CN103861561A - Carbide derived carbon adsorbent for removing low-concentration low-molecular-weight VOCs (volatile organic compounds) as well as preparation method of adsorbent - Google Patents
Carbide derived carbon adsorbent for removing low-concentration low-molecular-weight VOCs (volatile organic compounds) as well as preparation method of adsorbent Download PDFInfo
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Abstract
The invention discloses a carbide derived carbon adsorbent for removing low-concentration low-molecular-weight VOCs (volatile organic compounds) as well as a preparation method of the adsorbent, and belongs to the technical field of gas purification treatment technique. The preparation method comprises the following steps: firstly, heating commercial carbide in an inert atmosphere to 600-900 DEG C, and then introducing chlorine for 2-4 hours and etching at high temperature at the flow rate of 30-50ml/min; then introducing inert atmosphere again and cooling down to room temperature so as to obtain the primary carbide derived carbon product; then adding the carbide derived carbon primary product to an oxidizing solution and performing immersion treatment for 6-12 hours; and then washing by deionized water to be neutral, and drying at 105 DEG C for 3-8 hours, thereby obtaining the finished carbide derived carbon adsorbent product. Compared with existing commercial activated carbon, the adsorbent designed by the invention can efficiently adsorb low-concentration low-molecular-weight VOCs at high air speed, is high in adsorption capacity, has long service life, and is suitable for air purification treatment in rooms of buildings, airtight cabins and other limited spaces.
Description
Technical field
The present invention relates to a kind of adsorbent and preparation method thereof, particularly low concentration low-molecular-weight volatile organic matter adsorption cleaning adsorbent and preparation method thereof under a kind of room temperature, belongs to gas purification processing technology field.
Background technology
In recent years, the seriousness of room air pollution causes people's attention day by day.On the one hand, follow the raising of the airtight degree of building, indoor-outdoor air mass discrepancy is increasing.On the other hand, along with scientific and technological fast development, the position of the technical equipments such as aircraft cockpit, manned spacecraft, submarine, car and boat, underground fortification, extraordinary chemical workshop, extraordinary laboratory in human civilization life is more and more important.And the personnel that are in Indoor environment and closed in space and ambient atmosphere environment are completely or relative isolated, therefore its air quality and people's healthy and life, work quality, even life security is closely bound up.
In Indoor environment and closed in space, the multiple low concentration volatile organic matter (VOCs) that derives from material outgassing, instrument and equipment release and human body metabolism generation has a strong impact on air quality, and therefore controlling these VOCs becomes the important composition part of improving environmental quality.Absorption is to solve Indoor environment and the VOCs of closed in space to pollute effective method, conventional activated carbon of sorbent is because its pore structure is flourishing and surface oxygen functional group the advantage such as can regulate and control and can effectively adsorb the macromolecule VOCs such as benzene homologues, but high volatile volatile low-molecular-weight VOCs is very weak in the adsorption capacity of activated carbon surface.This is mainly that existing macropore, also contains mesopore and micropore because traditional active carbon pore-size distribution is wider, but low-molecular-weight VOCs only produces absorption on micropore, and the effect that provides VOCs to enter the path of adsorption site is only provided for macropore and mesopore.In addition, activated carbon surface oxygen-containing functional group also has important impact, the increase of oxygen-containing functional group that polarity is increased on absorption, can increase the absorption to polar molecule.Therefore need to adjust acticarbon pore structure and surface chemical property to improve its absorption property to low-molecular-weight VOCs.
Summary of the invention
Process the poor deficiency of low concentration low-molecular-weight organic matter adsorption capacity in Indoor environment and closed in space for traditional active carbon purifying, the invention provides one and both can efficient adsorption separate macromolecule volatile organic matter, adsorbent that again can efficient adsorption separating low concentration low-molecular-weight volatile organic matter and preparation method thereof.This adsorbent, taking commercial carbide as presoma, is prepared from through chlorine high temperature etching, impregnating step.This adsorbent specific area is at 1400m
2more than/g, pore volume is 0.4～0.8cm
3/ g, Micropore volume is 0.3～0.6cm
3/ g, aperture is mainly distributed in 0.7～2nm, and a large amount of oxygen-containing functional groups are contained on surface.This adsorbent has excellent absorption property to the typical low-molecular-weight VOCs existing in Indoor environment and closed in space, is 5～15 times of commercially available conventional active carbon to the dynamic adsorption capacity of the low-molecular-weight VOCs such as low concentration methanol, acetaldehyde and acetone.
The preparation method of adsorbent provided by the invention mainly comprises the following steps:
(1) first commercial carbide is warming up to 600～900 DEG C in inert atmosphere, then changes logical chlorine and within 2～4 hours, carry out high temperature etching, flow is 30-50ml/min.Then, logical inert atmosphere is cooled to room temperature again, obtains carbide-derived carbon primary product.Preferably, high temperature etching temperature is 700～800 DEG C.
(2) step (1) gained carbide-derived carbon primary product are joined in oxidizing solution and carry out impregnation process 6～12 hours.Then, to neutral, at 105 DEG C of temperature, be dried 3～8 hours with deionized water washing, obtain carbide-derived carbon adsorbent final products.
Commercial carbide described in above-mentioned steps (1) is any one in TiC, VC and NbC.
Certain density oxidizing solution described in above-mentioned steps (2) is the HNO of molar concentration 1～9mol/L
3, or the H of mass percent concentration 5～30%
2o
2.
The invention has the advantages that: compared with existing commercial active carbon, the adsorbent of the present invention's design is energy efficient adsorption low concentration low-molecular-weight VOCs under high-speed, adsorption capacity is large, and long service life is applicable to Indoor environment, closed in space and other confined space inner air-cleaning processing.
Brief description of the drawings
Fig. 1 is the graph of pore diameter distribution of carbide-derived carbon adsorbent of the present invention.
Fig. 2 (A) and Fig. 2 (B) are respectively the CO in the temperature programmed desorption process of carbide-derived carbon adsorbent of the present invention
2with CO effusion curve.
Detailed description of the invention
Carbide-derived carbon adsorbent below in conjunction with embodiment to removal low concentration low-molecular-weight VOCs of the present invention and preparation method thereof is elaborated.
4gTiC is warming up in inert atmosphere to 700 DEG C, then changes logical chlorine (30ml/min) and within 2 hours, carry out high temperature etching.Then, logical inert gas is cooled to room temperature again, obtains primary product.1g gained primary product are added to the oxidizing solution HNO that the molar concentration of 10ml is 5mol/L
3middle room temperature impregnation process 12 hours.Then, to neutral, at 105 DEG C of temperature, be dried 8 hours with deionized water washing, can obtain embodiment 1 adsorbent.
embodiment 2
4gVC is warming up in inert atmosphere to 600 DEG C, then changes logical chlorine (40ml/min) and within 4 hours, carry out high temperature etching.Then, logical inert gas is cooled to room temperature again, obtains primary product.1g gained primary product are added to the oxidizing solution H that the mass percent concentration of 10ml is 5%
2o
2middle room temperature impregnation process 6 hours.Then, to neutral, at 105 DEG C of temperature, be dried 5 hours with deionized water washing, can obtain embodiment 2 adsorbents.
4gTiC is warming up in inert atmosphere to 800 DEG C, then changes logical chlorine (30ml/min) and within 2 hours, carry out high temperature etching.Then, logical inert gas is cooled to room temperature again, obtains primary product.1g gained primary product are added to the oxidizing solution HNO that the molar concentration of 10ml is 9mol/L
3middle room temperature impregnation process 12 hours.Then, to neutral, at 105 DEG C of temperature, be dried 8 hours with deionized water washing, can obtain embodiment 3 adsorbents.
embodiment 4
4gNbC is warming up in inert atmosphere to 700 DEG C, then changes logical chlorine (50ml/min) and within 3 hours, carry out high temperature etching.Then, logical inert gas is cooled to room temperature again, obtains primary product.1g gained primary product are added to the oxidizing solution H that the mass percent concentration of 10ml is 30%
2o
2middle room temperature impregnation process 12 hours.Then, to neutral, at 105 DEG C of temperature, be dried 8 hours with deionized water washing, can obtain embodiment 4 adsorbents.
embodiment 5
4gTiC is warming up in inert atmosphere to 900 DEG C, then changes logical chlorine (40ml/min) and within 2 hours, carry out high temperature etching.Then, logical inert gas is cooled to room temperature again, obtains primary product.1g gained primary product are added to the oxidizing solution HNO that the molar concentration of 10ml is 1mol/L
3middle room temperature impregnation process 6 hours.Then, to neutral, at 105 DEG C of temperature, be dried 3 hours with deionized water washing, can obtain embodiment 5 adsorbents.
comparative example 1
Commercially available 1g coal mass active carbon is added to the oxidizing solution HNO that the molar concentration of 10ml is 5mol/L
3middle room temperature impregnation process 12 hours.Then, to neutral, at 105 DEG C of temperature, be dried 8 hours with deionized water washing, can obtain comparative example 1 adsorbent.
comparative example 2
Commercially available 1g cocoanut active charcoal is added to the oxidizing solution H that the mass percent of 10ml is 30%
2o
2middle room temperature impregnation process 12 hours.Then, to neutral, at 105 DEG C of temperature, be dried 8 hours with deionized water washing, can obtain comparative example 2 adsorbents.
The performance test of adsorbent of the present invention is carried out in fixed-bed micro-reactor, reactor diameter is 10mm, get 0.26g adsorbent, be positioned over and in reactor, carry out performance evaluation, experiment condition is as follows: low-molecular-weight VOCs methyl alcohol, acetaldehyde and acetone produce by Bubbling method, carrier gas is compressed air, and control methanol concentration is 45mg/m
3, acetaldehyde concentration is 20mg/m
3, acetone concentration is 260mg/m
3, reaction velocity (GHSV) is 25,000h
-1, reaction temperature is 25 DEG C.
Table 1 embodiment and the comparison of comparative example adsorbent to low-molecular-weight VOCs absorption property
Result is as shown in table 1, and adsorbent of the present invention has excellent absorption property to low-molecular-weight VOCs at ambient temperature, is 5～15 times of commercially available conventional active carbon to the dynamic adsorption capacity of the low-molecular-weight volatile organic matters such as low concentration methanol, acetaldehyde and acetone.Adsorbent is carried out to physicochemical properties analysis, and as shown in Figure 1, adsorbent specific area of the present invention is large, all at 1400m
2more than/g, aperture is mainly distributed in 0.7～2nm, and pore volume is 0.4～0.8cm
3/ g, Micropore volume is 0.3～0.6cm
3/ g.Measure adsorbent surface oxygen-containing functional group by temperature programming, by curve shown in Fig. 2 A and Fig. 2 B, at CO
2in effusion process, in curve, there is the characteristic peak of hydroxy-acid group, carboxylic acid anhydride group and lactone groups; In CO effusion process, in curve, there is the characteristic peak of phenolic group group and anhydride group, therefore can judge, adsorbent surface of the present invention has been rich in oxygen-containing functional group, these oxygen-containing functional groups make adsorbent surface have hydrophily and polarity, are beneficial to the absorption of the low-molecular-weight VOCs equally with polarity.
Claims (6)
1. a carbide-derived carbon adsorbent of removing low concentration low-molecular-weight volatile organic matter, is characterized in that: this adsorbent specific area is at 1400m
2more than/g, pore volume is 0.4～0.8cm
3/ g, Micropore volume is 0.3～0.6cm
3/ g, aperture 0.7～2nm, adsorbent surface contains oxygen-containing functional group.
2. the preparation method of carbide-derived carbon adsorbent according to claim 1, is characterized in that having following preparation process:
(1) first commercial carbide is warming up to 600～900 DEG C in inert atmosphere, then changes logical chlorine and within 2～4 hours, carry out high temperature etching, chlorine flowrate is 30-50ml/min; Then, logical inert atmosphere is cooled to room temperature again, obtains carbide-derived carbon primary product;
(2) step (1) gained carbide-derived carbon primary product are added in oxidizing solution and carry out impregnation process 6～12 hours; Then, to neutral, at 105 DEG C of temperature, be dried 3～8 hours with deionized water washing, obtain carbide-derived carbon adsorbent final products.
3. the preparation method of carbide-derived carbon adsorbent according to claim 2, is characterized in that: described etch temperature is 700～800 DEG C.
4. the preparation method of carbide-derived carbon adsorbent according to claim 2, is characterized in that: described commercial carbide is any one in TiC, VC and NbC.
5. the preparation method of carbide-derived carbon adsorbent according to claim 2, is characterized in that: described oxidizing solution is that molar concentration is the HNO of 1～9mol/L
3, or the mass percent concentration H that is 5～30%
2o
2.
6. the application of carbide-derived carbon adsorbent according to claim 1, it is characterized in that: described adsorbent is applicable to carry out air cleaning processing in Indoor environment, closed in space and other confined spaces, and the described confined space contains low-molecular-weight volatile organic matter.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107093527A (en) * | 2017-04-14 | 2017-08-25 | 燕山大学 | A kind of method for improving carbide-derived carbon super capacitor performance |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1815007A (en) * | 2005-02-02 | 2006-08-09 | 可乐丽化学株式会社 | Active carbon and process for producing the same |
| WO2007070455A2 (en) * | 2005-12-09 | 2007-06-21 | Drexel University | Mesporous carbons |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1815007A (en) * | 2005-02-02 | 2006-08-09 | 可乐丽化学株式会社 | Active carbon and process for producing the same |
| WO2007070455A2 (en) * | 2005-12-09 | 2007-06-21 | Drexel University | Mesporous carbons |
Non-Patent Citations (3)
| Title |
|---|
| C. MORENO-CASTILLA等: "Activated Carbon Surface Modifications by Nitric Acid，Hydrogen Peroxide，and Ammonium Peroxydisulfate Treatments", 《LANGMUIR》 * |
| HONGYAN WANG等: "Adsorption and desorption of small molecule volatile organic compounds over carbide-derived carbon", 《CARBON》 * |
| HONGYAN WANG等: "Adsorption and desorption of small molecule volatile organic compounds over carbide-derived carbon", 《CARBON》, vol. 67, 31 October 2013 (2013-10-31), pages 712 - 720, XP028790301, DOI: doi:10.1016/j.carbon.2013.10.063 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107093527A (en) * | 2017-04-14 | 2017-08-25 | 燕山大学 | A kind of method for improving carbide-derived carbon super capacitor performance |
| CN107093527B (en) * | 2017-04-14 | 2019-02-22 | 燕山大学 | A method of improving carbide-derived carbon super capacitor performance |
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Effective date of registration: 20201214 Address after: No.1324, No.77, Changjiang Road, Yantai Economic and Technological Development Zone, Shandong Province Patentee after: Shandong Hangyuan Environmental Technology Co.,Ltd. Address before: 100191 No. 37, Haidian District, Beijing, Xueyuan Road Patentee before: BEIHANG University |
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