and chestnut shell, Fructus Pistaciae Verae shell biological carbon are to the clearance of lead
84.9%, chestnut shell, Fructus Pistaciae Verae shell/Muyu-Stone adsorbent amount be 1.1157g, chestnut shell, Fructus Pistaciae Verae shell/Muyu-Stone adsorbent
It is 89.3% to the removal rate of lead.
3rd, to the removal of methylene blue
Chestnut shell, Fructus Pistaciae Verae shell biological carbon consumption be 1.1112g, the removal of chestnut shell, Fructus Pistaciae Verae shell biological carbon to methylene blue
Rate is 83.1%, and chestnut shell, Fructus Pistaciae Verae shell/Muyu-Stone adsorbent amount is 1.1121g, and chestnut shell, Fructus Pistaciae Verae shell/Muyu-Stone is inhaled
The attached dose of removal rate to methylene blue is 86.1%.
Embodiment 3
First, a kind of chestnut shell, Fructus Pistaciae Verae shell/Muyu-Stone adsorbent, is obtained as follows：
1st, biomass material pretreatment：By the chestnut shell of collection, broken 200 mesh sieves that sieve of Fructus Pistaciae Verae shell.
2nd, preparation method
（1）By the chestnut shell after above-mentioned crushing, Fructus Pistaciae Verae shell in mass ratio 1：10 ratios are mixed（Chestnut 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 dissolutioies 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 Muyu-Stone of 100 mesh sieves 3mol/L will be crushed（Muyu-Stone 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：Muyu-Stone：Biological carbonaceous
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 boric acid solution in solidify（Mass volume ratio suspension：CaCl2Saturation boric acid solution=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 in tubular type Muffle furnace the min of calcination 60 under 150 DEG C, 1.5MPa, is prepared into
Chestnut shell, Fructus Pistaciae Verae shell/Muyu-Stone adsorbent.
By obtained chestnut shell, Fructus Pistaciae Verae 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
242.3m2/g、0.1371cm3/g、0.2802cm3/g。
2nd, by chestnut shell obtained above, Fructus Pistaciae Verae shell biological carbon and chestnut shell, Fructus Pistaciae Verae shell/Muyu-Stone 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
Chestnut shell, Fructus Pistaciae Verae shell biological carbon consumption are 1.0116g, and chestnut shell, Fructus Pistaciae Verae shell biological carbon are to the clearance of chromium
82.7%, chestnut shell, Fructus Pistaciae Verae shell/Muyu-Stone adsorbent amount be 1.1041g, chestnut shell, Fructus Pistaciae Verae shell/Muyu-Stone adsorbent
It is 861% to the removal rate of chromium.
2nd, to the removal of lead
Chestnut shell, Fructus Pistaciae Verae shell biological carbon consumption are 1.1400g, and chestnut shell, Fructus Pistaciae Verae shell biological carbon are to the clearance of lead
83.9%, chestnut shell, Fructus Pistaciae Verae shell/Muyu-Stone adsorbent amount be 1.2140g, chestnut shell, Fructus Pistaciae Verae shell/Muyu-Stone adsorbent
It is 87.2% to the removal rate of lead.
3rd, to the removal of methylene blue
Chestnut shell, Fructus Pistaciae Verae shell biological carbon consumption be 1.0119g, the removal of chestnut shell, Fructus Pistaciae Verae shell biological carbon to methylene blue
Rate is 82.1%, and chestnut shell, Fructus Pistaciae Verae shell/Muyu-Stone adsorbent amount is 1.0683g, and chestnut shell, Fructus Pistaciae Verae shell/Muyu-Stone is inhaled
The attached dose of removal rate to methylene blue is 83.9%.
Claims (5)
1. a kind of chestnut shell, the preparation method of Fructus Pistaciae Verae shell biological carbon, it is characterised in that the charcoal is by chestnut shell and opens
Heart shell is obtained as follows：（1）Take chestnut shell, Fructus Pistaciae Verae shell and crush 20～200 mesh sieves respectively, it is standby；（2）Will be above-mentioned
Chestnut shell, Fructus Pistaciae Verae 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 chestnut shell, Fructus Pistaciae Verae shell powder gross mass 1%3)2·6H2O: Zr
(NO3)4·3H2O=5:3 mixed catalyst, the water dissolution for adding 10 times of amounts of mixed catalyst is 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 to 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 chestnut shell, the preparation method of Fructus Pistaciae Verae shell biological carbon, it is characterised in that the plate
Epicarpium Castaneae, Fructus Pistaciae Verae shell mass ratio are preferably 1：1, chestnut shell, Fructus Pistaciae Verae 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 chestnut shell, Fructus Pistaciae Verae shell/Muyu-Stone adsorbent, it is characterised in that it is to follow these steps to system
：
A. Muyu-Stone is processed：
A1. the Muyu-Stone 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 in tubular type Muffle furnace, 2h is calcined under the conditions of 800 DEG C, taken out standby；
B. prepared by chestnut shell, Fructus Pistaciae Verae shell/Muyu-Stone adsorbent：
B1. by chestnut shell, Fructus Pistaciae Verae shell biological carbon and the Muyu-Stone 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 plate for preparing is added immediately
Epicarpium Castaneae, Fructus Pistaciae Verae shell biological carbon are stirred into suspension, the sodium alginate：Polyvinyl alcohol：Muyu-Stone：It is chestnut 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 is 1 ~ 10%CaCl2Boric acid solution in solidify, mass volume ratio is suspension：CaCl2's
Saturation boric acid solution=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 chestnut shell, Fructus Pistaciae Verae shell/Muyu-Stone adsorbent.
4. as claimed in claim 3 a kind of chestnut shell, the preparation method of Fructus Pistaciae Verae shell/Muyu-Stone adsorbent, it is characterised in that：
Muyu-Stone 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；Polyvinyl alcohol and sodium alginate mixing post-heating dissolution time are more preferably 15min in B2 steps, alginic acid
Sodium：Polyvinyl alcohol：Muyu-Stone：Chestnut shell, Fructus Pistaciae Verae shell biological carbon mass ratio are preferably 1：5：8：20, make cold after suspension
But the time is more preferably 30min, CaCl2The weight/mass percentage composition of boric acid solution be more preferably 2%, hardening time
More preferably 15h.
5. a kind of chestnut shell as described in claim 3 or 4, the preparation method of Fructus Pistaciae Verae shell/Muyu-Stone 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.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611201208.5A CN106582524A (en) | 2016-12-22 | 2016-12-22 | Pine nut shell, pistachio nut shell and wooden fish-like stone 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 |
|---|---|---|---|
| CN201611201208.5A CN106582524A (en) | 2016-12-22 | 2016-12-22 | Pine nut shell, pistachio nut shell and wooden fish-like stone adsorbent and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106582524A true CN106582524A (en) | 2017-04-26 |
Family
ID=58603048
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611201208.5A Pending CN106582524A (en) | 2016-12-22 | 2016-12-22 | Pine nut shell, pistachio nut shell and wooden fish-like stone adsorbent and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106582524A (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 CN201611201208.5A patent/CN106582524A/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 |
|---|---|---|
| CN107096500A (en) | A kind of utilization Chinese medicine slag prepares the method for magnetic bio charcoal, magnetic bio charcoal and application | |
| CN105921110A (en) | Preparation method and application of cow dung biological carbon | |
| CN109603749B (en) | Preparation method and application of modified straw stalk biochar | |
| CN106179216A (en) | The preparation method of a kind of Magnetic Activated hydro-thermal charcoal and application | |
| CN106423051A (en) | Preparation method and application of magnetic activated hydrothermal biochar microspheres | |
| CN106732438A (en) | A kind of natural biomass adsorbent and preparation method and application | |
| CN102078791A (en) | Sludge activated carbon and preparation method thereof | |
| CN101829545A (en) | Heavy metal biological adsorbent using eggshell membrane as matrix and preparation method thereof | |
| CN104084126A (en) | Preparation method of biomass-based ferroaluminium complex spherical carbon | |
| CN107902653A (en) | For air purification and the shaddock peel activated carbon one-step preppn process of sewage disposal | |
| CN110142032A (en) | Chitosan biological carbon composite and its preparation method and application | |
| CN109317099A (en) | A kind of preparation method and application of load iron pig manure charcoal | |
| CN104275159B (en) | Preparation method of modified macadamia shell adsorbent | |
| CN102432144B (en) | Method for preparing microporous adsorbent from sludge, product and special equipment | |
| CN103830962B (en) | A kind of cordierite composite ceramic filter core and preparation method thereof | |
| CN106732365A (en) | A kind of thunderbolt shell, pinenut shell/limonite adsorbent and preparation method thereof | |
| CN106622135A (en) | Composite adsorbent and preparation method thereof | |
| CN106582528A (en) | High-adsorptivity biochar/tourmaline 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 | |
| CN106944001A (en) | A kind of preparation method of biological carbon adsorbent | |
| CN106582524A (en) | Pine nut shell, pistachio nut shell and wooden fish-like stone adsorbent and preparation method thereof | |
| CN108993393A (en) | A kind of preparation based on fish-bone biomass carbon greasy dirt adsorbent material | |
| CN106582584A (en) | Pine nut shell, hazelnut shell and Muyu stone adsorbent and preparation method thereof | |
| CN106582527A (en) | Biological carbon/tourmaline composite microspheres and preparation method thereof | |
| CN106732369A (en) | A kind of pinenut shell, Fructus Pistaciae Verae 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 | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170426 |