CN106902733A - A kind of preparation method of cotton leftover bits and pieces base load iron absorbent charcoal material - Google Patents
A kind of preparation method of cotton leftover bits and pieces base load iron absorbent charcoal material Download PDFInfo
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- CN106902733A CN106902733A CN201710081045.XA CN201710081045A CN106902733A CN 106902733 A CN106902733 A CN 106902733A CN 201710081045 A CN201710081045 A CN 201710081045A CN 106902733 A CN106902733 A CN 106902733A
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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
- B01J20/20—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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- 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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
- B01J20/0229—Compounds of Fe
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—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 physical properties
- B01J20/28009—Magnetic properties
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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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
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- 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
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Abstract
The invention discloses a kind of preparation method of cotton leftover bits and pieces base load iron absorbent charcoal material, i.e. with cotton leftover bits and pieces as raw material, make activator with iron chloride, cotton leftover bits and pieces base activated carbon containing iron is prepared using " one-step method ", i.e. collection charing, activation and supported ferriferous oxide is the process that carries out of a step prepares cotton leftover bits and pieces base load iron absorbent charcoal material.Gained cotton leftover bits and pieces base activated carbon containing iron has magnetic, can effectively remove Cr VI in water removal, i.e., repairing field in water pollution has a good application prospect.The problems such as preparation method solves cotton leftover bits and pieces pollution on the environment, and realize the recycling of cotton leftover bits and pieces.Using iron chloride as activator reduce preparation cost while, the cotton leftover bits and pieces base activated carbon containing iron recyclability that obtains is good, with added value of product and range of application higher.
Description
Technical field
Patent of the present invention is related to a kind of preparation method of activated carbon containing iron, and in particular to a kind of cotton leftover bits and pieces base load iron activity
The preparation method of Carbon Materials.
Background technology
Constantly increase with world population, society it is constantly progressive, the demand of textile also gradually increases, therefore, discard
The yield of textile also increases year by year.Wherein, the discarded cotton material of output when cotton leftover bits and pieces is cotton machining textile, if these are useless
Abandon cotton material mishandling, it is such as a large amount of to burn, fill or arbitrarily abandon, will necessarily directly or indirectly cause water body, air and soil
Environmental problem.Therefore, how discarded cotton material to be used, realizes that its recycling has important value.
Activated carbon is widely used to water process adsorbing domain as a kind of wide spectrum adsorbent.But conventional carbon has
Raw material（Such as shell, wooden）Relatively costly, adsorptive selectivity is poor, the problems such as adsorption capacity is relatively low.It is raw material energy with discarded object
Solve the problems, such as relatively costly in conventional carbon preparation process.The patent of Publication No. CN104071770A discloses a kind of profit
The method that porous Functional Carbon Fiber cluster is prepared with waste and old wollen fabrics, the method is successively through silane coupled by waste and old wollen fabrics
After agent, ammonium chloride solution, liquor zinci chloridi impregnation process, first in 150~300 DEG C of pre-oxidation, then completely cut off atmosphere temperature rising to 350~
950 DEG C carry out carbonization treatment, are changed into the porous Functional Carbon Fiber cluster that functional group is contained on surface, and discarded cotton material is switched into height
The absorbent charcoal material of absorption property, realizing turns waste into wealth, but the carbonization-activation temperature of the method is high, it is necessary at 550~950 DEG C
Carry out.And, liquor zinci chloridi has been used in preparation process, if the zinc ion in solution is discharged into natural water body, meeting and contain
Zinc complex ion participates in the replacement reaction in soil, often there is the fixed phenomenon of absorption.In addition, enrichment of the zinc in soil, will cause it
Enrichment in plant, this enrichment has harm to the humans and animals of plant and edible such plant.Excessive zinc can also
Soil enzyme is set to lose activity, number of bacteria is reduced, the microbial action in soil weakens.Ferriferous oxide is loaded into activated carbon
On, increase the active site position of carbon surface, increase ferriferous oxide and the contact area of pollutant, conventional carbon can be solved to pollution
The Selective adsorption of thing is poor, the problems such as adsorption capacity is relatively low.The patent of Publication No. CN104190360A individually discloses one kind
Oxidation-load iron-loaded modified activated carbon water treatment absorbent and preparation method thereof, the activated carbon containing iron iodine number that it is prepared is 417.46-
468.55 mg/g, specific surface area is 613.88-657.48 m2/g.Using phosphoric acid or the strong oxidizing property of nitric acid in preparation process,
Iron is introduced simultaneously（Hydrogen）Oxide, increases carbon surface functional group, improves suction of the activated carbon containing iron to metal ions such as Cr (VI)
Attached ability.
Paper Liu, Weifeng; Zhang, Chenglu; Zhang, Jian; Wang, Yifu; Li, Ye.
Adsorptive removal of Cr (VI) by Fe-modified activated carbon prepared
from Trapa natans husk. Chemical Engineering Journal. 2010;162(2):In 677- 684.
Propose to prepare biomass-based activated carbon using phosphoric acid activation, and secondary load is carried out using iron chloride and be modified, prepare and carry iron activity
Charcoal, its maximal absorptive capacity to Cr VI in water is 18.66 mg/g.
It is loaded modified that above patent and paper carry out iron primarily directed to commercial activated carbons or activated carbon from activated sludge, although carries
Its adsorptive selectivity high and adsorption capacity, but the step of increase secondary load, improve preparation cost.
For many defects present in existing activated carbon technology of preparing process, such as cost of material is higher, required activation temperature
Degree is high, the problems such as making activator with zinc chloride environment can be polluted.Meanwhile, conventional carbon has adsorptive selectivity poor,
Limited sorption capacity, the shortcoming being not easily recycled.Therefore, it is necessary to alternative lower-cost raw material is found, using to environment
The activator of less pollution, prepares that adsorption selectivity is excellent, and adsorption capacity is high and high added value of easy recycling is lived
Property charcoal.
Bibliography
[1] 、Liu, Weifeng; Zhang, Chenglu; Zhang, Jian; Wang, Yifu; Li, Ye.
Adsorptive removal of Cr (VI) by Fe-modified activated carbon prepared
from Trapa natans husk. Chemical Engineering Journal. 2010;162(2):677- 684.
The content of the invention
The invention aims to overcome, cost of material during existing activated carbon technology of preparing is higher, activation temperature is high
The defect such as big with the pollution produced when making activator with zinc chloride, and conventional carbon Selective adsorption is poor, adsorption capacity
It is low and reclaim difficult shortcoming, meanwhile, in order to reduce the technical problem such as the wasting of resources and its pollution to environment of cotton leftover bits and pieces
A kind of preparation method of cotton leftover bits and pieces base load iron absorbent charcoal material is provided, i.e., makees activator by with iron chloride, with cotton leftover bits and pieces
Be raw material, and use " one-step method ", that is, carbonize, activation and supported ferriferous oxide the process method that carries out simultaneously, be prepared into for
The cotton leftover bits and pieces base activated carbon containing iron of absorption degradation water body and heavy metal in soil.
Technical scheme
A kind of preparation method of cotton leftover bits and pieces base load iron absorbent charcoal material, i.e., with cotton leftover bits and pieces as raw material, activated with iron chloride
Agent, and it is the process that a step is carried out to prepare activated carbon containing iron, i.e. collection charing, activation and supported ferriferous oxide using " one-step method ",
The preparation method specifically includes following steps：
（1）, take cotton leftover bits and pieces, shred into appropriate size, preferably grow 0.5~1.0cm, obtain the first sample；
（2）, by iron chloride dissolving obtain in deionized water concentration be 200-800g/L ferric chloride in aqueous solution；
Again in iron chloride: the mass ratio of the first sample is 1~4: 1 ratio, step（1）In the first sample for obtaining be impregnated into
In the ferric chloride in aqueous solution of above-mentioned gained, taken out after 24~48h, obtain the second sample；
（3）, by step（2）In the second sample for obtaining control temperature to dry 24h under the conditions of 50~70 DEG C, obtain the 3rd sample
Product；
（4）, by step（3）In the 3rd sample that obtains be placed in tube furnace, control temperature under the effect of high-purity protective gas
Carbonized to continue 0.5~4.0h under the conditions of 300~500 DEG C, activated and supported ferriferous oxide, then naturally cooled to room temperature
After take out, obtain the 4th sample；
Described high-purity protective gas is nitrogen, helium, neon or argon gas；
（5）, by step（4）In the 4th sample that obtains be put into micro-boiling hydrochloric acid solution, taken out after embathing 10~30s, obtain the
Five samples；
Described hydrochloric acid solution, the mixed solution being made up of for the aqueous hydrochloric acid solution and water of 36-38% mass percent concentration,
Calculate by volume, mass percent concentration is the aqueous hydrochloric acid solution of 36-38%：Water is 1:9；
（6）, with deionized water by step（5）In the pH that is rinsed to efflux of the 5th sample that obtains be 6.5-7, obtain the
Six samples；
（7）, by step（6）In the 6th sample that obtains be placed in drying box, control temperature to dry 12 under the conditions of 70~90 DEG C
~24h, obtains final product cotton leftover bits and pieces base load iron absorbent charcoal material.
The cotton leftover bits and pieces base activated carbon containing iron of above-mentioned gained has magnetic after testing, can effectively remove Cr VI in water removal,
There is very strong absorption degradation ability to Cr VI, i.e., repairing field in water pollution has a good application prospect.
Beneficial effects of the present invention
The preparation method of a kind of cotton leftover bits and pieces base load iron absorbent charcoal material of the invention, because preparation process is with cotton leftover bits and pieces as former
Material, therefore have the advantages that cost of material is low, cotton leftover bits and pieces recycling is reduced in addition and is processed mishandling to environment
The technical problems such as the pollution for causing.
Further, the preparation method of a kind of cotton leftover bits and pieces base load iron absorbent charcoal material of the invention, because preparation process is adopted
Make activator with iron chloride, compared to zinc chloride, ferro element toxicity is relatively low, and the harm to environment is smaller, effectively eliminates useless
In water the problems such as pollution of the contained zinc ion in water environment.
Further, the preparation method of a kind of cotton leftover bits and pieces base load iron absorbent charcoal material of the invention, due to preparation process step
Suddenly（4）Collection charing, activation and supported ferriferous oxide are the process that a step is carried out, i.e., " one-step method " is completed, and the preparation
Temperature used is relatively low, therefore the preparation method has energy consumption low and the characteristics of small production cost.
Further, in the cotton leftover bits and pieces base load iron absorbent charcoal material obtained by preparation method of the invention, due to being loaded with iron
Oxide, mainly including di-iron trioxide（Fe2O3）, ferroso-ferric oxide（Fe3O4）Deng so that the activated carbon containing iron material has
There is certain magnetic, both improve its adsorption capacity to pollutant, its recycling is conducive to again.
Brief description of the drawings
The SEM of the cotton leftover bits and pieces used when preparing activated carbon containing iron in Fig. 1 a, embodiment 1 schemes；
The SEM figures of Fig. 1 b, the cotton leftover bits and pieces base activated carbon containing iron of the gained of embodiment 1；
The XPS figures of Fig. 2, the cotton leftover bits and pieces base activated carbon containing iron of the gained of embodiment 1；
The XRD of Fig. 3, the cotton leftover bits and pieces base activated carbon containing iron of the gained of embodiment 1.
Specific embodiment
The present invention is expanded on further below by specific embodiment and with reference to accompanying drawing, but is not intended to limit the present invention.
Embodiment 1
A kind of preparation method of cotton leftover bits and pieces base load iron absorbent charcoal material, specifically includes following steps：
（1）, take 5g cotton leftover bits and pieces, shred into size for 0.5~1.0cm, obtain the first sample；
（2）, take 15g iron chloride and be dissolved in 25mL deionized waters, configuration concentration is the ferric chloride in aqueous solution of 600g/L；
Again in iron chloride: the mass ratio of the first sample is 3: 1 ratio, step（1）In the first sample for obtaining be impregnated into
In the ferric chloride in aqueous solution of the above-mentioned gained of 25ml, taken out after 24h, obtain the second sample；
（3）, by step（2）In the second sample for obtaining be placed in drying box, 24h is dried under the conditions of 60 DEG C, then take out, obtain
To the 3rd sample；
（4）, by step（3）In the 3rd sample that obtains be placed in tube furnace, control temperature under the effect of high-purity protective gas
Carbonized to continue 1.0h under the conditions of 300 DEG C, activated and supported ferriferous oxide, taken out after then naturally cooling to room temperature, obtained
To the 4th sample；
Described high-purity protective gas is nitrogen, wherein nitrogen flow rate 100mLmin-1；
（5）, by step（4）In the 4th sample that obtains be put into micro-boiling hydrochloric acid solution, taken out after embathing 20s, obtain the 5th sample
Product；
Described hydrochloric acid solution, by the aqueous hydrochloric acid solution that mass percent concentration is 36% and the mixed solution that water is constituted, by body
Than calculating, mass percent concentration is 36% aqueous hydrochloric acid solution to product：Water is 1:9；
（6）, with deionized water by step（5）In the pH that is rinsed to efflux of the 5th sample that obtains be 6.5-7, obtain the
Six samples；
（7）, by step（6）In the 6th sample that obtains be placed in drying box, control temperature to dry 12h under the conditions of 80 DEG C, i.e.,
Obtain cotton leftover bits and pieces base load iron absorbent charcoal material 1.
Using FDAC S4800 SEM to the cotton leftover bits and pieces used in above-described embodiment 1 and implementation
The cotton leftover bits and pieces base activated carbon containing iron of gained is scanned in example 1, and the SEM figures of gained are respectively if Fig. 1 (a), Fig. 1 (b) are shown.
From Fig. 1 (a), Fig. 1 (b) as can be seen that script surface is in the cotton leftover bits and pieces of smooth state, after being activated by iron chloride, surface
Occur in that many cellular holes of presentation and pore passage structure.Result above shows that iron chloride is right in charing and activation process
The hole of cotton leftover bits and pieces is formed and played an important role.
Using Al (hv=1486.6 eV) as radiation source, using the silent winged generation that ESCALAB 250Xi type X-rays of U.S.'s match
Photoelectron spectrograph is measured to the cotton leftover bits and pieces base load iron absorbent charcoal material 1 of above-mentioned gained, and the XPS of gained is schemed such as Fig. 2 institutes
Show.From figure 2 it can be seen that occurring in that Photoelectron peak at 710.6 eV and 724.2 eV, α-Fe are attributed to2O3Middle Fe3+,
And the peak for combining energy 726.8 eV and 729.3 eV is then respectively belonging to Fe (III) 2p1/2With Fe (II) 2p1/2.Further, it is also possible to
Find out, a Photoelectron peak is also occurred in that in 714.6 eV, this can be attributed to the iron ion being complexed with electronegativity surface ligand.With
Upper result shows that the cotton leftover bits and pieces base load iron activated carbon surface obtained by preparation method of the present invention has loaded different types of iron oxidation
Thing.
According to wide-angle XRD method, using German Brooks D8 Advance x-ray diffractometers to the cotton of above-mentioned gained
Leftover bits and pieces base load iron absorbent charcoal material 1 is measured, and the XRD of gained is as shown in Figure 3.From figure 3, it can be seen that being in the angle of diffraction
Occur the characteristic peak of graphite peaks, i.e. activated carbon at 23 ° and 43 °, show that it is activity by final product after charcoal activation process
Charcoal, while also there is Fe in figure2O3And Fe3O4Characteristic peak, show that it has loaded various ferriferous oxides, that is, illustrate institute of the present invention
The cotton leftover bits and pieces base activated carbon containing iron for obtaining has certain magnetic, is conducive to its recycling.
Result above proves, above-mentioned steps（4）In, a step completes charing, three reactions of activation and supported ferriferous oxide.
Embodiment 2
A kind of preparation method of cotton leftover bits and pieces base load iron absorbent charcoal material, step is as follows：
In above-described embodiment 1, the mass ratio between iron chloride and cotton leftover bits and pieces is changed to 1: 1, other are same as Example 1, most
Cotton leftover bits and pieces base activated carbon containing iron 2 is obtained eventually.
Embodiment 3
A kind of preparation method of cotton leftover bits and pieces base load iron absorbent charcoal material, step is as follows：
In above-described embodiment 1, the mass ratio between iron chloride and cotton leftover bits and pieces is changed to 4: 1, other are same as Example 1, most
Cotton leftover bits and pieces base activated carbon containing iron 3 is obtained eventually.
Embodiment 4
A kind of preparation method of cotton leftover bits and pieces base load iron absorbent charcoal material, step is as follows：
In above-described embodiment 1, the heating-up temperature in tube furnace is changed to 400 DEG C, other are same as Example 1, finally give
Cotton leftover bits and pieces base activated carbon containing iron 4.
Embodiment 5
A kind of preparation method of cotton leftover bits and pieces base load iron absorbent charcoal material, step is as follows：
In above-described embodiment 1, the heating-up temperature in tube furnace is changed to 500 DEG C, other are same as Example 1, finally give
Cotton leftover bits and pieces base activated carbon containing iron 5.
Embodiment 6
A kind of preparation method of cotton leftover bits and pieces base load iron absorbent charcoal material, step is as follows：
In above-described embodiment 1, the heating duration in tube furnace is changed to 0.5h, other are same as Example 1, finally give cotton
Leftover bits and pieces base activated carbon containing iron 6.
Embodiment 7
A kind of preparation method of cotton leftover bits and pieces base load iron absorbent charcoal material, step is as follows：
In above-described embodiment 1, the heating duration in tube furnace is changed to 4h, other are same as Example 1, finally give under cotton
Heel base activated carbon containing iron 7.
Application Example 1
The cotton leftover bits and pieces base activated carbon containing iron of the gained of embodiment 1 is used for the absorption degradation to Cr VI, step is as follows：
（1）, take 50mL concentration for 100mgL-1Potassium bichromate solution be placed in centrifuge tube, weigh 0.1g realities with electronic balance
Apply the cotton leftover bits and pieces base load iron absorbent charcoal material prepared in example 1, and put into the potassium bichromate solution in centrifuge tube；
（2）, centrifuge tube is placed in shaking table, at 25 DEG C, 24h is reacted under the conditions of 150rpm；
（3）, take step（2）Supernatant in centrifuge tube, dilutes 50 times.
Measured using the plasma emission spectrometer Optima 8000 of PE companies of the U.S. six in the supernatant of above-mentioned gained
The concentration of valency chromium.The concentration that measurement obtains Cr VI in supernatant is 19.63mgL-1, while calculating, prepared by embodiment 1
Cotton leftover bits and pieces base load iron absorbent charcoal material be 80.37% to the degraded clearance of Cr VI, adsorbance is 40.2mg/g.
Above-mentioned Application Example 1 is also pressed to the cotton leftover bits and pieces base load iron absorbent charcoal material obtained by above-described embodiment 2-7 simultaneously
Mode, be measured its final removal ability to Cr VI in water, as a result show the cotton leftover bits and pieces base obtained by embodiment 2-7
Activated carbon containing iron material has very strong absorption degradation ability to Cr VI, and its degraded clearance to Cr VI is 74.20-
80.12 %, adsorbance is 34.1-39.8mg/g.It is indicated above the cotton leftover bits and pieces base load iron activity obtained by preparation method of the present invention
Carbon Materials are repaired field and are had a good application prospect in water pollution.
Using the assay method of GB/T 12496.8-1999 wood activated charcoal test method iodine sorption values to embodiment 1-7
The iodine number of the cotton leftover bits and pieces base load iron absorbent charcoal material of gained is measured, and iodine number is 358.12-456.23mg/g, particularly
Using the gained of embodiment 1 cotton leftover bits and pieces base load iron absorbent charcoal material when, iodine number is 456.23 mg/g to the maximum.In general iodine
Porosity its micropore ratio higher of value its material higher is also bigger, as a result shows, cotton leftover bits and pieces base load iron prepared by embodiment 1
Activated carbon has highest porosity and micropore ratio.It is indicated above that the cotton leftover bits and pieces base load obtained by preparation method of the invention
Iron absorbent charcoal material surface has abundant porosity and more microcellular structure.
It is right at a temperature of 77k using U.S.'s Kang Ta companies specific surface area and pore-size distribution analyzer autosorb-iQ-2MP
Cotton leftover bits and pieces base load iron absorbent charcoal material obtained by above-described embodiment 1-7 is analyzed measure, and specific surface area is 467.28-
630.97m2/g.Especially with the gained of embodiment 1 cotton leftover bits and pieces base load iron absorbent charcoal material when, specific surface area is to the maximum
630.97mg/g, shows the material pore-forming best results for preparing with this understanding.It is indicated above that preparation method gained of the invention
Cotton leftover bits and pieces base load iron absorbent charcoal material have specific surface area higher.
In sum, the present invention provide with cotton leftover bits and pieces as raw material, make activator with iron chloride, using " step is carried out
The cotton leftover bits and pieces base load iron activated carbon surface that charing, activation and supported ferriferous oxide method " is prepared forms good hole knot
Structure, with specific surface area higher, and is loaded with ferriferous oxide, is easy to improve it for Cr VI while recycling
Adsorption capacity.
The above is only the citing of embodiments of the present invention, it is noted that for the ordinary skill of the art
For personnel, on the premise of the technology of the present invention principle is not departed from, some improvement and modification can also be made, these improve and become
Type also should be regarded as protection scope of the present invention.
Claims (9)
1. a kind of preparation method of cotton leftover bits and pieces base load iron absorbent charcoal material, it is characterised in that described preparation method is with cotton
Heel is raw material, and activator is made with iron chloride, and collection charing, activation and supported ferriferous oxide carry out being prepared from cotton leftover bits and pieces for a step
Material base load iron absorbent charcoal material.
2. a kind of preparation method of cotton leftover bits and pieces base load iron absorbent charcoal material as claimed in claim 1, it is characterised in that specific
Comprise the following steps：
（1）, take cotton leftover bits and pieces, shred, obtain the first sample；
（2）, by iron chloride dissolving obtain in deionized water concentration be 200-800g/L ferric chloride in aqueous solution；
Again in iron chloride: the mass ratio of the first sample is 1~4: 1 ratio, step（1）In the first sample for obtaining be impregnated into
In the ferric chloride in aqueous solution of above-mentioned gained, taken out after 24~48h, obtain the second sample；
（3）, by step（2）In the second sample for obtaining control temperature to dry 24h under the conditions of 50~70 DEG C, obtain the 3rd sample
Product；
（4）, by step（3）In the 3rd sample that obtains be placed in tube furnace, control temperature under the effect of high-purity protective gas
Carbonized to continue 0.5~4.0h under the conditions of 300~500 DEG C, activated and supported ferriferous oxide, then naturally cooled to room temperature
After take out, obtain the 4th sample；
Described high-purity protective gas is nitrogen, helium, neon or argon gas；
（5）, by step（4）In the 4th sample that obtains be put into micro-boiling hydrochloric acid solution, taken out after embathing 10~30s, obtain the
Five samples；
Described hydrochloric acid solution, the mixed solution being made up of for the aqueous hydrochloric acid solution and water of 36-38% mass percent concentration,
Calculate by volume, mass percent concentration is the aqueous hydrochloric acid solution of 36-38%：Water is 1:9；
（6）, with deionized water by step（5）In the pH that is rinsed to efflux of the 5th sample that obtains be 6.5-7, obtain the
Six samples；
（7）, by step（6）In the 6th sample that obtains control temperature to dry 12~24h under the conditions of 70~90 DEG C, obtain final product under cotton
Heel base load iron absorbent charcoal material.
3. a kind of preparation method of cotton leftover bits and pieces base load iron absorbent charcoal material as claimed in claim 2, it is characterised in that step
（1）In cotton leftover bits and pieces, be cut into the fragment of 0.5~1.0cm long.
4. a kind of preparation method of cotton leftover bits and pieces base load iron absorbent charcoal material as claimed in claim 2, it is characterised in that step
（2）The concentration of middle configuration ferric chloride in aqueous solution is 600g/L；Step（2）Middle iron chloride: the mass ratio of the first sample is 3: 1.
5. a kind of preparation method of cotton leftover bits and pieces base load iron absorbent charcoal material as claimed in claim 4, it is characterised in that step
（3）It is middle by step（2）In the second sample for obtaining control temperature to be dried under the conditions of 60 DEG C.
6. a kind of preparation method of cotton leftover bits and pieces base load iron absorbent charcoal material as claimed in claim 5, it is characterised in that step
（4）In control temperature under the effect of high-purity protective gas for persistently 1.0h is carbonized, activated and load iron under the conditions of 300 DEG C
Oxide；
Described high-purity protective gas is nitrogen, wherein nitrogen flow rate 100mLmin-1。
7. a kind of preparation method of cotton leftover bits and pieces base load iron absorbent charcoal material as claimed in claim 6, it is characterised in that step
（5）It is middle by step（4）In the 4th sample that obtains be put into micro-boiling hydrochloric acid solution in embathe the time for 20s.
8. a kind of preparation method of cotton leftover bits and pieces base load iron absorbent charcoal material as claimed in claim 7, it is characterised in that step
（7）It is middle by step（6）In the 6th sample that obtains control temperature to dry 12h under the conditions of 80 DEG C.
9. a kind of cotton leftover bits and pieces base activated carbon containing iron material that the preparation method as described in claim 1-8 any claims is obtained
Expect for removing Cr VI in water removal.
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| CN112892475B (en) * | 2021-01-15 | 2023-02-28 | 仲恺农业工程学院 | Iron modified biochar and preparation method and application thereof |
| CN115634676A (en) * | 2022-12-17 | 2023-01-24 | 王翀 | Composite environment-friendly water purifying material |
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