CN104359907A - Evaluation method of oxygen-containing functional group on surface of active carbon - Google Patents
Evaluation method of oxygen-containing functional group on surface of active carbon Download PDFInfo
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Abstract
The invention relates to a performance research method of an active carbon material, and in particular to an evaluation method of an oxygen-containing functional group on a surface of active carbon. The method comprises the following steps: (1) qualitatively judging the type of the oxygen-containing functional groups on the surfaces of to-be-tested carbon samples under different technical conditions by adopting a Fourier transform infrared spectrometer, wherein the testing conditions are as follows: the mass ratio of KBr to the carbon samples is 200:1, the thickness of a product tablet is 0.8mm-1.2mm, the scanning range is 4000cm<-1> to 450cm<-1>, the scanning speed is 0.20cm/s, the scanning time is 1min, the scanning times is 4, the unit of longitudinal coordinates is T% and the resolution ratio is 4.0cm<-1>; judging whether the surfaces of the to-be-tested carbon samples have the oxygen-containing functional groups such as carboxyl, lactone groups and phenolic hydroxyl groups or not according to a spectral peak, if so, executing step (2).
Description
Technical field
The present invention relates to the performance study method of absorbent charcoal material, be specially a kind of evaluation method of activated carbon surface oxygen-containing functional group.
Background technology
Activated charcoal has higher specific surface, abundant pore structure and is easy to the surface functional group of modulation, its surface chemistry has a great impact the surface reaction of activated charcoal, parent's (dredging) water-based, the tool such as catalytic property and surface charge, the dispersiveness of these properties influence catalyzer and activity, the absorption behavior etc. of adsorbent.And Surface Chemistry of Activated Carbon characteristic is to a great extent by classification and the quantity decision of surface functional group, modal functional group is oxygen-containing functional group.
At present, the domestic working specification that there is no a set of perfect activated carbon surface oxygen-containing functional group qualitative-and-quantitative method and standardization.
Summary of the invention
The object of the present invention is to provide a kind of evaluation method of activated carbon surface oxygen-containing functional group, the test method of a kind of reliable specification that this evaluation method is summed up by lot of experiments, for the selection of the catalytic performance of catalyzer and the absorption property of adsorbent provides theoretical foundation.
The present invention adopts following technical scheme to realize:
An evaluation method for activated carbon surface oxygen-containing functional group, comprises the steps:
(1), the to be measured charcoal sample of Fourier transformation infrared spectrometer to different technology conditions is adopted to qualitatively judge the classification of its surface oxygen functional group; Wherein, test condition is as follows:
Potassium bromide KBr and charcoal sample mass ratio to be measured are 200:1;
Sample sheeting thickness is 0.8 ~ 1.2mm;
Scan scope 4000 ~ 450cm
-1;
Scan speed 0.20cm/s, scan time 1min, scan number of times 4;
Ordinate unit T%;
Resolution 4.0cm
-1;
Judge whether charcoal sample to be measured surface contains the oxygen-containing functional group of carboxyl, lactone group and phenolic hydroxyl group according to spectrum peak, if containing, carry out step (2).
(2), the preparation of standard solution and demarcation
The preparation of a, 0.05mol/L HCl standard solution and demarcation;
The preparation of b, 0.05mol/L NaOH standard solution and demarcation;
C, 0.05mol/L Na
2cO
3the preparation of standard solution and demarcation;
D, 0.05mol/L NaHCO
3the preparation of standard solution and demarcation.
(3), sample granularity 200 order of charcoal sample to be measured, dry 24h for 120 DEG C, electronic balance is adopted accurately to take at least 3 parts, charcoal sample to be measured, put into taper triangular flask respectively, add the one in above-mentioned standard alkali lye, filter after vibration 24h and fully wash with wash bottle, collecting all filtrate, take methyl red as end point indicator, with still unreacted alkali lye in HCl standard solution titration filtrate to terminal.
(4), result calculates
The content n(mmol/g of the acidic functionality of unit mass activated charcoal and each standard alkaline reaction), calculate by formula (I), (II), (III):
The reacting dose of NaOH is as follows
n
NaOH=[c
NaOH×V
NaOH﹣c
HCl(V
HCl﹣△V
1﹣V
b)]/W…………………（ⅰ）
Na
2cO
3reacting dose as follows
n
Na2CO3=[2c
Na2CO3×V
Na2CO3﹣c
HCl(V
HCl﹣△V
2﹣V
b)]/W…………（ⅱ）
NaHCO
3reacting dose as follows
n
NaHCO3=[c
NaHCO3×V
NaHCO3﹣c
HCl(V
HCl﹣△V
3﹣V
b)]/W…………（ⅲ）
In formula: V
b-distilled water blank value (mL);
V
hClthe volume (mL) of the hydrochloric acid standard solution that-titration is used;
C
ithe concentration (mol/L) of the standard solution i that-subscript is corresponding;
W-sample mass (g);
The HCl standard solution volume modified value of theoretical end point when △ V-by the theoretical directing terminal of methyl red is corrected to acid base titration.
△V
1=(V
NaOH+V
HCl)([H
+]
R﹣[H
+]
T1)/c
HCl……………………（ⅳ）
△V
2=(2V
Na2CO3+V
HCl)([H
+]
R﹣[H
+]
T2)/c
HCl……………………（ⅴ）
△V
3=(V
NHCO3+V
HCl)([H
+]
R﹣[H
+]
T3)/c
HCl……………………（ⅵ）
Wherein, [H
+]
r=10
-5mol/L is the proton concentration of the theoretical directing terminal of methyl red; [H
+]
t1, [H
+]
t2, [H
+]
t3represent HCl titration NaOH, Na respectively
2cO
3and NaHCO
3time the proton concentration of theoretical end point.
From n
naOH, n
na2CO3and n
naHCO3between difference can to calculate the content of oxygen-containing functional group carboxyl, lactone group and phenolic hydroxyl group in charcoal sample to be measured as follows:
n
RCOOH=n
NaHCO3；
n
RCOOCOR=n
Na2CO3﹣n
NaHCO3；
n
ArOH=n
NaOH﹣n
Na2CO3。
In above-mentioned process of the test, as long as operation just can obtain, unfailing test data strong to the stability of charcoal sample to be measured as stated above, experimentally result is chosen the dedicated suction enclosure material removing toxic ingredient in contaminated air.
The present invention is reasonable in design, there is provided a kind of method of the active carbon adsorption material arbitrarily containing oxygen-containing functional groups such as carboxyl, lactone group and phenolic hydroxyl groups being carried out to reliable specification test, for the selection of the catalytic performance of catalyzer and the absorption property of adsorbent provides theoretical foundation.
Embodiment
Below specific embodiments of the invention are described in detail.
An evaluation method for activated carbon surface oxygen-containing functional group, comprises the steps:
(1), the to be measured charcoal sample of Spectrum100 type Fourier transformation infrared spectrometer to different technology conditions of PE company of the U.S. is adopted to qualitatively judge the classification of its surface oxygen functional group; Wherein, test condition is as follows:
KBr and charcoal sample mass ratio are 200:1;
Sample sheeting thickness is 0.8 ~ 1.2mm;
Scan scope 4000 ~ 450cm
-1;
Scan speed 0.20cm/s, scan time 1min, scan number of times 4;
Ordinate unit T%;
Resolution 4.0cm
-1.
Wherein, in order to obtain more clear, more satisfactory, the good spectrogram of quality, generally baseline correction and smoothing processing are carried out to spectrogram.
Judge that whether charcoal sample surface to be measured is containing oxygen-containing functional group carboxyl, lactone group and phenolic hydroxyl group according to spectrum peak, if containing, carry out step (2).
(2), the Acidity of Aikalinity of activated carbon surface causes primarily of carboxyl, lactone group and phenolic hydroxyl group, to react carry out quantitative test mensuration according to the alkali of varying strength from different oxygen-containing functional group.Wherein, NaHCO
3only and carboxyl, Na
2cO
3in and carboxyl and lactone group, in NaOH and carboxyl, lactone group, phenolic hydroxyl group.Adopt connection alkali neutralisation to measure and distinguish the quantitative test mensuration of acidic surface oxygen groups and basic group.
Preparation and the demarcation of standard solution are as follows:
The preparation of a, 0.05mol/L HCl standard solution and demarcation;
Measure 4.5mL hydrochloric acid, inject 1000mL water, shake up;
To take in 300 DEG C of high temperature furnaces calcination to the natrium carbonicum calcinatum standard reagent 0.01g of constant weight, be placed in 250mL conical flask, the water 50mL added without carbon dioxide dissolves, add 10 bromcresol greens-methyl red indicator solution, be titrated to solution with the hydrochloric acid solution prepared and become kermesinus from green, continuing to be titrated to solution after boiling 2min cooling is kermesinus, does blank test simultaneously.The numerical value of HCl standard solution is accurate to four figures after radix point.
The preparation of b, 0.05mol/L NaOH standard solution and demarcation;
Take 110g NaOH, be dissolved in 100mL and shake up without in the water of carbon dioxide, inject PE bottle airtight placement solution limpid, measure supernatant liquor 2.7mL with transfer pipet, be diluted to 1000mL with the water without carbon dioxide and shake up;
Take 110 DEG C of Potassium Hydrogen Phthalate standard reagent 0.36g dried to constant weight, be placed in 250mL conical flask, the water 50mL added without carbon dioxide dissolves, and adds 2 instructions phenolphthalein solutions (10g/L), be titrated to solution pinkiness with the sodium hydroxide solution prepared, and keep 30s.Do blank test simultaneously.The numerical value of NaOH standard solution is accurate to four figures after radix point.
C, 0.05mol/L Na
2cO
3the preparation of standard solution and demarcation;
Take natrium carbonicum calcinatum 5.3g, inject 1000mL water, shake up;
Measure the sodium carbonate liquor that 35.00mL prepares, add 20mL water, add 10 bromcresol greens-methyl red indicator solution, be titrated to solution become kermesinus from green with the hydrochloric acid solution of 0.05mol/L, continuing to be titrated to solution after boiling 2min cooling is kermesinus; By Na
2cO
3the numerical value of standard solution is accurate to four figures after radix point.
D, 0.05mol/L NaHCO
3the preparation of standard solution and demarcation;
Take natrium carbonicum calcinatum 4.201g, inject 1000mL water, shake up;
Measure the sodium carbonate liquor that 35.00mL prepares, add 20mL water, add 10 bromcresol greens-methyl red indicator solution, be titrated to solution become kermesinus from green with the hydrochloric acid solution of 0.05mol/L, continuing to be titrated to solution after boiling 2min cooling is kermesinus; By NaHCO
3the numerical value of standard solution is accurate to four figures after radix point.
(3), sample granularity 200 order of charcoal sample to be measured, dry 24h for 120 DEG C, adopt electronic balance accurately to take and treat that 1.0g surveys 6 parts, charcoal sample, put into 100ml taper triangular flask respectively, add the one in the above-mentioned standard alkali lye of 25ml, filter after vibration 24h and fully wash with wash bottle, collecting all filtrate, take methyl red as end point indicator, reddened by yellow to solution with still unreacted alkali lye in HCl standard solution titration filtrate.
Attention the choosing Fourier transformation infrared spectrometer test condition when carrying out qualitative test; Carrying out, quantitative test process is necessary rigorous, reduces error as far as possible.
(4), result calculates
The content n of the acidic functionality of unit mass activated charcoal and each standard alkaline reaction, unit is mmol/g, calculates by formula (I), (II), (III):
The reacting dose of NaOH is as follows
n
NaOH=[c
NaOH×V
NaOH﹣c
HCl(V
HCl﹣△V
1﹣V
b)]/W…………………（ⅰ）
Na
2cO
3reacting dose as follows
n
Na2CO3=[2c
Na2CO3×V
Na2CO3﹣c
HCl(V
HCl﹣△V
2﹣V
b)]/W…………（ⅱ）
NaHCO
3reacting dose as follows
n
NaHCO3=[c
NaHCO3×V
NaHCO3﹣c
HCl(V
HCl﹣△V
3﹣V
b)]/W…………（ⅲ）
In formula: V
b-distilled water blank value (mL);
V
hClthe volume (mL) of the hydrochloric acid standard solution that-titration is used;
C
ithe concentration (mol/L) of the standard solution i that-subscript is corresponding;
W-sample mass (g);
The HCl standard solution volume modified value of theoretical end point when △ V-by the theoretical directing terminal of methyl red is corrected to acid base titration.
△V
1=(V
NaOH+V
HCl)([H
+]
R﹣[H
+]
T1)/c
HCl………………………（ⅳ）
△V
2=(2V
Na2CO3+V
HCl)([H
+]
R﹣[H
+]
T2)/c
HCl………………………（ⅴ）
△V
3=(V
NHCO3+V
HCl)([H
+]
R﹣[H
+]
T3)/c
HCl………………………（ⅵ）
Wherein, [H
+]
r=10
-5mol/L is the proton concentration of the theoretical directing terminal of methyl red; [H
+]
t1, [H
+]
t2, [H
+]
t3represent HCl titration NaOH, Na respectively
2cO
3and NaHCO
3time the proton concentration of theoretical end point, its numerical value directly can be found from reference books.
Finally, from n
naOH, n
na2CO3and n
naHCO3between difference can to calculate the concrete content of carboxyl, lactone group and phenolic hydroxyl group as follows:
n
RCOOH=n
NaHCO3；
n
RCOOCOR=n
Na2CO3﹣n
NaHCO3；
n
ArOH=n
NaOH﹣n
Na2CO3。
Claims (5)
1. an evaluation method for activated carbon surface oxygen-containing functional group, is characterized in that: comprise the steps:
(1), the to be measured charcoal sample of Fourier transformation infrared spectrometer to different technology conditions is adopted to qualitatively judge the classification of its surface oxygen functional group; Wherein, test condition is as follows:
KBr and charcoal sample mass ratio to be measured are 200:1;
Sample sheeting thickness is 0.8 ~ 1.2mm;
Scan scope 4000 ~ 450cm
-1;
Scan speed 0.20cm/s, scan time 1min, scan number of times 4;
Ordinate unit T%;
Resolution 4.0cm
-1;
Judge whether charcoal sample to be measured surface contains the oxygen-containing functional group of carboxyl, lactone group and phenolic hydroxyl group according to spectrum peak, if containing, carry out step (2);
(2), the preparation of standard solution and demarcation
The preparation of a, 0.05mol/L HCl standard solution and demarcation;
The preparation of b, 0.05mol/L NaOH standard solution and demarcation;
C, 0.05mol/L Na
2cO
3the preparation of standard solution and demarcation;
D, 0.05mol/L NaHCO
3the preparation of standard solution and demarcation;
(3), sample granularity 200 order of charcoal sample to be measured, dry 24h for 120 DEG C, electronic balance is adopted accurately to take at least 3 parts, charcoal sample to be measured, put into taper triangular flask respectively, add the one in above-mentioned standard alkali lye, filter after vibration 24h and fully wash with wash bottle, collecting all filtrate, take methyl red as end point indicator, with still unreacted alkali lye in HCl standard solution titration filtrate to terminal;
(4), result calculates
The content n of the acidic functionality of unit mass activated charcoal and each standard alkaline reaction, unit is mmol/g, calculates by formula (I), (II), (III):
The reacting dose of NaOH is as follows
n
NaOH=[c
NaOH×V
NaOH﹣
HCl(V
HCl﹣△V
1-V
b)]/W ……………………（ⅰ）
Na
2cO
3reacting dose as follows
n
Na2CO3=[2c
Na2CO3×V
Na2CO3﹣c
HCl(V
HCl﹣△V
2﹣V
b)]/W ……………（ⅱ）
NaHCO
3reacting dose as follows
n
NaHCO3=[c
NaHCO3×V
NaHCO3﹣c
HCl(V
HCl﹣△V
3﹣V
b)]/W ……………（ⅲ）
In formula: V
b-distilled water blank value, Unit/mL;
V
hClthe volume of the hydrochloric acid standard solution that-titration is used, Unit/mL;
C
ithe concentration of the standard solution i that-subscript is corresponding, unit mol/L;
W-sample mass, unit g;
The HCl standard solution volume modified value of theoretical end point when △ V-by the theoretical directing terminal of methyl red is corrected to acid base titration;
△V
1=(V
NaOH+V
HCl)([H
+]
R﹣[H
+]
T1)/c
HCl…………….…………（ⅳ）
△V
2=(2V
Na2CO3+V
HCl)([H
+]
R﹣[H
+]
T2)/c
HCl………………………（ⅴ）
△V
3=(V
NHCO3+V
HCl)([H
+]
R﹣[H
+]
T3)/c
HCl………………………（ⅵ）
Wherein, [H
+]
r=10
-5mol/L is the proton concentration of the theoretical directing terminal of methyl red; [H
+]
t1, [H
+]
t2, [H
+]
t3represent HCl titration NaOH, Na respectively
2cO
3and NaHCO
3time the proton concentration of theoretical end point;
From n
naOH, n
na2CO3and n
naHCO3between difference can to calculate the content of carboxyl, lactone group and phenolic hydroxyl group as follows:
n
RCOOH=n
NaHCO3；
n
RCOOCOR=n
Na2CO3﹣n
NaHCO3；
n
ArOH=n
NaOH﹣n
Na2CO3。
2. the evaluation method of activated carbon surface oxygen-containing functional group according to claim 1, is characterized in that: in step (2), and the preparation of 0.05mol/L HCl standard solution and demarcation are specific as follows:
Measure 4.5mL hydrochloric acid, inject 1000mL water, shake up;
To take in 300 DEG C of high temperature furnaces calcination to the natrium carbonicum calcinatum standard reagent 0.01g of constant weight, be placed in 250mL conical flask, the water 50mL added without carbon dioxide dissolves, add 10 bromcresol greens-methyl red indicator solution, be titrated to solution with the hydrochloric acid solution prepared and become kermesinus from green, continuing to be titrated to solution after boiling 2min cooling is kermesinus, does blank test simultaneously; The numerical value of HCl standard solution is accurate to four figures after radix point.
3. the evaluation method of activated carbon surface oxygen-containing functional group according to claim 1, is characterized in that: in step (2), and the preparation of 0.05mol/L NaOH standard solution and demarcation are specific as follows:
Take 110g NaOH, be dissolved in 100mL and shake up without in the water of carbon dioxide, inject PE bottle airtight placement solution limpid, measure supernatant liquor 2.7mL with transfer pipet, be diluted to 1000mL with the water without carbon dioxide and shake up;
Take 110 DEG C of Potassium Hydrogen Phthalate standard reagent 0.36g dried to constant weight, be placed in 250mL conical flask, the water 50mL added without carbon dioxide dissolves, and adds 2 instructions phenolphthalein solutions, is titrated to solution pinkiness, and keeps 30s with the sodium hydroxide solution prepared; Do blank test simultaneously; The numerical value of NaOH standard solution is accurate to four figures after radix point.
4. the evaluation method of activated carbon surface oxygen-containing functional group according to claim 1, is characterized in that: in step (2), 0.05mol/L Na
2cO
3the preparation of standard solution and demarcation, specific as follows:
Take natrium carbonicum calcinatum 5.3g, inject 1000mL water, shake up;
Measure the sodium carbonate liquor that 35.00mL prepares, add 20mL water, add 10 bromcresol greens-methyl red indicator solution, be titrated to solution become kermesinus from green with the hydrochloric acid solution of 0.05mol/L, continuing to be titrated to solution after boiling 2min cooling is kermesinus; By Na
2cO
3the numerical value of standard solution is accurate to four figures after radix point.
5. the evaluation method of activated carbon surface oxygen-containing functional group according to claim 1, is characterized in that: in step (2), 0.05mol/L NaHCO
3the preparation of standard solution and demarcation, specific as follows:
Take natrium carbonicum calcinatum 4.201g, inject 1000mL water, shake up;
Measure the sodium carbonate liquor that 35.00mL prepares, add 20mL water, add 10 bromcresol greens-methyl red indicator solution, be titrated to solution become kermesinus from green with the hydrochloric acid solution of 0.05mol/L, continuing to be titrated to solution after boiling 2min cooling is kermesinus; By NaHCO
3the numerical value of standard solution is accurate to four figures after radix point.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105424642A (en) * | 2015-12-11 | 2016-03-23 | 浙江新安化工集团股份有限公司 | Method for measuring content of alkyl groups or alkoxy groups in polysiloxane |
| CN106018673A (en) * | 2016-07-21 | 2016-10-12 | 中国科学院山西煤炭化学研究所 | Quantitative analysis method for surface oxygenic functional groups of graphene materials |
| CN113687014A (en) * | 2021-08-04 | 2021-11-23 | 山东利特纳米技术有限公司 | Qualitative and quantitative analysis method for graphene oxide surface functional groups |
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2014
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105424642A (en) * | 2015-12-11 | 2016-03-23 | 浙江新安化工集团股份有限公司 | Method for measuring content of alkyl groups or alkoxy groups in polysiloxane |
| CN106018673A (en) * | 2016-07-21 | 2016-10-12 | 中国科学院山西煤炭化学研究所 | Quantitative analysis method for surface oxygenic functional groups of graphene materials |
| CN113687014A (en) * | 2021-08-04 | 2021-11-23 | 山东利特纳米技术有限公司 | Qualitative and quantitative analysis method for graphene oxide surface functional groups |
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Application publication date: 20150218 |