بررسی پارامترهای موثر بر سنتز گوتیت به روش اکسیداسیون محلول در مقیاس آزمایشگاهی

نوع مقاله : پژوهشی اصیل

نویسندگان

1 مجتمع دانشگاهی شیمی و مهندسی شیمی، دانشگاه صنعتی مالک اشتر، تهران، ایران

2 مجتمع دانشگاهی شیمی و مهندسی شیمی

3 • مجتمع دانشگاهی شیمی و مهندسی شیمی، دانشگاه صنعتی مالک اشتر، تهران، ایران

چکیده
نانو ذرات گوتیت خالص با موفقیت با روش اکسیداسیون محلول و با استفاده از پیش­ماده­های سولفات ­آهن(II) هفت­آبه(FeSO4.7H2O) و هیدروکسیدسدیم(NaOH) سنتز شد. در این پژوهش با طراحی آزمایش توسط نرم افزارMinitab ، با استفاده از روش فاکتوریل کامل، در دمای oC۴۰، تغییرات دو پارامتر، دبی هوای دمیده شده در محلول واکنش(Q) و نسبت درصد جرمی مواد اولیه(R) (درصد جرمی سولفات ­آهن(II) به درصد جرمی هیدروکسیدسدیم)، در دو سطح (Lit/min۳/۱۳و۲Q=) و (۳و۱R=)، مورد بررسی قرار گرفتند. تحلیل کیفی نتایج آزمایشات، توسط پراش اشعه ایکس(XRD سنتز فاز گوتیت (α-FeOOH) اکسی­هیدروکسیدآهن را مورد تایید قرار داد و نتایج طیف­سنجی پراکندگی انرژی پرتو ایکس(EDX)، نشان داد که گوتیت سنتز شده دارای درصد خلوص نقطه­ای بالای (٪۸/۹۹) می­باشد. نتایج میکروسکوپ الکترونی روبشی(FESEM) برای گوتیت، ساختار بلوری میله­ای شکل، با متوسط اندازه­ی مجموعه ­ذراتی بین ​​(nm۴۳-۲۳)، بسته به میزان R و Q را گزارش داد و با تحلیل نتایج پتانسیل اکسایش-کاهش (ORP)، مشاهده شد که زمان پایان واکنش تشکیل گوتیت بین s۶۳۵ الی s۲۲۱۰ می­باشد. تحلیل آماری نتایج، توسط نرم افزار Minitab، سبب بدست آمدن روابط همبستگی[1] ،بین دو پارامتر (Q و R) دو پاسخ (زمان پایان واکنش(t) و متوسط اندازه­ی مجموعه­ ذرات(d)) در دمای محلول واکنشoC۴۰، برای گوتیت گردید. با توجه به این روابط مشاهده شد در دمای محلول واکنش oC۴۰، با افزایش دبی هوا(Q) و کاهش نسبت درصد جرمی مواد اولیه(R)، زمان پایان واکنش و متوسط اندازه­ی مجموعه ­ذرات گوتیت، به طور کلی کاهش می­یابند و بالعکس. همچنین درصد تغییرات(R)، تاثیرات بیشتری نسبت به تغییرات (Q)، بر متوسط اندازه­ی مجموعه ­ذرات و زمان پایان واکنش، دارد.


[1] Correlation

کلیدواژه‌ها

موضوعات


عنوان مقاله English

Investigation of effective parameters on synthesis of Goethite with solution oxidation method in the laboratory scale

نویسندگان English

Meghdad Azimi 1
Saeed Tavangar 2
Seyed Ghorban Hosseini 3
Muhammad Eghdamtalab 3
1 1 Faculty of Chemistry and Chemical Engineering, Malek Ashtar University of Technology, Tehran, Iran
2 Faculty of Chemistry and Chemical Engineering, Malek Ashtar University of Technology, Tehran, Iran
3 Faculty of Chemistry and Chemical Engineering, Malek Ashtar University of Technology, Tehran, Iran
چکیده English

Abstract

Research subject: The pure Goethite nanoparticles were synthesized successfully with solution oxidation method and by using raw materials Iron (II) sulfate heptahydrate (FeSO4.7H2O) and sodium hydroxide (NaOH).

Research approach: In this study, the simulation of experiment was implemented by Minitab software, with complete factorial method, at 40°C, the variation of two parameters including the flow rate of entered gas in the solution reaction (Q) and mass percent ratio of raw materials (R) (mass percent of iron (II) sulphate to mass percent of sodium hydroxide), in two levels (Q=2 and 13.3 Lit/min) and (R=1 and 3) were evaluated. The qualitative analysis of results was performed by X-ray diffraction (XRD), synthesis of Goethite phase (α-FeOOH) confirmed Iron oxyhydroxide and the Energy-dispersive X-ray spectroscopy (EDX), illustrated that the synthesized Goethite has high purity percentage (≥99.8%). The field emission scanning electron microscopy (FESEM) for Goethite reported a bar-shaped crystal structure, with an average particle Cluster size between (23-43nm), based on R and Q and by analyzing the oxidation-reduction potential(ORP) results, it was seen that the reaction time of Goethite formation is between 635-2210s.

Main results: The statistical analysis of results with Minitab software can create Correlation relations for Goethite, between two parameters(Q and R) and two response (reaction time(t) and average particle Cluster size(d)) at the temperature of reaction solution 40°C. regarding the relations, it was seen that at the temperature of reaction solution 40°C, with an increase in air flow rate(Q) and decrease of the mass percent ratio of raw materials(R), the reaction time and average particles Cluster size of Goethite decrease generally and vice versatile. Also, the percentage change (R) has a higher impact on average particles Cluster size and reaction time than changes (Q).

کلیدواژه‌ها English

Goethite
Solution oxidation method
Oxidation-Reduction Potential (ORP)
Reaction time
Correlation relations
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