Піролізна регенерація активованого вугілля використаного для очищення гліцерину
In this work, we investigated granular activated carbons Norit 1240 (AC) – initial and spent (SAC) with adsorbed impurities after purification of technical glycerin and subsequent washing with water. The aim of the work was to establish the optimal conditions for the thermal regeneration of AC at th...
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Chuiko Institute of Surface Chemistry National Academy of Sciences of Ukraine
2022
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Surface| _version_ | 1869291913206562816 |
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| author | Борисенко, М. В. Борисенко, Л. І. Клюс, В. П. Клюс, С. В. Шинкаренко, В. І. |
| author_facet | Борисенко, М. В. Борисенко, Л. І. Клюс, В. П. Клюс, С. В. Шинкаренко, В. І. |
| author_institution_txt_mv | [
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"author": "М. В. Борисенко",
"institution": "Інститут хімії поверхні ім. О.О.Чуйка Національної академії наук України"
},
{
"author": "Л. І. Борисенко",
"institution": "Інститут відновлювальної енергетики Національної академії наук України"
},
{
"author": "В. П. Клюс",
"institution": "Інститут відновлювальної енергетики Національної академії наук України"
},
{
"author": "С. В. Клюс",
"institution": "Інститут відновлювальної енергетики Національної академії наук України"
},
{
"author": "В. І. Шинкаренко",
"institution": "Полтавський національний педагогічний університет ім. В.Г. Короленка"
}
] |
| author_sort | Борисенко, М. В. |
| baseUrl_str | |
| collection | OJS |
| datestamp_date | 2023-04-20T10:24:32Z |
| description | In this work, we investigated granular activated carbons Norit 1240 (AC) – initial and spent (SAC) with adsorbed impurities after purification of technical glycerin and subsequent washing with water. The aim of the work was to establish the optimal conditions for the thermal regeneration of AC at the pyrolysis unit and to quantify the adsorbed impurities in the SAC using thermogravimetric analysis (TGA). For all AC samples, the specific surface area (S), adsorption activity on iodine and mass fraction of moisture were measured. It was established by the TGA method that water is released in the temperature range of 20 – 180 °C, and glycerin – 180 – 400 °C. Spent AC contains up to 31.3 wt. % H2O and up to 37.3 wt. % C3H5(OH)3. The pyrolysis reactor was used for the regeneration of SAC samples. It was shown that after the reactivation of SACs, their specific surface area is restored to 45-94% of the initial one. There is a weak correlation between S and iodine number, R=0.64. Adsorption activity for iodine and S increase in the same row ACspent > ACregenerated > ACinitial. As a result of regeneration, activated carbons suitable for reuse were obtained. |
| doi_str_mv | 10.15407/Surface.2022.14.095 |
| first_indexed | 2025-09-24T17:25:28Z |
| format | Article |
| fulltext |
Поверхня. 2022. Вип. 14(29). С. 95–100 95
ФІЗИКО‐ХІМІЯ ПОВЕРХНЕВИХ ЯВИЩ
UDC 544.723; 661.183.2
PYROLYSIS REGENERATION OF ACTIVATED
CARBON USED FOR GLYCERIN PURIFICATION
M.V. Borysenko1, L.I. Borysenko2, V.P. Klius2, S.V. Klius2, V.I. Shynkarenko3
1
Chuiko Institute of Surface Chemistry, NAS of Ukraine, 17 General Naumov Str., Kyiv 03164,
Ukraine, borysenko@nas.gov.ua
2
Institute of Renewable Energy, NAS of Ukraine, 20A Hnata Khotkevycha Str., Kyiv 02094,
Ukraine
3Poltava V.G. Korolenko National Pedagogical University, 2 Ostrohradskyi Str.,
Poltava 36003, Ukraine
In this work, we investigated granular activated carbons Norit 1240 (AC) – initial and
spent (SAC) with adsorbed impurities after purification of technical glycerin and subsequent
washing with water. The aim of the work was to establish the optimal conditions for the thermal
regeneration of AC at the pyrolysis unit and to quantify the adsorbed impurities in the SAC using
thermogravimetric analysis (TGA). For all AC samples, the specific surface area (S), adsorption
activity on iodine and mass fraction of moisture were measured. It was established by the TGA
method that water is released in the temperature range of 20 – 180 °C, and glycerin – 180 – 400
°C. Spent AC contains up to 31.3 wt. % H2O and up to 37.3 wt. % C3H5(OH)3. The pyrolysis
reactor was used for the regeneration of SAC samples. It was shown that after the reactivation of
SACs, their specific surface area is restored to 45-94% of the initial one. There is a weak
correlation between S and iodine number, R=0.64. Adsorption activity for iodine and S increase
in the same row ACspent > ACregenerated > ACinitial. As a result of regeneration, activated
carbons suitable for reuse were obtained.
Key words: spent activated carbon, thermal analysis, regeneration, pyrolysis reactor
Introduction
Glycerin, the simplest triatomic alcohol C3H5(OH)3, is a product of the multi-ton
chemical industry. It is used in paints, food, medical, textile, paper, leather, tobacco, agriculture,
detergents and cosmetics, plastics such as polyurethanes, glyphthalic, alkyd and epoxy resins [1].
A reliable way to purify glycerin from impurities is their adsorption using activated
carbon (AC) [1 – 3]. However, after prolonged usage, adsorption capacity of the resulted spent
AC (SAC) reached saturation which affects its adsorption performances [3]. Reactivation can be
carried out by various routes which include thermal reactivation (in the presence of steam/CO2),
chemical reactivation (treated with different chemicals e.g. KOH, NaOH, ZnCl2, H2SO4) and
bioreactivation (using microorganisms) [2 – 4].
In this work, the adsorption capability of SAC was restored by thermal reactivation in a
pyrolysis reactor. Thermogravimetric analysis was used for the quantitative and qualitative
evaluation of adsorbed impurities in the spent adsorbent. The presented material is a continuation
of the general research direction of the laboratory of oxide nanocomposites of the Chuiko
Institute of Surface Chemistry regarding the synthesis and characterization of carbon adsorbents
[4 – 10].
96
Materials and methods
In this work, we investigated granular activated carbons Norit 1240 – initial and spent
with adsorbed impurities after purification of technical glycerin. ACs were purchased from LLC
"Ukrhimresurs", Ukraine. The numbering and characteristics of AC samples are given in the
table.
Thermogravimetric analysis of AC samples was carried out in air using a Q-1500D
derivatograph (Hungary) with computer data recording. The heating rate was 10 °C/min, the
weight was 0.15 g.
The specific surface area of the samples was measured by the chromatographic method of
low-temperature adsorption of argon at -196 °C [11]. The essence of the method is that the
experimental samples are analyzed in identical conditions to the standard sample with the known
and stable for a long time specific surface. In this case certified reference material BAM-P109
(activated nanoporous carbon) with BET specific surface area of 1396±24 m2/g was used as a
standard. The value of the specific surface of the experimental sample can be calculated by the
formula: S = SstꞏFstꞏmst/F/m, where S і Sst – is the specific surface of the sample under study and
the standard, m2/g; F і Fst – the area of the desorption peak of the sample and the standard
(chromatographic data), arb. unit.; m і mst – is the weight of the sample and the standard
respectively, g. Acceptable measurement error was 10%. The gas mixture of 5 vol.% Ar (gas
adsorbate) and 95 vol. % He (gas carrier) was used in the experiment.
Adsorption activity on iodine and Mass fraction of moisture were measured according to
GOST 6217 [12] and GOST 12597 [13], respectively.
Table. Physico-chemical characteristics of the initial, spent and regenerated activated carbons
##
AC
Sample Specific surface
area, m2
/g
Adsorption activity
on iodine, %
Mass fraction of
moisture, %
Mass fraction
of glycerin, %
1 1initial 931 83 0,8 –
2 1spent 56 53 14,5 37.3
3 1.0 regenerated 623 64 0,6 not determined
4 1.1 regenerated 799 84 0,5 1.8
5 1.2 regenerated 542 75 0,9 6.8
6 2initial 924 92 1,3 –
7 2spent 242 48 31,3 7.1
8 2.0 regenerated 865 58 0,3 not determined
9 2.1 regenerated 447 85 0,3 not determined
Results and discussion
Figure 1 shows at the same scale the thermograms of the initial ACs (#1, #6) and spent
ACs (#2, #7) activated carbons. On the thermograms of the samples, weight loss is observed
with maxima at ~ 100 °C and 260 – 275 °C in the temperature range 20 – 550 °C (DTG). The
first process refers to the loss of adsorbed water; it is also observed for the initial activated
carbon. The second process is the evaporation of glycerin [4]. It is clearly seen from the DTG
curves that H2O is released in the temperature range 20 – 180 °C, and C3H5(OH)3– 180 – 400 °C.
This makes it possible to calculate their amount in samples (table). Spent ACs (#2/#7) contain
14,5/31,3 wt. % H2O and 37,3/7,1 wt. % C3H5(OH)3, respectively.
The pyrolysis reactor (Institute of Renewable Energy of the National Academy of
Sciences of Ukraine, Department of Renewable Organic Energy) has been used for the
regeneration of spent activated carbon (Fig. 2).
97
100 200 300 400 500 600 700 800 9001000
100
90
80
70
60
50
40
30
20
10
0
100 200 300 400 500 600 700 800 9001000
-0,6
-0,4
-0,2
0,0
100 200 300 400 500 600 700 800 9001000
-0,6
-0,4
-0,2
0,0
100 200 300 400 500 600 700 800 9001000
100
90
80
70
60
50
40
30
20
10
0
W
e
ig
h
t
lo
ss
,
%
1
2
6
Temperature, °C
D
T
G
,
re
la
tiv
e
u
n
its
1
2
6
Temperature, °C
4
5
5
4
D
T
G
,
re
la
tiv
e
u
n
its
7
W
e
ig
h
t
lo
ss
,
%
7
Fig. 1. TG, DTG – thermal analysis curves of initial (1, 6), spent (2, 7) and regenerated (4, 5)
AC. The numbering of the curves corresponds to #AC samples as in the table
The pyrolysis reactor is designed for recycling fuel into generator gas (full gasification),
or pyrolysis gas and AC (partial gasification or oxidative pyrolysis). The process of partial fuel
gasification is carried out in a gas generator with a moving gasification zone (Fig. 2). After
igniting the fuel (in our case, wheat straw pellets), the gasification zone begins to move towards
the air flow at a constant speed. The SAC layer is continuously heated; volatile substances are
released and oxidized by the blowing air. Next, the gasification reactions of SAC with water
vapor and carbon dioxide formed in the pyrolysis process proceed. Behind the gasification zone
remains a layer of hot AC, in which thermal decomposition of resins takes place [14].
AC2 was regenerated at three different regimes (samples 3-5) and AC7 – at two ones
(samples 8, 9). The regimes differed in different rates of air supply to the lower part of the
reactor.
As a result, the amount of water (Table) and glycerin in the samples were significantly
reduced. The glycerin content of AC4 and AC5 was determined from TG curves (Fig. 1).
98
Fig. 2. Photo of the pyrolysis reactor and the scheme of regeneration of spent activated carbon
1 2 3 4 5 6 7 8 9
0
20
40
60
80
100
## AC
1.2
1.1
D
eg
re
e
of
r
eg
en
er
at
io
n,
%
1 initial
1 spent
1.0
2 initial
2 spent
2.0
2.1
0 200 400 600 800 1000
40
50
60
70
80
90
100
4
6
1
8
3
5
7
9
A
ds
or
pt
io
n
a
ct
iv
ity
o
n
io
di
ne
,
%
Specific surface area, m2/g
2
spent initialregenerated
Fig. 3. The degree of AC regeneration,
calculated from the values of the
specific surface area
Fig. 4. Dependence between specific surface
area and iodine number of ACs
The value of the specific surface area of the samples (S) was taken as a measure of the
degree of regeneration. The specific surface area of the initial granular adsorbents is 931 and 924
m2/g, respectively, and is taken as 100 %. After using these adsorbents in the process of
purifying glycerin, their S decreases to 56 m2/g (sample AC2) and to 242 m2/g (sample AC7).
99
After regeneration, the specific surface area increases to 447-865 m2/g. The highest degree of
regeneration of the AC samples after activation was 85 % (AC4) and 94 % (AC8) (Fig. 3). Such
ACs can be used to repurify glycerin.
The iodine number is a relative indicator of the porosity of activated carbons. The iodine
number is not a measure of the ability of activated carbons to adsorb other substances. The
iodine number can be used to approximate the specific surface area of some types of activated
carbons. However, it must be taken into account that strict relationships between specific surface
area and iodine number cannot be established. These indicators vary depending on the source
material of activated carbons, on the conditions for their preparation and the pore size
distribution in them. The presence of adsorbed volatile substances, sulfur and water-extractable
substances in ACs can affect the value of the iodine number. [12]. As can be seen from Fig. 4,
there is still a weak correlation between S and iodine number, R=0.64. Adsorption activity for
iodine and S increase in the same row ACspent > ACregenerated > ACinitial. No such
dependence was observed for methylene blue [4].
Conclusions
Using thermogravimetric analysis, a quantitative and qualitative evaluation of adsorbed
impurities in spent activated carbon Norit 1240 after glycerol purification was carried out. It has
been established that H2O is released in the temperature range 20 – 180 °C, and C3H5(OH)3–
180 – 400 °C. Spent AC contains up to 31.3 wt. % H2O and up to 37.3 wt. % C3H5(OH)3.
The pyrolysis reactor has been successfully used for the regeneration of spent activated
carbon. It is shown that after the reactivation of SACs, their specific surface area is restored to
45-94 % of the initial one. There is a weak correlation between S and iodine number, R=0.64.
Adsorption activity for iodine and S increase in the same row ACspent > ACregenerated >
ACinitial. Subject to the optimal regeneration regime, samples suitable for reuse can be obtained.
References
1. Ardi M.S., Aroua M.K., Hashim N. Awanis. Progress, prospect and challenges in glycerol
purification process: A review. Renewable and Sustainable Energy Reviews. 2015. 42:1164.
2. Patent UA 97323. Skachko V.P., Chorna T.S. The method of purification of glycerin. 2015.
3. Khok Y.-T., Ooi C.-H., Matsumoto A., Yeoh F.-Y. Reactivation of spent activated carbon for
glycerine purification. Adsorption. 2020. 26:1015.
4. Borysenko M.V., Chubenko Ya.M., Voitko I.I., Chorna T.S. Thermal analysis as a method for
evaluating the quality of regeneration of activated carbon used for purification of glycerine.
Poverhn. 2020. 12(27): 137. [in Russian].
5. Makhno S.N., Bogatyrov V.M., Gunya G.M., Oranska E.I., Cherniavska Т.V., Borysenko
M.V., Gorbyk P.P. Synthesis and electrophysical properties of composites based on porous
carbon and metal nickel nanoparticles. Nanostructured Materials Science. 2013. 2: 79. [in
Russian].
6. Galaburda M.V., Bogatyrov V.M., Oranska O.I., Skubiszewska-Zieba J., Gun’ko V.M.,
Sternik D. Magneto-sensitive Ni/C adsorbents: Synthesis, properties and applications.
Adsorption Science & Technology. 2015. 33(6–8): 523.
7. Galaburda M., Bogatyrov V., Oranska O., Gun’ko V., Skubiszewska-Zięba J., Urubkov I.
Synthesis and characterization of carbon composites containing Fe, Co, Ni nanoparticles. J.
Therm. Analysis and Calorimetry. 2015. 122(2): 553.
8. Bogatyrov V.M., Galaburda M.V., Oranska O.I., Borysenko M.V., Vasilyeva O.O., Voitko I.I.
Synthesis and adsorption properties of magneto-sensitive nanocomposites based on Ni/C.
Poverhn. 2015. 7(22): 196. [in Russian].
100
9. Galaburda M.V., Bogatyrov V.M., Skubiszewska-Zięba J., Oranska O.I., Sternic D., Gunko
V.M. Synthesis and structural features of resorcinol-formaldehyde resin chars containing nickel
nanoparticles. Appl. Surf. Sci. 2016. 360: 722.
10. Galaburda M.V., Bogatyrov V.M., Tomaszewski W., Oranska O.I., Borysenko M.V.,
Skubiszewska-Zięba J., Gun’ko V.M. Adsorption/desorption of explosives on Ni–, Co–, and
NiCo–carbon composites: Application in solid phase extraction. Colloids and Surfaces A. 2017.
529: 950.
11. Interstate Standard (GOST 14922-77). Aerosil (silicon dioxide). Specifications
http://vsegost.com/Catalog/15/15604.shtml.
12. Interstate Standard (GOST 6217-74). Wood crushed activated carbon. Specifications
https://files.stroyinf.ru/Data2/1/4294823/4294823192.pdf.
13. Interstate Standard (GOST 12597-67). Method for determination of moisture fraction of total
mass in activated carbons and catalysts on their base. Specifications
http://vsegost.com/Catalog/44/44006.shtml.
14. Klius S.V. Ph.D (Techn.) Thesis. (Kyiv, 2017). [in Ukrainian].
ПІРОЛІЗНА РЕГЕНЕРАЦІЯ АКТИВОВАНОГО ВУГІЛЛЯ
ВИКОРИСТАНОГО ДЛЯ ОЧИЩЕННЯ ГЛІЦЕРИНУ
М.В. Борисенко1, Л.І. Борисенко2, В.П. Клюс2, С.В. Клюс2, В.І. Шинкаренко3
1Інститут хімії поверхні ім. О.О. Чуйка Національної академії наук України
вул. Генерала Наумова 17, Київ, 03164, Україна, borysenko@nas.gov.ua
2Інститут відновлювальної енергетики Національної академії наук України
вул. Гната Хоткевича, 20а, Київ, 02094, Україна
3Полтавський національний педагогічний університет ім. В.Г. Короленка, вул.
Остроградська, 2, Полтава, 36003, Україна
В роботі досліджували гранульовані активовані вугілля Norit 1240 (АВ) – вихідні
та відпрацьовані з адсорбованими домішками після очищення технічного гліцерину та
подальшого промивання водою. Мета роботи – встановлення оптимальних умов
термічної регенерації АВ на установці піролізу та кількісне визначення адсорбованих
домішок у відпрацьованому АВ за допомогою термогравіметричного аналізу (ТГА). Для
всіх зразків АВ вимірювали питому поверхню (S), адсорбційну активність по йоду та
масову частку вологи. Методом ТГА встановлено, що вода виділяється в інтервалі
температур 20 – 180 °С, а гліцерин – 180 – 400 °С. Відпрацьоване АВ містить до 31,3
мас. % H2O і до 37,3 мас. % C3H5(OH)3. Для регенерації зразків АВ використали піролізний
реактор. Показано, що після реактивації відпрацьованих АВ їх питома поверхня
відновлюється до 45-94% від початкової. Спостерігається слабка кореляція між S та
йодним числом, R=0,64. Адсорбційна активність по йоду та S збільшується в тому
самому ряду AВвідпрацьоване > AВрегенероване > AВвихідне. В результаті регенерації
отримано активоване вугілля, придатне для повторного використання.
Ключові слова: відпрацьоване активоване вугілля, термічний аналіз, регенерація,
піролізний реактор
|
| id | oai:ojs.pkp.sfu.ca:article-748 |
| institution | Surface |
| keywords_txt_mv | keywords |
| language | English |
| last_indexed | 2025-09-24T17:45:58Z |
| publishDate | 2022 |
| publisher | Chuiko Institute of Surface Chemistry National Academy of Sciences of Ukraine |
| record_format | ojs |
| resource_txt_mv | surfacezbircomua/19/7ae05d20da423883465a53dcac8e5119.pdf |
| spelling | oai:ojs.pkp.sfu.ca:article-7482023-04-20T10:24:32Z Pyrolysis regeneration of activated carbon used for glycerin purification Піролізна регенерація активованого вугілля використаного для очищення гліцерину Борисенко, М. В. Борисенко, Л. І. Клюс, В. П. Клюс, С. В. Шинкаренко, В. І. spent activated carbon thermal analysis regeneration pyrolysis reactor відпрацьоване активоване вугілля термічний аналіз регенерація піролізний реактор In this work, we investigated granular activated carbons Norit 1240 (AC) – initial and spent (SAC) with adsorbed impurities after purification of technical glycerin and subsequent washing with water. The aim of the work was to establish the optimal conditions for the thermal regeneration of AC at the pyrolysis unit and to quantify the adsorbed impurities in the SAC using thermogravimetric analysis (TGA). For all AC samples, the specific surface area (S), adsorption activity on iodine and mass fraction of moisture were measured. It was established by the TGA method that water is released in the temperature range of 20 – 180 °C, and glycerin – 180 – 400 °C. Spent AC contains up to 31.3 wt. % H2O and up to 37.3 wt. % C3H5(OH)3. The pyrolysis reactor was used for the regeneration of SAC samples. It was shown that after the reactivation of SACs, their specific surface area is restored to 45-94% of the initial one. There is a weak correlation between S and iodine number, R=0.64. Adsorption activity for iodine and S increase in the same row ACspent > ACregenerated > ACinitial. As a result of regeneration, activated carbons suitable for reuse were obtained. В роботі досліджували гранульовані активовані вугілля Norit 1240 (АВ) – вихідні та відпрацьовані з адсорбованими домішками після очищення технічного гліцерину та подальшого промивання водою. Мета роботи – встановлення оптимальних умов термічної регенерації АВ на установці піролізу та кількісне визначення адсорбованих домішок у відпрацьованому АВ за допомогою термогравіметричного аналізу (ТГА). Для всіх зразків АВ вимірювали питому поверхню (S), адсорбційну активність по йоду та масову частку вологи. Методом ТГА встановлено, що вода виділяється в інтервалі температур 20 – 180 °С, а гліцерин – 180 – 400 °С. Відпрацьоване АВ містить до 31,3 мас. % H2O і до 37,3 мас. % C3H5(OH)3. Для регенерації зразків АВ використали піролізний реактор. Показано, що після реактивації відпрацьованих АВ їх питома поверхня відновлюється до 45-94% від початкової. Спостерігається слабка кореляція між S та йодним числом, R=0,64. Адсорбційна активність по йоду та S збільшується в тому самому ряду AВвідпрацьоване > AВрегенероване > AВвихідне. В результаті регенерації отримано активоване вугілля, придатне для повторного використання. Chuiko Institute of Surface Chemistry National Academy of Sciences of Ukraine 2022-11-30 Article Article application/pdf https://surfacezbir.com.ua/index.php/surface/article/view/748 10.15407/Surface.2022.14.095 Surface; No. 14(29) (2022): Surface; 95-100 Поверхность; № 14(29) (2022): Поверхня; 95-100 Поверхня; № 14(29) (2022): Поверхня; 95-100 3154-8091 3154-8083 10.15407/Surface.2022.14 en https://surfacezbir.com.ua/index.php/surface/article/view/748/742 Авторське право (c) 2022 М.В. Борисенко, Л.І. Борисенко, В.П. Клюс, С.В. Клюс, В.І. Шинкаренко |
| spellingShingle | відпрацьоване активоване вугілля термічний аналіз регенерація піролізний реактор Борисенко, М. В. Борисенко, Л. І. Клюс, В. П. Клюс, С. В. Шинкаренко, В. І. Піролізна регенерація активованого вугілля використаного для очищення гліцерину |
| title | Піролізна регенерація активованого вугілля використаного для очищення гліцерину |
| title_alt | Pyrolysis regeneration of activated carbon used for glycerin purification |
| title_full | Піролізна регенерація активованого вугілля використаного для очищення гліцерину |
| title_fullStr | Піролізна регенерація активованого вугілля використаного для очищення гліцерину |
| title_full_unstemmed | Піролізна регенерація активованого вугілля використаного для очищення гліцерину |
| title_short | Піролізна регенерація активованого вугілля використаного для очищення гліцерину |
| title_sort | піролізна регенерація активованого вугілля використаного для очищення гліцерину |
| topic | відпрацьоване активоване вугілля термічний аналіз регенерація піролізний реактор |
| topic_facet | spent activated carbon thermal analysis regeneration pyrolysis reactor відпрацьоване активоване вугілля термічний аналіз регенерація піролізний реактор |
| url | https://surfacezbir.com.ua/index.php/surface/article/view/748 |
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