發(fā)布時(shí)間：2019-03-29 17:14

【摘要】：本文以伊利石粘土礦的工藝礦物學(xué)研究為基礎(chǔ),其含鐵鈦等染色雜質(zhì)過多,久置后顏色發(fā)黃,影響其應(yīng)用價(jià)值,探索各種方法進(jìn)行除鐵試驗(yàn)研究,最終發(fā)現(xiàn)整體除鐵效果有限。以該伊利石粘土礦為天然礦物原料,經(jīng)過煅燒,成功活化成了無(wú)定形物質(zhì),以活化熟料合成絲光沸石分子篩,并對(duì)比了以除鐵原料和為除鐵原料制成的絲光沸石分子篩的催化性能。(1)伊利石粘土礦主要成分為石英SiO2和氧化鋁Al2O3。含金屬礦物較多,黃鐵礦、磁鐵礦、褐鐵礦、黃鉀鐵礬、金紅石、鋯英石,其中金屬礦物主要為黃鐵礦為主。由于金屬礦物雜質(zhì)鐵的存在,伊利石粘土礦久置后會(huì)出現(xiàn)白度降低,顏色發(fā)黃的現(xiàn)象,要直接利用,需考慮先將鐵礦物雜質(zhì)除去。而其中的染色雜質(zhì)黃鐵礦及黃鉀鐵礬堪布粒度過細(xì),將嚴(yán)重影響除鐵的效果。(2)伊利石粘土礦(半軟質(zhì))Al2O3含量為12.11%,SiO2含量為71.51%,其n(SiO2)/n(Al2O3)=9.84,符合以天然礦物制備絲光沸石分子篩的硅鋁比要求。差熱分析和XRD分析結(jié)果與伊利石粘土礦標(biāo)準(zhǔn)圖譜對(duì)比,發(fā)現(xiàn)其并不屬于典型的高含量伊利石粘土礦,在合成絲光沸石分子篩的試驗(yàn)研究中,可將其視為鉀長(zhǎng)石KAl3SiO8。(3)對(duì)伊利石粘土礦進(jìn)行除鐵試驗(yàn),包括浮選試驗(yàn)、高梯度磁選試驗(yàn)、超導(dǎo)磁選試驗(yàn)。研究發(fā)現(xiàn),在浮選前磨礦階段加入水玻璃0.3g有助于浮選除Fe,Fe含量最低達(dá)到0.38%,而對(duì)活化劑和捕收劑用量的考察發(fā)現(xiàn)其對(duì)除鐵效果影響不顯著;浮選-磁選聯(lián)合除鐵試驗(yàn)效果不佳;單獨(dú)高梯度磁選的效果不佳;使用超導(dǎo)磁選除鐵的效果整體來(lái)說(shuō)較浮選及高梯度磁選的效果好很多,但是仍然無(wú)法達(dá)到預(yù)期中除去大部分鐵雜質(zhì)的效果。(4)對(duì)伊利石原礦進(jìn)行煅燒活化試驗(yàn)。通過對(duì)煅燒溫度、煅燒保溫時(shí)間、煅燒時(shí)原礦與純堿質(zhì)量比、煅燒時(shí)的入料細(xì)度進(jìn)行考察。結(jié)果發(fā)現(xiàn)在煅燒溫度650℃,保溫90min,原礦與純堿質(zhì)量比為1:1,煅燒前磨礦15min的最佳條件下,伊利石在煅燒過程中被破壞了原有的結(jié)構(gòu),羥基失去水而導(dǎo)致重排晶格,得到可溶性硅鋁酸鈉粉末。(5)采用煅燒活化熟料進(jìn)行水熱反應(yīng)制備絲光沸石分子篩,通過考察硅堿比、水堿比、晶化時(shí)間,以XRD圖譜表征作為評(píng)價(jià)標(biāo)準(zhǔn)。發(fā)現(xiàn)在6Na2O:Al2O3:10SiO2:150H2O,晶化溫度170度,晶化時(shí)間24h時(shí)獲得的產(chǎn)物XRD圖譜與參考值非常相近,峰值尖銳且相對(duì)峰強(qiáng)與參考值相符,可認(rèn)為獲得了質(zhì)量較好的絲光沸石產(chǎn)品。(6)以前述超導(dǎo)磁選產(chǎn)物(除鐵后Fe含量0.37%)以最佳條件制備絲光沸石分子篩,并與未除鐵伊利石制備的絲光沸石一同進(jìn)行甲苯催化反應(yīng),對(duì)產(chǎn)物分析可知,以伊利石為天然礦物原料制備的絲光沸石產(chǎn)品催化效率遠(yuǎn)高于FeCl3,且經(jīng)過除鐵后的伊利石制備的絲光沸石催化效果好于未除鐵伊利石制備的絲光沸石。
[Abstract]:Based on the study of process mineralogy of Illite clay ore, there are too many dyeing impurities, such as iron and titanium, and the color is yellowed for a long time, which affects the application value of Illite clay ore. Various methods are explored to carry on the iron removal experiment research, and it is found that the overall iron removal effect is limited. Using the Illite clay ore as the natural mineral raw material, the amorphous material was successfully activated by calcining, and the mordenite molecular sieve was synthesized by activating the clinker. The catalytic properties of mordenite molecular sieves from iron removal and iron removal were compared. (1) Illite clay is mainly composed of quartz SiO2 and alumina Al2O3.. There are many metallic minerals, such as pyrite, magnetite, limonite, pyrite, rutile and zircon, among which the main metal minerals are pyrite. Due to the existence of metal mineral impurity iron, the whiteness of Illite clay ore will decrease and the color will turn yellow after long-term placement. In order to use it directly, the impurity of iron mineral should be removed first. But the dyeing impurity pyrite and pyrite alum are too fine, which will seriously affect the effect of iron removal. (2) Illite clay (semi-soft) Al2O3 content is 12.11%, Sio _ 2 content is 71.51%, and the iron removal effect of Illite clay ore (semi-soft) is 12.11%, and Sio _ 2 content is 71.51%. Its n (SiO2) / n (Al2O3) = 9.84, which meets the requirements of Si-Al ratio for the preparation of mordenite molecular sieves from natural minerals. The results of differential thermal analysis and XRD analysis were compared with the standard maps of Illite clay ore. It was found that it was not a typical Illite clay ore with high content. In the experimental study on the synthesis of mordenite molecular sieve, it was found that Illite clay ore was not a typical Illite clay ore. It can be regarded as potassium feldspar KAl3SiO8. (3) to remove iron from Illite clay ore, including flotation test, high gradient magnetic separation test and superconducting magnetic separation test. It was found that adding 0.3g of water glass in the flotation pre-grinding stage could reduce the Fe,Fe content of flotation to 0.38%, while the amount of activator and collector had no significant effect on iron removal. Flotation-magnetic separation combined iron removal test is not good, high gradient magnetic separation alone is not good; The effect of iron removal by superconducting magnetic separation is much better than that of flotation and high gradient magnetic separation, but it is still unable to achieve the expected effect of removing most iron impurities. (4) calcining activation test of Illite ore is carried out. The calcination temperature, calcination holding time, the mass ratio of raw ore to soda, and the fineness of raw material during calcination were investigated. The results show that under the optimum conditions of calcining temperature 650 鈩，

本文編號(hào)：2449726