CN108722355A - A kind of preparation method for using modified cotton stalk matrix activated carbon except formaldehyde - Google Patents
A kind of preparation method for using modified cotton stalk matrix activated carbon except formaldehyde Download PDFInfo
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- CN108722355A CN108722355A CN201810547421.4A CN201810547421A CN108722355A CN 108722355 A CN108722355 A CN 108722355A CN 201810547421 A CN201810547421 A CN 201810547421A CN 108722355 A CN108722355 A CN 108722355A
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- activated carbon
- cotton stalk
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- formaldehyde
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/704—Solvents not covered by groups B01D2257/702 - B01D2257/7027
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/708—Volatile organic compounds V.O.C.'s
Abstract
The invention discloses a kind of except the formaldehyde preparation method of modified cotton stalk matrix activated carbon, includes the following steps：It is put in outdoor after cotton stalk is washed with water to dry, is broken into powder, then cotton stalk powder is placed in bellows dry；Cotton stalk powder is impregnated in a period of time in liquor zinci chloridi, is put into roasting in Muffle furnace after isolating solid, washing to neutrality is dry, obtains cotton stalk matrix activated carbon；Cotton stalk matrix activated carbon is immersed in copper nitrate solution, dispersion is ultrasonically treated, sodium hydroxide solution is then added and adjusts pH to neutrality, stands, isolates solid, then toast under vacuum, obtain modified activated carbon a；It is scattered in hydrochloric acid solution after modified activated carbon a is mixed with aniline, stirs, ammonium chloride solution is then added, reacted, isolate solid, dry, heating roasting is cooling, obtains except the modified cotton stalk matrix activated carbon of formaldehyde.
Description
Technical field
The present invention relates to formaldehyde to understand technical field more particularly to a kind of preparation being modified cotton stalk matrix activated carbon except formaldehyde
Method.
Background technology
Formaldehyde is the high carcinogenic that World Health Organization is assert and the high abnormalities chemicals of cause, is breakneck allergic reaction
Original, while being not easy to be discovered by people.Lot of documents is recorded, and formaldehyde, which is presented as the harm major part table of human body, causes people to exhale
It inhales unsmooth, nauseous, can also induce respiratory disease, such as bronchitis, chemical pneumonia, lung cancer.When concentration of formaldehyde is in air
Interior arrival 0.06-0.07mg/m3When, child will cause asthma；When concentration of formaldehyde reaches 0.1mg/m in air3When, human body
Discovering has peculiar smell and with slight uncomfortable；Reach 0.5mg/m3When, human body sensory eye is stimulated, phenomenon of shedding tears occurs；First
Aldehyde concentration is close to 0.6mg/m3, that is, cause throat pain, acutely cough；Concentration further increases, and can cause hyperemesis, uncomfortable in chest
Nausea, with serious asthma and pulmonary edema；Increase to 30mg/m3When, it can make one dead at once.Activated carbon is as a kind of absorption
The porous material of function admirable has good removal ability to multiple pollutant, is widely used in the adsorption treatment of formaldehyde.
In addition, being shown according to the statistical data of China's report hall website, China has big as developing large agricultural country
The agricultural straw resource of amount fails rationally to be utilized.Wherein cotton is as important agricultural product and the raw material of industry, per annual meeting
A large amount of cotton stalk is generated, but the cotton stalk of pulverized returning to the field or on-site incineration occupies prodigious proportion, this is both to cotton stalk
The waste of resource can bring the problems such as pollution environment again.And cotton stalk contains abundant carbon, can be used for producing activated carbon, therefore
How using discarded cotton stalk resource the activated carbon being had excellent performance except formaldehyde is produced, for environmental protection, improves the profit of resource
Have great importance with rate.
Invention content
Based on background technology there are the problem of, the present invention proposes a kind of preparation except formaldehyde modification cotton stalk matrix activated carbon
Method, but the purifying formaldehyde rate of the modification cotton stalk matrix activated carbon of this method preparation is more than 80%, after absorption for 24 hours after adsorbing 12h
More than 99%.
The present invention proposes a kind of preparation method except the modified cotton stalk matrix activated carbon of formaldehyde, includes the following steps：
S1, it is put in outdoor after washing with water cotton stalk and dries, be broken into powder, then cotton stalk powder is placed in bellows
Dry 8-20h at 105 DEG C；
S2, cotton stalk powder is impregnated in the liquor zinci chloridi of a concentration of 57-64wt%, after 1-3h, is consolidated what is isolated
Body is put into Muffle furnace heats 0.5-1h under the conditions of temperature is 580-630 DEG C, and washing to neutrality is dry, obtains the work of cotton stalk base
Property charcoal；
S3, cotton stalk matrix activated carbon is immersed in copper nitrate solution, is ultrasonically treated 20-40min, is then added a concentration of
The sodium hydroxide solution of 10-30wt% adjusts pH to neutrality, stands 20-40min, isolates solid, is then 380- in temperature
Vacuum bakeout 35-55min under the conditions of 410 DEG C, obtains modified activated carbon a；
S4, it is scattered in hydrochloric acid solution after mixing modified activated carbon a with aniline, stirs 90-110min, be then added dense
Degree is the ammonium chloride solution of 10-25wt%, reacts 5-8h, isolates solid, dry, and 30-50min is kept the temperature at 510-530 DEG C,
It is cooled to room temperature, obtains except the modified cotton stalk matrix activated carbon of formaldehyde.
Preferably, in S1, the grain size of cotton stalk powder is less than 1mm after being crushed.
Preferably, in S2, the impregnating ratio of cotton stalk powder and liquor zinci chloridi is 1-6:1-2.
Preferably, in S2, drying temperature is less than 100 DEG C.
Preferably, in S3, a concentration of 10-15wt% of copper nitrate solution.
Preferably, in S4, the mass ratio of the modified activated carbon a and aniline is 15-25:2-3.
Preferably, in S4, the mass ratio of modified activated carbon a and ammonium chloride solution is 35-55:6-9.
Preferably, in S4, drying temperature is the drying time 8-20h less than 100 DEG C.
The present invention prepares activated carbon using cotton stalk extra in Cotton Production as carbon source, can be crushed to avoid cotton stalk returning to the field or
The problems such as person's on-site incineration results in waste of resources and pollutes environment improves resource utilization and economic benefit；In addition, being removed in preparation
During the modified cotton stalk matrix activated carbon of formaldehyde, the present invention first cleans up cotton stalk, dry after be broken for grain size and be less than 1mm
Powder, then cotton stalk powder is impregnated in liquor zinci chloridi, zinc chloride is in lower temperature to the fiber in cotton stalk powder
Element plays certain swelling effect, makes occur original hole in cotton stalk powder, is dehydrated later when Muffle furnace high temperature carbonizes, and
Rationally control zinc oxide concentration, impregnating ratio, carbonization temperature, carbonization time make the cotton stalk matrix activated carbon of generation be formed a large amount of micro-
Hole is conducive to formaldehyde adsorption；Secondly, the present invention is modified cotton stalk matrix activated carbon, is loaded to copper ion using infusion process
In activated carbon, on the one hand, copper ion is attached to activated carbon surface so that surface is more coarse, and specific surface area increases, and enhances to first
On the other hand the suction-operated of aldehyde since copper ion charge radius is larger, is easy living with carbonyl, the carboxyl of activated carbon surface etc.
Property functional group interaction, cause activated carbon structure defect hole increase, for formaldehyde entrance provide more channels thus
Increase the physical absorption amount of formaldehyde；The last present invention also adopts home position polymerization reaction and high temperature carbonization using aniline, successfully by nitrogen
Activated carbon surface is mixed, because nitrogen-atoms has excess electron pair, it is possible to increase hole ambient electron cloud density and electronegativity, and formaldehyde contains
Carbonyl be unsaturated group, its carbon atom is height electron deficient, is easy to be polarized and generates carbonyl carbonium ion, institute
With the present invention enhances the attraction of carbonyl carbonium ion in PARA FORMALDEHYDE PRILLS(91,95) using activated carbon surface doping nitrogen-atoms, to improve this
The adsorbance and adsorption rate of invention PARA FORMALDEHYDE PRILLS(91,95) gas.After testing, the formaldehyde for the modification cotton stalk matrix activated carbon that prepared by the present invention is net
Rate is more than 80% after adsorbing 12h, and absorption is more than 99% afterwards for 24 hours.
Specific implementation mode
Technical solution of the present invention is described in detail with reference to specific embodiment.
Embodiment 1
A kind of preparation method for using modified cotton stalk matrix activated carbon except formaldehyde, includes the following steps：
S1, it is put in outdoor after washing with water cotton stalk and dries, be broken into powder, then cotton stalk powder is placed in bellows
Dry 8h at 105 DEG C；
S2, cotton stalk powder is impregnated in the liquor zinci chloridi of a concentration of 64wt%, after 1h, the solid isolated is put into
0.5h is heated in Muffle furnace under the conditions of temperature is 630 DEG C, washing to neutrality is dry, obtains cotton stalk matrix activated carbon；
S3, cotton stalk matrix activated carbon is immersed in copper nitrate solution, is ultrasonically treated 20min, is then added a concentration of
The sodium hydroxide solution of 30wt% adjusts pH to neutrality, stands 20min, isolates solid, then under the conditions of temperature is 410 DEG C
Vacuum bakeout 35min obtains modified activated carbon a；
S4, it is scattered in hydrochloric acid solution after mixing modified activated carbon a with aniline, stirs 110min, concentration is then added
For the ammonium chloride solution of 10wt%, 8h is reacted, solid is isolated, it is dry, 50min is kept the temperature at 510 DEG C, is cooled to room temperature, is obtained
To except the modified cotton stalk matrix activated carbon of formaldehyde.
Embodiment 2
A kind of preparation method for using modified cotton stalk matrix activated carbon except formaldehyde, includes the following steps：
S1, it is put in outdoor after washing with water cotton stalk and dries, the powder that grain size is less than 1mm is broken into, then by cotton stalk powder
End is placed in bellows at 105 DEG C dry 8h；
S2, cotton stalk powder is impregnated in the liquor zinci chloridi of a concentration of 57wt%, after 3h, the solid isolated is put into
1h is heated in Muffle furnace under the conditions of temperature is 580 DEG C, washing to neutrality is dry under the conditions of temperature is less than 100 DEG C, obtains cotton
Bar matrix activated carbon；The impregnating ratio of cotton stalk powder and liquor zinci chloridi is 1:2；
S3, cotton stalk matrix activated carbon is immersed in the copper nitrate solution of a concentration of 10wt%, is ultrasonically treated 40min, then
The sodium hydroxide solution that a concentration of 10wt% is added adjusts pH to neutrality, stands 40min, isolates solid, be then in temperature
Vacuum bakeout 55min under the conditions of 380 DEG C, obtains modified activated carbon a；
S4, it is scattered in hydrochloric acid solution after mixing modified activated carbon a with aniline, stirs 90min, be then added a concentration of
The ammonium chloride solution of 25wt% reacts 5h, isolates solid, and dry 20h, keeps the temperature at 510 DEG C under the conditions of less than 100 DEG C
50min is cooled to room temperature, and is obtained except the modified cotton stalk matrix activated carbon of formaldehyde；The mass ratio of the modified activated carbon a and aniline is
15:3；The mass ratio of modified activated carbon a and ammonium chloride solution is 35:9.
Embodiment 3
A kind of preparation method for using modified cotton stalk matrix activated carbon except formaldehyde, includes the following steps：
S1, it is put in outdoor after washing with water cotton stalk and dries, the powder that grain size is less than 1mm is broken into, then by cotton stalk powder
End is placed in bellows at 105 DEG C dry 20h；
S2, cotton stalk powder is impregnated in the liquor zinci chloridi of a concentration of 64wt%, after 1h, the solid isolated is put into
0.5h is heated in Muffle furnace under the conditions of temperature is 630 DEG C, washing to neutrality is dry under the conditions of temperature is less than 100 DEG C, obtains
Cotton stalk matrix activated carbon；The impregnating ratio of cotton stalk powder and liquor zinci chloridi is 6:1；
S3, cotton stalk matrix activated carbon is immersed in the copper nitrate solution of a concentration of 15wt%, is ultrasonically treated 20min, then
The sodium hydroxide solution that a concentration of 30wt% is added adjusts pH to neutrality, stands 20min, isolates solid, be then in temperature
Vacuum bakeout 35min under the conditions of 410 DEG C, obtains modified activated carbon a；
S4, it is scattered in hydrochloric acid solution after mixing modified activated carbon a with aniline, stirs 110min, concentration is then added
For the ammonium chloride solution of 10wt%, 8h is reacted, solid is isolated, dry 8h, keeps the temperature at 530 DEG C under the conditions of less than 100 DEG C
30min is cooled to room temperature, and is obtained except the modified cotton stalk matrix activated carbon of formaldehyde；The mass ratio of the modified activated carbon a and aniline is
25:2；The mass ratio of modified activated carbon a and ammonium chloride solution is 55:6.
Embodiment 4
A kind of preparation method for using modified cotton stalk matrix activated carbon except formaldehyde, includes the following steps：
S1, it is put in outdoor after washing with water cotton stalk and dries, the powder that grain size is less than 1mm is broken into, then by cotton stalk powder
End is placed in bellows at 105 DEG C dry 13h；
S2, cotton stalk powder is impregnated in the liquor zinci chloridi of a concentration of 61wt%, after 2h, the solid isolated is put into
0.8h is heated in Muffle furnace under the conditions of temperature is 590 DEG C, washing to neutrality is dry under the conditions of temperature is less than 100 DEG C, obtains
Cotton stalk matrix activated carbon；The impregnating ratio of cotton stalk powder and liquor zinci chloridi is 3:1；
S3, cotton stalk matrix activated carbon is immersed in the copper nitrate solution of a concentration of 12wt%, is ultrasonically treated 28min, then
The sodium hydroxide solution that a concentration of 17wt% is added adjusts pH to neutrality, stands 32min, isolates solid, be then in temperature
Vacuum bakeout 47min under the conditions of 396 DEG C, obtains modified activated carbon a；
S4, it is scattered in hydrochloric acid solution after mixing modified activated carbon a with aniline, stirs 96min, be then added a concentration of
The ammonium chloride solution of 18wt% reacts 6h, isolates solid, and dry 15h, keeps the temperature at 520 DEG C under the conditions of less than 100 DEG C
40min is cooled to room temperature, and is obtained except the modified cotton stalk matrix activated carbon of formaldehyde；The mass ratio of the modified activated carbon a and aniline is
20:3；The mass ratio of modified activated carbon a and ammonium chloride solution is 45:7.
Performance detection
Modification cotton stalk matrix activated carbon prepared by embodiment 1-4 is in the straight type polytetrafluoroethylene (PTFE) tube reaction of Φ 18mm, long 180mm
Formaldehyde adsorption property test is carried out in device, the filling size of the modified cotton stalk matrix activated carbon is Φ 18mm*40mm (modified cotton stalks
Matrix activated carbon filling diameter is identical as straight type polytetrafluoroethylene (PTFE) pipe reactor, ensures that the gas passed through is lived by modified cotton stalk base
Property charcoal processing), unstripped gas group becomes：Concentration of formaldehyde 5ppm, remaining is air.Reaction carries out under 25 DEG C of atmospheric pressure environments, reacts
Air volume air speed (GHSV) is 6000h-1, detects that concentration of formaldehyde calculates by the portable formaldehyde gas detectors of domestic GD80
To purifying formaldehyde rate, the experimental results showed that, the purifying formaldehyde rate of modification cotton stalk matrix activated carbon prepared by embodiment 1-4 is being adsorbed
80% is all higher than after 12h, absorption is all higher than 99% afterwards for 24 hours.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (8)
1. a kind of except the formaldehyde preparation method of modified cotton stalk matrix activated carbon, which is characterized in that include the following steps：
S1, it is put in outdoor after washing with water cotton stalk and dries, be broken into powder, then cotton stalk powder is placed on 105 in bellows
Dry 8-20h at DEG C；
S2, cotton stalk powder is impregnated in the liquor zinci chloridi of a concentration of 57-64wt%, after 1-3h, the solid isolated is put
Enter and heat 0.5-1h in Muffle furnace under the conditions of temperature is 580-630 DEG C, washing to neutrality is dry, obtains cotton stalk matrix activated carbon；
S3, cotton stalk matrix activated carbon is immersed in copper nitrate solution, is ultrasonically treated 20-40min, a concentration of 10- is then added
The sodium hydroxide solution of 30wt% adjusts pH to neutrality, stands 20-40min, isolates solid, is then 380-410 in temperature
Vacuum bakeout 35-55min under the conditions of DEG C obtains modified activated carbon a；
S4, it is scattered in hydrochloric acid solution after mixing modified activated carbon a with aniline, stirs 90-110min, be then added a concentration of
The ammonium chloride solution of 10-25wt% reacts 5-8h, isolates solid, dry, and 30-50min is kept the temperature at 510-530 DEG C, cooling
To room temperature, obtain except the modified cotton stalk matrix activated carbon of formaldehyde.
2. preparation method according to claim 1, which is characterized in that in S1, the grain size of broken rear cotton stalk powder is less than
1mm。
3. preparation method according to claim 1 or 2, which is characterized in that in S2, the leaching of cotton stalk powder and liquor zinci chloridi
Stain ratio is 1-6:1-2.
4. according to claim 1-3 any one of them preparation methods, which is characterized in that in S2, drying temperature is less than 100 DEG C.
5. according to claim 1-4 any one of them preparation methods, which is characterized in that in S3, copper nitrate solution it is a concentration of
10-15wt%.
6. according to claim 1-5 any one of them preparation methods, which is characterized in that in S4, the modified activated carbon a and benzene
The mass ratio of amine is 15-25:2-3.
7. according to claim 1-6 any one of them preparation methods, which is characterized in that in S4, modified activated carbon a and ammonium chloride
The mass ratio of solution is 35-55:6-9.
8. according to claim 1-7 any one of them preparation methods, which is characterized in that in S4, drying temperature is less than 100
DEG C, drying time 8-20h.
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| CN113952975A (en) * | 2021-10-19 | 2022-01-21 | 中国科学院江西稀土研究院 | B, N co-doped carbon fiber-based catalytic material and preparation method thereof |
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| CN113952975A (en) * | 2021-10-19 | 2022-01-21 | 中国科学院江西稀土研究院 | B, N co-doped carbon fiber-based catalytic material and preparation method thereof |
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Application publication date: 20181102 |