İğde çekirdeği ve kayın ağacından üretilen aktif karbonun ağır metal ve boyarmadde gideriminde kullanılması
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Tarih
2015-07-28
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Selçuk Üniversitesi Fen Bilimleri Enstitüsü
Erişim Hakkı
info:eu-repo/semantics/openAccess
Özet
Doktora tez çalışması kapsamında yapılan deneysel çalışmalar iki basamakta gerçekleştirilmiştir. Birinci basamakta öğtülmüş iğde çekirdeği ve kayın ağacı talaşından ZnCI2, H3PO4, H2SO4, Na2CO3 ve KOH aktifleştiricileri kullanılarak azot gazı varlığında kimyasal aktivasyon yöntemi ve CO2 ile su buharı gaz karışımı varlığında fiziksel aktivasyon yöntemiyle aktif karbon üretim şartları belirlenmiştir. Kimyasal aktivasyon yöntemiyle aktif karbon hazırlanmasında; aktifleştirici/hammadde oranı, aktifleştirici emdirilme süresi, aktivasyon sıcaklığı ve aktivasyon süresi parametrelerinin etkileri incelenmiştir. Fiziksel aktivasyon yöntemiyle aktif karbon hazırlanırken aktivasyon sıcaklığı ve aktivasyon süresi parametrelerinin etkileri incelenmiştir. Elde edilen aktif karbonların iyon sayıları belirlenerek yüksek iyot sayısına sahip aktif karbonların kararkterizasyonu; yüzey alanı (BET), FT-IR ve SEM cihazlarıyla gerçekleştirilmiştir. Sentezlenen yüksek iyot sayısına sahip aktif aktif karbonların BET yüzey alanı belirlenmiş ve yüksek yüzey alanına sahip olanlar, kimyasal emdirilmiş ama aktifleştirilmemiş numune ve hammaddenin yüzey morfolojisi SEM analizi ile gerçekleştirilmiştir. Yüksek yüzey alanına sahip olan aktif karbon, kimyasal emdirilmiş ama aktifleştirilmemiş numunelerin, hammadde ve adsorpsiyondan sonraki aktif karbonların kimyasal yapısı FT-IR cihazı yardım ile belirlenmiştir. İğde çekirdeğinden ZnCI2 ve H3PO4 aktifleştiricileri ile elde edilen aktif karbonların kodlanlanması sırasıyla İÇAC ve İFAC iken kayın ağacından ZnCI2 ve H3PO4 aktifleştiricisi ile elde edilen aktif karbonlar sırasıyla KÇAC ve KFAC olarak kodlanmaştır. Çalışmanın ikinci basamağında ise yüksek yüzey alanlarına sahip İÇAC38, İÇAC75, İFAC84, KÇAC85 ve KFAC88 kodlu aktif karbonlar seçilerek metilen mavisi ve malahit yeşili boyarmaddeleri ve kurşun(II) ve krom(VI) ağır metallerinin adsorpsiyonunda kullanılmıştır. Boyarmadde ve ağır metal adsorpsiyonunda zaman, çözelti başlangıç derişimi, çözelti başlangıç pH'ı, aktif karbon miktarı ve çözelti ortamı sıcaklığı parametrelerinin etkileri incelenmiştir. Adsorpsiyon denge verileri Langmuir, Freundlich, Temkin, D-R izotermlerine uygulanmıştır. Adsorpsiyon kinetiğinin incelenmesi için yalancı birinci derece, yalancı ikinci derece, Elovich ve partikül içi difüzyon modelleri incelenmiştir. Adsorpsiyon termodinamik parametreleri belirlenmiştir. İÇAC38, İÇAC75, İFAC84, KÇAC85 ve KFAC88 kodlu aktif karbonlar kullanılarak ağır metal ve boyarmadde adsorpsiyonun deney tasarımı gerçekleştirilmiştir. Deney tasarımı Design Expert bilgisayar programının Yüzey Yanıt Yöntemi bünyesinde yer alan Box-Behnken tasarım modeli kullanılarak yapılmıştır. Deney tasarımında; çözelti başlangıç derişimi, çözelti ortamı sıcaklığı ve zaman parametrelerinin ikili değerlerinin adsorpsiyon kapasitesine olan etkileri incelenmiştir. Yüzey Yanıt Yöntemi Box-Behnken tasarım modeli ile her bir ağır metal ve boyarmadde için ANOVA tablosu oluşturularak seçilen parametrelerin adsorpsiyon kapasitesine tekli ve ikili etkileri belirlenmiştir. Deney tasarım metodu ile seçilen parametrelerin boyarmadde ve ağır metal adsorsiyon kapasitesine olan etkileri 3 boyutlu grafikleri çizilerek incelenmiştir. Box-Behnken tasarım modeliyle hem ağır metal hem de boyarmadde için regresyon işlemi yapılmış ve regresyon eşitlikleri türetilmiştir. Regresyon eşitliği ile tahmin edilen adsorpsiyon kapasitesi sonuçları ile deneysel olarak elde edilen adsorpsiyon kapasitesi sonuçların birbirine çok yakın olduğu tespit edilmiştir. Box-Behnken tasarım modeliyle seçilen parametrelerin değerleri için optimizasyon işlemi de yapılmıştır.
The experimental studies were performed in two steps within the scope of the thesis. In the first step, the conditions for the production of activated carbon were determined from elaeagnus angustifalia seed and beech tree by using chemical activation method in the presence of nitrogen with ZnCI2, H3PO4, H2SO4, Na2CO3 and KOH activators and by using physical activation method in the presence of CO2 and aqueous vapor. The effects of parameters such as chemical agent/raw material ratio, chemical impregnation time, activation temperature and activation time investigated for the production of activated carbon by chemical activation method. While producing activated carbon by physical activation method, the effects of activation temperature and activation time parameters were investigated. The number of iodine was determined for the activated carbons obtained and the characterization of activated carbons having high iodine numbers was carried out by surface are (BET), FT-IR and SEM instruments. BET surface areas of synthesized activated carbons with high iodine number were determined and surface morphology of ones with large surface area as well as chemically impregrated but non-activated samples and raw materials was performed by SEM analysis. The chemical structures of activated carbons with large surface area, the samples which are impregnated chemically but non-activated, raw materials and activated carbons after adsorption were determined by means of FT-IR. While the activated carbons obtained from elaeagnus angustifalia seeds by activating ZnCI2 and H3PO4 were named as İÇAC and İFAC, respectively, those obtained from beech tree by activating ZnCI2 and H3PO4 were named as KÇAC and KFAC, respectively. The activated carbons which have higher surface areas coded by İÇAC38, İÇAC75, İFAC84, KÇAC85 and KFAC88 were selected and used in the adsorption of coloring agents such as methylene blue and malachite green and heavy metals such as lead (II) and chromium(VI). The effects of parameters such as initial concentration and pH of solution, the amount of adsorbent and the medium temperature were examined for the adsorption of coloring agents and heavy metals. The equilibrium data for adsorption were applied to Langmuir, Freundlich, Temkin and D-R isotherm. It is aimed to investigate the kinetics of adsorption by using pseudo first order and pseudo-second order kinetic models, Elovich and inner particle diffusion models. The thermodynamic parameters of adsorption were determined. The experimental design for the adsorption process of coloring agents and heavy metals was conducted in Design Expert software by using activated carbons coded by İÇAC38, İÇAC75, İFAC84, KÇAC85 and KFAC88. Box-Behnken design model was used as response surface. The effects of the pairwise interactions among parameters such as initial concentration of solution, temperature and time on adsorption capacity were studied in the experimental design of the coloring agents and heavy metals. Box-Behnken response surface methodology was used and the single and pair effects of selected parameters on adsorption capacity were determined in the table of ANOVA. These effects were shown on the graphs in three dimensions. The regression equations were obtained for coloring agents and heavy metals. It was determined that the adsorption capacity results estimated via regresition equations were very close to adsorpsition capacity results which were obtainated experimentally. The parameter optimization process was conducted for the values of selected parameters in Box-Behnken design.
The experimental studies were performed in two steps within the scope of the thesis. In the first step, the conditions for the production of activated carbon were determined from elaeagnus angustifalia seed and beech tree by using chemical activation method in the presence of nitrogen with ZnCI2, H3PO4, H2SO4, Na2CO3 and KOH activators and by using physical activation method in the presence of CO2 and aqueous vapor. The effects of parameters such as chemical agent/raw material ratio, chemical impregnation time, activation temperature and activation time investigated for the production of activated carbon by chemical activation method. While producing activated carbon by physical activation method, the effects of activation temperature and activation time parameters were investigated. The number of iodine was determined for the activated carbons obtained and the characterization of activated carbons having high iodine numbers was carried out by surface are (BET), FT-IR and SEM instruments. BET surface areas of synthesized activated carbons with high iodine number were determined and surface morphology of ones with large surface area as well as chemically impregrated but non-activated samples and raw materials was performed by SEM analysis. The chemical structures of activated carbons with large surface area, the samples which are impregnated chemically but non-activated, raw materials and activated carbons after adsorption were determined by means of FT-IR. While the activated carbons obtained from elaeagnus angustifalia seeds by activating ZnCI2 and H3PO4 were named as İÇAC and İFAC, respectively, those obtained from beech tree by activating ZnCI2 and H3PO4 were named as KÇAC and KFAC, respectively. The activated carbons which have higher surface areas coded by İÇAC38, İÇAC75, İFAC84, KÇAC85 and KFAC88 were selected and used in the adsorption of coloring agents such as methylene blue and malachite green and heavy metals such as lead (II) and chromium(VI). The effects of parameters such as initial concentration and pH of solution, the amount of adsorbent and the medium temperature were examined for the adsorption of coloring agents and heavy metals. The equilibrium data for adsorption were applied to Langmuir, Freundlich, Temkin and D-R isotherm. It is aimed to investigate the kinetics of adsorption by using pseudo first order and pseudo-second order kinetic models, Elovich and inner particle diffusion models. The thermodynamic parameters of adsorption were determined. The experimental design for the adsorption process of coloring agents and heavy metals was conducted in Design Expert software by using activated carbons coded by İÇAC38, İÇAC75, İFAC84, KÇAC85 and KFAC88. Box-Behnken design model was used as response surface. The effects of the pairwise interactions among parameters such as initial concentration of solution, temperature and time on adsorption capacity were studied in the experimental design of the coloring agents and heavy metals. Box-Behnken response surface methodology was used and the single and pair effects of selected parameters on adsorption capacity were determined in the table of ANOVA. These effects were shown on the graphs in three dimensions. The regression equations were obtained for coloring agents and heavy metals. It was determined that the adsorption capacity results estimated via regresition equations were very close to adsorpsition capacity results which were obtainated experimentally. The parameter optimization process was conducted for the values of selected parameters in Box-Behnken design.
Açıklama
Anahtar Kelimeler
Adsorpsiyon, Aktif karbon, Deney tasarımı, İğde çekirdeği, Kayın ağacı, Elaeagnus angustifolia seeds, Beech tree, Activated carbon, Adsorption, Design of experiments
Kaynak
WoS Q Değeri
Scopus Q Değeri
Cilt
Sayı
Künye
Baytar, O. (2015). İğde çekirdeği ve kayın ağacından üretilen aktif karbonun ağır metal ve boyarmadde gideriminde kullanılması. Selçuk Üniversitesi, Yayımlanmış doktora tezi, Konya.