CN106540666A - The preparation method of the modified Carbon Materials of Adsorption of Heavy Metal Ions silk cocoon - Google Patents
The preparation method of the modified Carbon Materials of Adsorption of Heavy Metal Ions silk cocoon Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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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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- 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
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
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Abstract
The invention discloses a kind of preparation method of the modified Carbon Materials of Adsorption of Heavy Metal Ions silk cocoon, belongs to feature charing sorbing material technical field.The preparation method of the modified Carbon Materials of Adsorption of Heavy Metal Ions silk cocoon, step is：With silk cocoon as raw material, modified to carbonize in Muffle furnace, shown charing is that, from 20 DEG C of ramps with 2 DEG C/min to 100 DEG C, insulation 120min is raised to 200 DEG C from 100 DEG C of speed with 1 DEG C/min again, and the modified Carbon Materials of silk cocoon are obtained final product after insulation 120min.The present invention carries out low-temperature carbonization and Carbon Materials is obtained with silk cocoon as raw material after modified process, yield is high, and pollution is few, and the absorption property of product heavy metal ion is good.
Description
Technical field
The invention belongs to feature charing sorbing material technical field, and in particular to a kind of Adsorption of Heavy Metal Ions silk cocoon changes
The preparation method of property Carbon Materials.
Background technology
Carbon Materials have highly developed pore structure and huge specific surface area, with acid and alkali-resistance, water insoluble, easy
The features such as regeneration, as which has the advantages that degree for the treatment of height and stable effluent quality when sewage is processed, and it is widely used in
Water-treatment technology field.When for water process, Carbon Materials can be used to purify source of sewage, the main color included removing in sewage,
Smell, taste and organic matter etc.；The inorganic matter in Adsorption water is can be used to simultaneously, mainly the huge sum of money such as including Cu2+, Pd2+, Cd2+
Category ion；It can in addition contain the organic matter gone in eliminating water, mainly including BOD, COD and the organic matter of some difficult degradations.
The absorption property of Carbon Materials is affected mainly there are two aspect factors：One is pore structure, such as specific surface area, aperture and hole point
Cloth etc., to a certain extent, can be by the reaction conditions such as the selection of raw material, activated media, temperature, time adjustment control Carbon Materials
The pore structure and pore-size distribution of material；Two is surface chemical structure, such as species and content of surface functional group etc., it and adsorptivity
The Relationship Comparison complexity of energy still needs to be understood in depth；Additionally, adsorbance is also relevant with the characteristic of adsorption molecule itself.
Silk is one of maximum natural fiber of current yield in the world, mainly by 2 kinds of protein of fibroin albumen and silk gum
Composition.Fibroin albumen is main part in silk, accounts for the 70% of gross weight, and has the characteristics of can be easily separated purification,
Fibroin albumen after purification have it is many uniqueness physicochemical properties and excellent biocompatibility, can prepare film forming, gel,
The variforms such as microcapsules.Therefore, fibroin albumen is in biomedical sector, especially defeated in tissue engineering bracket material, medicine
Send, the aspect such as medical dressing has huge application potential.Fibroin albumen is kind of a high molecular weight protein, comprises more than 5000
Amino acid, its main peptide chain great majority are made up of the low glycine of reactivity and alanine, however, still have substantial amounts of can make
Active group for the center that is modified is present in the main peptide chain of fibroin albumen amino acid and side chain, as accounted for mass percent 12.1%
Serine, the hydroxyl of threonine (0.9%), the phenolic hydroxyl group of tyrosine (5.3%), aspartic acid (0.5%) and glutamic acid (0.6%)
Amino of carboxyl, the guanidine radicals of arginine (0.3%) and lysine (0.2%) etc..
Conventional chemical modification method has grafting, copolymerization and modification, interpenetrating networks modified and cross-linking modified etc..Generally,
Its some side base can be changed by chemical reaction, or other functions group, such as sulfonic group, phosphorus are introduced by the reaction with side base
Acidic group, epoxy radicals etc. carry out chemical modification to fibroin albumen.
The content of the invention
It is an object of the invention to provide a kind of preparation method of the modified Carbon Materials of Adsorption of Heavy Metal Ions silk cocoon.
The present invention processes silk cocoon with formaldehyde crosslinking and the modified Jing of Lauxite respectively with silk cocoon as raw material, nitrogenous to increase
Functional group and pore structure is easily formed, better performances can be obtained by low-temperature carbonization, suitable for Adsorption of Heavy Metal Ions raw material of wood-charcoal
Material.
The present invention is achieved by the following technical solutions：
A kind of preparation method of the modified Carbon Materials of the silk cocoon of Adsorption of Heavy Metal Ions：
With silk cocoon as raw material, it is modified Muffle furnace carbonize, shown charing be from 20 DEG C of ramps with 2 DEG C/min to
100 DEG C, insulation 120min is raised to 200 DEG C from 100 DEG C of speed with 1 DEG C/min again, obtains final product silk cocoon Modified Activated Carbon after insulation 120min
Material.
Further, it is described it is modified be that formaldehyde crosslinking is modified, specifically silk cocoon is shredded, with NaHCO3, and formalin
Mix in there-necked flask in solution, under the conditions of 95 DEG C after magnetic agitation reaction 5h, remove condenser pipe, tailing adapter reaction
0.5h, wherein the mass concentration of described formalin is 37%, described silk cocoon：NaHCO3Mass ratio be 3:3.6, institute
The silk cocoon stated is 3 with the mass volume ratio of formalin:7,
It is described it is modified hydrolyzed with NaOH after to be that formaldehyde crosslinking is modified specifically shred silk cocoon, be subsequently adding NaHCO3,
NaHCO3, and formalin in there-necked flask mix, under the conditions of 95 DEG C magnetic agitation reaction 5h after, remove condenser pipe,
Tailing adapter reaction 0.5h.
It is described it is modified be that Lauxite is modified, after specifically shred silk cocoon, add urea, NaHCO3 and formaldehyde water-soluble
Liquid mixes in there-necked flask, at 95 DEG C, after magnetic agitation reaction 5h, removes condenser pipe, and 0.5h is reacted in tailing adapter again.
Further, the invention discloses a kind of preparation method of the modified Carbon Materials of silk cocoon of Adsorption of Heavy Metal Ions：
Silk cocoon is carbonized in Muffle furnace, shown charing is from 20 DEG C of ramps with 2 DEG C/min to 100 DEG C, insulation
120min is raised to 200 DEG C from 100 DEG C of speed with 1 DEG C/min again, is incubated 120min, is subsequently adding NaHCO3 and formaldehyde is water-soluble
Liquid, is blended in a there-necked flask, and temperature is magnetic agitation reaction 5h at 95 DEG C, removes condenser pipe, and tailing adapter is reacted again
0.5h, obtains final product.
Silk cocoon is carbonized in Muffle furnace, shown charing is, from 20 DEG C of ramps with 2 DEG C/min to 100 DEG C, to protect
Warm 120min is raised to 200 DEG C from 100 DEG C of speed with 1 DEG C/min again, is incubated 120min, is subsequently adding urea and formaldehyde is water-soluble
Liquid, is blended in a there-necked flask, and temperature is magnetic agitation reaction 5h at 95 DEG C, removes condenser pipe, and tailing adapter is reacted again
0.5h, obtains final product.
The present invention pre-processes silk cocoon with different methods, and raw material of wood-charcoal is obtained after different temperatures charing with silk cocoon as raw material
Material, obtained Carbon Materials all remain with nitrogen-containing functional group, and have adsorption function to metal ion, wherein silk cocoon ginseng after hydrolysis
The Carbon Materials that the Carbon Materials obtained with reaction charing, the Carbon Materials ratio formaldehyde crosslinking obtained with Lauxite reaction are obtained retain
More nitrogen-containing functional groups, have bigger adsorbance to ion；The Carbon Materials carbonized at 200 DEG C than 300 DEG C at carbonize
Carbon Materials remain more nitrogen-containing functional groups, the Carbon Materials carbonized at 300 DEG C than 200 DEG C at the Carbon Materials that carbonize have it is more
Pore structure.
Compared with prior art, the present invention carries out low-temperature carbonization and Carbon Materials is obtained with silk cocoon as raw material after modified process,
Yield is high, and pollution is few, and the absorption property of product heavy metal ion is good.
Description of the drawings
Infrared spectrograms of the Fig. 1 for CJ200-4 and CJ200-4-UF；
Infrared spectrograms of the Fig. 2 for CJ300-0-UF and CJ300-4-UF；
Infrared spectrograms of the Fig. 3 for CJ200-4-UF and CJ300-4-UF；
Fig. 4 is silk cocoon, silk cocoon, 200 DEG C of charing silk cocoons and C200J infrared spectrograms after hydrolysis.Specific embodiment
The invention will be further described with reference to embodiments.
1 formaldehyde of embodiment is carbonized after being directly crosslinked
3g silk cocoons are weighed, is shredded, be put in there-necked flask, add the NaHCO of 3.6g3, 7mL mass concentration be 37% formaldehyde
The aqueous solution, the magnetic agitation reaction 5h under the conditions of temperature is for 95 DEG C remove condenser pipe, and 0.5h is reacted in tailing adapter again, will be above-mentioned
Cross-linking products are carbonized in Muffle furnace, from 20 DEG C of room temperatures with the ramp of 2 DEG C/min to 100 DEG C, are incubated 120min again from 100
DEG C 200 DEG C are raised to the speed of 1 DEG C/min, be incubated 120min at this temperature, the Carbon Materials for obtaining are labeled as into CJ200-0,
Yield 31%；Change temperature, obtain CJ300-0, yield 18.6%.
Carbonize after formaldehyde crosslinking after the degraded of embodiment 2
3g silk cocoons are weighed, addition polytetrafluoroethyllining lining water heating kettle is shredded, plus NaOH solution hydrolyzes 3h at 100 DEG C；Use hydrochloric acid
The pH value of silk cocoon after hydrolysis is adjusted to 8-10,3.6g NaHCO are added3, 7mL mass concentration be 37% formalin,
It is blended in a there-necked flask, the magnetic agitation reaction 5h under the conditions of temperature is for 95 DEG C removes condenser pipe, and tailing adapter is anti-again
0.5h is answered, above-mentioned cross-linking products are carbonized in Muffle furnace, from 20 DEG C of room temperatures with the ramp of 2 DEG C/min to 100 DEG C, be incubated
120min is raised to 200 DEG C from 100 DEG C of speed with 1 DEG C/min again, is incubated 120min at this temperature, by the Carbon Materials for obtaining
It is labeled as CJ200-4, yield 25.5%；Change temperature, obtain CJ300-4, yield 14.5%.
Carbonize after 3 ureaformaldehyde forerunner's precursor reactant of embodiment
3g silk cocoons are weighed, is shredded；Add 3g urea, 3.6g NaHCO3, 7mL mass concentration be 37% formalin, mix
Close in a there-necked flask, temperature is, at 95 DEG C, after magnetic agitation reaction 5h, to remove condenser pipe, and tailing adapter is reacted again
0.5h；Above-mentioned cross-linking products are carbonized in Muffle furnace, heating rate is controlled with temperature controller, from 20 DEG C of room temperatures with 2 DEG C/min's
Ramp to 100 DEG C, insulation 120min are raised to 200 DEG C from 100 DEG C of speed with 1 DEG C/min again, are incubated at this temperature
The Carbon Materials for obtaining are labeled as CJ200-0-UF, yield 79.3% by 120min；Change temperature, obtain CJ300-0-UF, yield
68.6%。
Carbonize after ureaformaldehyde forerunner's precursor reactant after the degraded of embodiment 4
3g silk cocoons are weighed, and are shredded addition polytetrafluoroethyllining lining water heating kettle, with 1%NaOH concentration, 3h are hydrolyzed at 100 DEG C；Use salt
Acid adjusts the pH value of silk cocoon after hydrolysis to 8-10, adds 3g urea, 3.6g NaHCO3, the formaldehyde that 7mL mass concentrations are 37%
The aqueous solution, is blended in a there-necked flask, and temperature is, at 95 DEG C, after magnetic agitation reaction 5h, to remove condenser pipe, tailing adapter
0.5h is reacted again；By above-mentioned cross-linking products Muffle furnace carbonize, with temperature controller control heating rate, from 20 DEG C of room temperatures with 2 DEG C/
The ramp of min to 100 DEG C, insulation 120min are raised to 200 DEG C from 100 DEG C of speed with 1 DEG C/min again, at this temperature
The Carbon Materials for obtaining are labeled as CJ200-4-UF, yield 73.9% by insulation 120min；Change temperature, obtain CJ300-4-UF,
Yield 65.1%.
It is crosslinked after 5 low-temperature carbonization of embodiment
About 3g silk cocoons are carbonized in Muffle furnace, heating rate is controlled with temperature controller, from 20 DEG C of room temperatures with the speed liter of 2 DEG C/min
To 100 DEG C, insulation 120min is raised to 200 DEG C from 100 DEG C of speed with 1 DEG C/min to temperature again, is incubated 120min at this temperature,
Obtain dark brown powder；3.6g NaHCO are added in dark brown powder3, the formalin that 7mL mass concentrations are 37%, mixing
In a there-necked flask, temperature is magnetic agitation reaction 5h at 95 DEG C, removes condenser pipe, and 0.5h is reacted in tailing adapter again, will
Product Labeling is C200J；
It is crosslinked after 6 low-temperature carbonization of embodiment
About 3g silk cocoons are carbonized in Muffle furnace, heating rate is controlled with temperature controller, from 20 DEG C of room temperatures with the speed liter of 2 DEG C/min
To 100 DEG C, insulation 120min is raised to 200 DEG C from 100 DEG C of speed with 1 DEG C/min to temperature again, is incubated 120min at this temperature,
Obtain dark brown powder；3g urea, 3.6g NaHCO in dark brown powder3, the formalin that 15mL mass concentrations are 37%,
It is blended in a there-necked flask, temperature is magnetic agitation reaction 5h [30] at 95 DEG C, removes condenser pipe, tailing adapter is anti-again
0.5h is answered, is C200J-UF by Product Labeling.
7 performance test of embodiment
The various Carbon Materials that embodiment 1-6 is obtained repeatedly are washed to neutrality with distilled water respectively, are dried, are smashed, and are store
In drier, test for structural characterization and adsorption experiment, including infrared, BET.
Adsorption experiment
Absorption of the Carbon Materials to each ion
Weigh quality be the CJ200-0 of 0.05g, CJ200-4, CJ200-0-UF, CJ200-4-UF, CJ300-0, CJ300-4,
CJ300-0-UF, CJ300-4-UF, C200J and C200J-UF, are added separately in the conical flask with cover of 100mL, bore to ten
Move into the metal ion storing solution of 100 g/mL of the pH4 of 25mL in shape bottle respectively with pipette, be 25 DEG C in design temperature
In water-bath constant temperature oscillator, after vibration absorption 12h, then 12h is stood, take supernatant；By supernatant and certain times of original solution dilution
Absorbance is revert to metal ion calibration curve, learns its concentration by number, mensuration absorbance；
Carbon Materials are calculated to the adsorbance formula (1) of metal ion：
(1)
Wherein：Qe represents the equilibrium adsorption capacity (mg/g) on Carbon Materials, and C0 is the initial concentration (mg/L) of metal ion in solution,
The concentration (mg/L) of metal ion in solution when Ce is adsorption equilibrium, volumes (L) of the V for adsorbent solution, consumptions of the m for adsorbent
(g)。
NaOH solution of the use quality fraction for 0-10%, hydrolyzes 0-12 hours, and results of hydrolysis shows and uses 1% NaOH molten
Liquid, hydrolyzes 3 hours, and hydrolysis effect is optimal.
Silk cocoon and formaldehyde and the infrared figure of Lauxite product, the infrared figure of wherein CJ200-4 and CJ200-4-UF is such as
Shown in Fig. 1, it will be seen from figure 1 that the infrared spectrum of CJ200-4 and CJ200-4-UF, 1500-1700cm-1Place, CJ200-4 and
CJ200-4-UF has bimodal, belongs to the stretching vibration of amide groups, illustrates all to remain nitrogen-containing functional group；In 3600-
300cm-1There is obvious biabsorption peak at place, belongs to N-H stretching vibration peaks, illustrates that CJ200-4 and CJ200-4-UF are remained
More nitrogen-containing functional groups, show that silk cocoon adds formaldehyde crosslinking and adds Lauxite presoma protect well to after hydrolysis
Nitrogen-containing functional group in silk cocoon, the two contrast is it is found that silk cocoon forms urea with addition urea directly with formaldehyde crosslinking after degraded
Urea formaldehyde degraded silk cocoon cross-linking products prepare Carbon Materials, and functional group is similar to.Fig. 2 is red for CJ300-0-UF's and CJ300-4-UF
External spectrum figure, two kinds of Carbon Materials are in 1500-1700cm as can be seen from Figure 2-1Place, CJ300-0-UF and CJ300-4-UF have double
Peak, belongs to the stretching vibration of amide groups, illustrates all to remain nitrogen-containing group；In 3600-3300cm-1There is significantly absorption at place
Peak, belongs to N-H stretching vibration peaks.Infrared figures of the Fig. 3 for CJ200-4-UF and CJ300-4-UF, from figure 3, it can be seen that
1500-1700cm-1Place, CJ200-4-UF and CJ300-4-UF have bimodal, belong to the stretching vibration of amide groups, illustrate all to protect
Nitrogen-containing group is stayed；In 3600-300cm-1There is obvious absworption peak at place, belongs to N-H stretching vibration peaks, but CJ200-4-UF
It is bimodal to become apparent from, illustrate that CJ200-4-UF and CJ300-4-UF remain more nitrogen-containing functional groups.Fig. 4 be silk cocoon, hydrolysis after silkworm
Cocoon, 200 DEG C of charing silk cocoons and the infrared figures of C200J, from fig. 4, it can be seen that C200J is in 3500-3000cm-1Place and 1500-
1700cm-1Place has significantly bimodal；In 3500-3000cm-1Place, the strong absworption peak of C200J belong to N-H stretching vibration peaks；
1500-1700cm-1Place, the bimodal stretching vibration for belonging to amide groups of C200J, show Jing charing and crosslinking Treatment after, its
All the time nitrogen-containing functional group is remained, is conducive to the absorption to ion.
Carbon Materials absorption property comparing result is as shown in table 1,
1 absorption property of table is contrasted
As can be seen from Table 1：Carbon Materials heavy metal ion is prepared using this method preferably absorption, to conventional aluminium, iron ion
Absorption is less, and this is that have abundant nitrogen-containing functional group due to the Carbon Materials for preparing, and has preferable coordination ability with heavy metal ion, but
Increase with temperature, nitrogen-containing functional group easily decomposes, while abundant pore structure can be formed, increase surface area, carbonize from 200,300 degree
Material absorption is as can be seen that increase with temperature, adsorbance typically increases.The Carbon Materials prepared with undegraded silk cocoon and degraded silk cocoon
CJ200-0, CJ300-0, CJ200-4, CJ300-4 absorption is as can be seen that easily decompose in material carbonization process after degraded, nitrogenous official
Loss can be rolled into a ball larger, but easily form hole, increase surface area.Substantially carried using Carbon Materials absorption property prepared by urea-modified material
Height, this is, due to forming higher degree of crosslinking product, while increased nitrogen-containing functional group, to recycle the easily decomposes formation of degraded silk cocoon
Preferably duct, has increased considerably surface area, has enable have preferable enriching heavy metal ion in 200 degree of CJ200-4-UF for obtaining
Power, it is not necessary to which very high temperature can obtain preferable enriching heavy metal Carbon Materials.
BET is characterized
CJ300-0, CJ300-0-UF, CJ200-4-UF, C200J material is selected to carry out BET signs, as a result as shown in table 2,
2 specific surface area of table and pore volume pore-size distribution
| Carbon Materials | Specific surface area (m2/g) | Average pore size (nm) | Micropore total pore volume (cm3/g) | Most probable pore size (nm) |
| CJ300-0 | 10.78 | 8.65 | 0.116 | 1.62 |
| CJ300-0-UF | 106.51 | 6.33 | 1.310 | 2.01 |
| CJ200-4-UF | 196.14 | 2.11 | 2.33 | 1.21 |
| C200J | 2.60 | 9.89 | 0.00095 | 1.06 |
As can be seen from Table 2 using silk cocoon, urea by formaldehyde crosslinking can at a lower temperature 200 degree to obtain surface area larger
Carbon Materials, most probable pore size typically in 1-2 rans, with metal ion sizableness, are conducive to heavy metal ionic adsorption.
It is crosslinked after first carbonizing silk cocoon, regardless of whether Carbon Materials adsorption capacity obtained by addition urea is general, this is because when silk cocoon is carbonized,
Surface nitrogen-containing functional group loss is larger, does not form preferable duct, and this can also characterize from BET and be verified.
Claims (6)
1. the preparation method of the modified Carbon Materials of a kind of silk cocoon of Adsorption of Heavy Metal Ions, it is characterised in that with silk cocoon as raw material, change
Property after carbonize in Muffle furnace, shown charing is that from 20 DEG C of ramps with 2 DEG C/min to 100 DEG C, insulation 120min is again
200 DEG C are raised to from 100 DEG C of speed with 1 DEG C/min, the modified Carbon Materials of silk cocoon after insulation 120min, are obtained final product.
2. the preparation method of the modified Carbon Materials of the silk cocoon of Adsorption of Heavy Metal Ions according to claim 1, it is characterised in that
It is described it is modified be that formaldehyde crosslinking is modified, specifically silk cocoon is shredded, with NaHCO3, and formalin in there-necked flask
Mixing, under the conditions of 95 DEG C after magnetic agitation reaction 5h, removes condenser pipe, tailing adapter reaction 0.5h, wherein described formalin
The mass concentration of solution is 37%, described silk cocoon：NaHCO3Mass ratio be 3:3.6, described silk cocoon and formalin
Mass volume ratio is 3:7.
3. the preparation method of the modified Carbon Materials of the silk cocoon of Adsorption of Heavy Metal Ions according to claim 1, it is characterised in that
It is described it is modified hydrolyzed with NaOH after to be that formaldehyde crosslinking is modified specifically shred silk cocoon, be subsequently adding NaHCO3, NaHCO3, and
Mix in there-necked flask in formalin, under the conditions of 95 DEG C after magnetic agitation reaction 5h, remove condenser pipe, tailing adapter is anti-
Answer 0.5h.
4. the preparation method of the modified Carbon Materials of the silk cocoon of Adsorption of Heavy Metal Ions according to claim 1, it is characterised in that
It is described it is modified be that Lauxite is modified, after specifically shred silk cocoon, add urea, NaHCO3 and formalin at three mouthfuls
Mix in flask, at 95 DEG C, after magnetic agitation reaction 5h, remove condenser pipe, 0.5h is reacted in tailing adapter again.
5. the preparation method of the modified Carbon Materials of a kind of silk cocoon of Adsorption of Heavy Metal Ions, it is characterised in that step is：Silk cocoon is existed
Muffle furnace is carbonized, and shown charing is that, from 20 DEG C of ramps with 2 DEG C/min to 100 DEG C, 120min is again from 100 DEG C for insulation
200 DEG C are raised to the speed of 1 DEG C/min, 120min are incubated, are subsequently adding NaHCO3 and formalin, are blended in one three
In mouth flask, temperature is magnetic agitation reaction 5h at 95 DEG C, removes condenser pipe, and tailing adapter is reacted 0.5h again, obtained final product.
6. the preparation method of the modified Carbon Materials of a kind of silk cocoon of Adsorption of Heavy Metal Ions, it is characterised in that step is：Silk cocoon is existed
Muffle furnace is carbonized, and shown charing is that, from 20 DEG C of ramps with 2 DEG C/min to 100 DEG C, 120min is again from 100 DEG C for insulation
200 DEG C are raised to the speed of 1 DEG C/min, 120min are incubated, are subsequently adding urea and formalin, are blended in one three mouthfuls
In flask, temperature is magnetic agitation reaction 5h at 95 DEG C, removes condenser pipe, and tailing adapter is reacted 0.5h again, obtained final product.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107362770A (en) * | 2017-07-21 | 2017-11-21 | 浙江省农业科学院 | A kind of silk cocoon biological carbon materials for adsorbing heavy metal cadmium |
| CN114390920A (en) * | 2019-04-16 | 2022-04-22 | 自然进化公司 | Chemically linked silk fibroin coatings and methods of making and using the same |
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| CN107362770A (en) * | 2017-07-21 | 2017-11-21 | 浙江省农业科学院 | A kind of silk cocoon biological carbon materials for adsorbing heavy metal cadmium |
| CN114390920A (en) * | 2019-04-16 | 2022-04-22 | 自然进化公司 | Chemically linked silk fibroin coatings and methods of making and using the same |
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| CN106540666B (en) | 2019-04-02 |
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