超(亞)臨界水熱活化聯(lián)合鹽酸酸浸提取煤矸石中硅、鋁的研究
發(fā)布時(shí)間:2018-04-04 02:05
本文選題:煤矸石 切入點(diǎn):超(亞)臨界水熱活化 出處:《太原理工大學(xué)》2017年碩士論文
【摘要】:近年來,超臨界流體技術(shù),廣泛應(yīng)用于萃取分離、化學(xué)反應(yīng)工程、環(huán)境保護(hù)、材料科學(xué)等方面,有很好的發(fā)展前景。煤矸石是采煤過程和洗煤過程中排放的固體廢物。本文以煤矸石制備白炭黑和氧化鋁技術(shù)開發(fā)為背景,將超臨界流體技術(shù)用于固體廢物的處理。論文重點(diǎn)研究超(亞)臨界水中煤矸石活化的反應(yīng)特性,考察超(亞)臨界水熱活化的反應(yīng)條件對(duì)硅、鋁溶出率的影響。實(shí)驗(yàn)結(jié)果表明,與傳統(tǒng)的煤矸石活化方法相比,超(亞)臨界水活化技術(shù)具有反應(yīng)溫度低、化學(xué)反應(yīng)介質(zhì)廉價(jià)和綠色環(huán)保的優(yōu)勢(shì);诖,本文提出了以煤矸石為原料,超(亞)臨界水熱活化聯(lián)合鹽酸浸提取煤矸石中的硅鋁用于制備白炭黑和氧化鋁的新工藝。選取五種煤矸石作為實(shí)驗(yàn)原料。首先,通過超臨界水熱活化實(shí)驗(yàn),采用添加無機(jī)堿作為活化劑,對(duì)產(chǎn)物進(jìn)行一系列的分析,獲取SiO_2和Al_2O_3提取率的數(shù)據(jù)。初步建立實(shí)驗(yàn)方案、分析手段及計(jì)算方法。其次,對(duì)堿在煤矸石活化中的影響作了簡要分析。通過XRD、ICP-OES等表征手段,發(fā)現(xiàn)當(dāng)添加NaOH、Na2CO3和KOH時(shí),對(duì)應(yīng)的活化樣品中主要的物相分布為鈣霞石、方鈉石和鉀霞石,并且這些硅鋁酸鹽是能夠溶于稀酸。所有的活化樣品都采用鹽酸酸浸用以獲取SiO_2和Al_2O_3。當(dāng)2.0 mol/L NaOH為活化劑時(shí),SiO_2和Al_2O_3的溶出率分別為70.41%和65.74%;當(dāng)2.0 mol/L Na2CO3為活化劑時(shí),SiO_2和Al_2O_3的溶出率分別為77.03%和71.57%;當(dāng)2.0 mol/L KOH為活化劑時(shí),SiO_2和Al_2O_3的溶出率分別為71.46%和83.04%。為了拓寬活化實(shí)驗(yàn)的溫度范圍,考察了煤矸石的亞臨界水熱活化效果,同時(shí)探索提高分離出來的白炭黑和氧化鋁的收率。借助XRD、ICP-OES、TG-DTG、FTIR、BET等測(cè)試方法,分析出二氧化硅的溶出率在50%以上,氧化鋁的溶出率在80%以上。通過分離提純可以制得比表面積最高可達(dá)818.1m2/g,純度達(dá)到了96.3%的白炭黑產(chǎn)品和純度達(dá)到99.17%的氧化鋁產(chǎn)品。最后,在煤矸石為原料超(亞)臨界水熱法制備白炭黑和氧化鋁工藝的基礎(chǔ)上,經(jīng)過簡單的物料衡算和經(jīng)濟(jì)效益分析以及環(huán)境評(píng)價(jià),證明它是一種產(chǎn)品附加值高,資源利用率高且環(huán)境友好的優(yōu)良工藝。
[Abstract]:In recent years, supercritical fluid technology has been widely used in extraction separation, chemical reaction engineering, environmental protection, material science and so on.Coal gangue is the solid waste discharged during coal mining and coal washing.In this paper, supercritical fluid technology is applied to solid waste treatment under the background of technology development of coal gangue preparation of silica and alumina.In this paper, the reaction characteristics of coal gangue activation in supercritical water were studied, and the effect of reaction conditions on the dissolution rate of Si and Al was investigated.The experimental results show that the supercritical water activation technology has the advantages of low reaction temperature, cheap chemical reaction medium and green environmental protection compared with the traditional coal gangue activation method.Based on this, a new process for the preparation of silica and alumina from coal gangue by supercritical hydrothermal activation combined with hydrochloric acid leaching was proposed.Five kinds of coal gangue were selected as experimental raw materials.Firstly, through supercritical hydrothermal activation experiment, adding inorganic base as activator, a series of analysis was carried out on the product, and the data of SiO_2 and Al_2O_3 extraction rate were obtained.The experimental scheme, the analysis method and the calculation method are preliminarily established.Secondly, the effect of alkali on the activation of coal gangue is briefly analyzed.By means of XRDX ICP-OES, it was found that the main phases of the activated samples were calcium nepheline, calcinite and potassium nepheline when NaOHN Na 2CO 3 and KOH were added, and these aluminates were soluble in dilute acid.All activated samples were soaked with hydrochloric acid to obtain SiO_2 and Al _ 2O _ 3.褰,
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