某伊利石矿合成丝光沸石分子筛的实验研究
发布时间：2019-03-29 17:14
【摘要】：本文以伊利石粘土矿的工艺矿物学研究为基础,其含铁钛等染色杂质过多,久置后颜色发黄,影响其应用价值,探索各种方法进行除铁试验研究,最终发现整体除铁效果有限。以该伊利石粘土矿为天然矿物原料,经过煅烧,成功活化成了无定形物质,以活化熟料合成丝光沸石分子筛,并对比了以除铁原料和为除铁原料制成的丝光沸石分子筛的催化性能。(1)伊利石粘土矿主要成分为石英SiO2和氧化铝Al2O3。含金属矿物较多,黄铁矿、磁铁矿、褐铁矿、黄钾铁矾、金红石、锆英石,其中金属矿物主要为黄铁矿为主。由于金属矿物杂质铁的存在,伊利石粘土矿久置后会出现白度降低,颜色发黄的现象,要直接利用,需考虑先将铁矿物杂质除去。而其中的染色杂质黄铁矿及黄钾铁矾堪布粒度过细,将严重影响除铁的效果。(2)伊利石粘土矿(半软质)Al2O3含量为12.11%,SiO2含量为71.51%,其n(SiO2)/n(Al2O3)=9.84,符合以天然矿物制备丝光沸石分子筛的硅铝比要求。差热分析和XRD分析结果与伊利石粘土矿标准图谱对比,发现其并不属于典型的高含量伊利石粘土矿,在合成丝光沸石分子筛的试验研究中,可将其视为钾长石KAl3SiO8。(3)对伊利石粘土矿进行除铁试验,包括浮选试验、高梯度磁选试验、超导磁选试验。研究发现,在浮选前磨矿阶段加入水玻璃0.3g有助于浮选除Fe,Fe含量最低达到0.38%,而对活化剂和捕收剂用量的考察发现其对除铁效果影响不显著;浮选-磁选联合除铁试验效果不佳;单独高梯度磁选的效果不佳;使用超导磁选除铁的效果整体来说较浮选及高梯度磁选的效果好很多,但是仍然无法达到预期中除去大部分铁杂质的效果。(4)对伊利石原矿进行煅烧活化试验。通过对煅烧温度、煅烧保温时间、煅烧时原矿与纯碱质量比、煅烧时的入料细度进行考察。结果发现在煅烧温度650℃,保温90min,原矿与纯碱质量比为1:1,煅烧前磨矿15min的最佳条件下,伊利石在煅烧过程中被破坏了原有的结构,羟基失去水而导致重排晶格,得到可溶性硅铝酸钠粉末。(5)采用煅烧活化熟料进行水热反应制备丝光沸石分子筛,通过考察硅碱比、水碱比、晶化时间,以XRD图谱表征作为评价标准。发现在6Na2O:Al2O3:10SiO2:150H2O,晶化温度170度,晶化时间24h时获得的产物XRD图谱与参考值非常相近,峰值尖锐且相对峰强与参考值相符,可认为获得了质量较好的丝光沸石产品。(6)以前述超导磁选产物(除铁后Fe含量0.37%)以最佳条件制备丝光沸石分子筛,并与未除铁伊利石制备的丝光沸石一同进行甲苯催化反应,对产物分析可知,以伊利石为天然矿物原料制备的丝光沸石产品催化效率远高于FeCl3,且经过除铁后的伊利石制备的丝光沸石催化效果好于未除铁伊利石制备的丝光沸石。
[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，
本文编号：2449726
[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，
本文编号：2449726
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