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高純氫氧化鎂的合成

發(fā)布時(shí)間:2018-03-20 03:13

  本文選題:輕燒粉 切入點(diǎn):酸浸 出處:《沈陽(yáng)工業(yè)大學(xué)》2015年碩士論文 論文類型:學(xué)位論文


【摘要】:氫氧化鎂是現(xiàn)代工業(yè)中十分重要的化工原料和添加劑,它具有阻燃、抑煙、填充等功能,并且無(wú)毒、無(wú)害、無(wú)腐蝕性,極具發(fā)展?jié)摿,具有較高的經(jīng)濟(jì)和社會(huì)價(jià)值,近年來(lái)成為研究熱點(diǎn)。本文針對(duì)遼寧省豐富的輕燒粉資源現(xiàn)狀,氫氧化鎂的市場(chǎng)潛力,及生產(chǎn)中存在的主要問(wèn)題,以輕燒粉為原料,酸浸除雜后得精制硫酸鎂溶液,與氨水反應(yīng)合成氫氧化鎂,再經(jīng)水熱改性,最終得到高純氫氧化鎂。 通過(guò)實(shí)驗(yàn)得到了輕燒粉酸浸的最佳條件:在常壓下,硫酸濃度(質(zhì)量濃度)10.0%,硫酸與硫酸銨比7:3,復(fù)配酸鎂比1.4:1,反應(yīng)溫度75℃,反應(yīng)時(shí)間40min,攪拌強(qiáng)度450r·min-1,浸取率可達(dá)96.29%。通過(guò)X射線衍射(XRD)檢測(cè),煅燒后的樣品為硫酸鎂。 依據(jù)不同金屬離子水解時(shí)pH值的差別,在提純粗硫酸鎂溶液時(shí),,用氨水嚴(yán)格控制pH值為6,60℃恒溫水浴,除去鐵、鋁等雜質(zhì),再調(diào)節(jié)pH值為8.5左右,加熱至沸過(guò)濾,精制后的硫酸鎂溶液經(jīng)蒸發(fā)、結(jié)晶、煅燒后,純度達(dá)到99.93%以上。 通過(guò)實(shí)驗(yàn)研究了精制硫酸鎂溶液濃度、反應(yīng)溫度、氨水用量、攪拌速度對(duì)氫氧化鎂收率的影響,確定了合成氫氧化鎂的最佳實(shí)驗(yàn)條件:硫酸鎂濃度為1.5mol·L-1,反應(yīng)溫度50℃,反應(yīng)時(shí)間為50min,氨鎂比為3:1,轉(zhuǎn)數(shù)為450r·min-1。所得產(chǎn)品為卡房狀氫氧化鎂聚集體,表觀平均粒徑為24.55μm,純度達(dá)99.9%以上,收率為90.16%。研究了陰離子型、陽(yáng)離子型、非離子型和復(fù)配型多種類型添加劑對(duì)氫氧化鎂的影響,均沒(méi)有改變氫氧化鎂的晶形和形貌,但是會(huì)引起晶體的極性和結(jié)晶度的變化,可能是因?yàn)榱蛩徭V中的反離子起了主要作用。 通過(guò)實(shí)驗(yàn)研究了水熱改性對(duì)最佳條件下合成的氫氧化鎂晶形和形貌的影響,確定了氫氧化鎂水熱改性的最佳條件:水熱時(shí)間為12h,水熱溫度為220℃,氫氧化鈉濃度6.0mol·L-1。所得樣品極性小,形貌規(guī)則,分散性良好,結(jié)晶度高,熱穩(wěn)定性好,表觀平均粒徑為2.16μm,純度達(dá)99.94%以上,收率為88.13%。
[Abstract]:Magnesium hydroxide is very important in modern industry, chemical raw materials and additives, it has flame retardant and smoke suppression, filling and other functions, and is non-toxic, harmless, non corrosive, has great potential for development, with high economic and social value, in recent years become the focus of research. Based on Liaoning province abundant light burning powder resources 2 market potential, and the existing problems in the production, with the light burning powder as raw material, acid leaching solution was prepared after Magnesium Sulfate, and synthesis of magnesium hydroxide by reaction of ammonia, hydrothermal modification, finally obtained the Gao Chunqing Magnesium Oxide.
The optimum conditions of the light burning powder obtained by acid leaching experiment: under normal pressure, concentration of sulfuric acid (concentration 10%), sulfuric acid and ammonium sulfate than 7:3, mixed acid magnesium ratio 1.4:1, reaction temperature 75 C, reaction time 40min, stirring intensity of 450R - min-1, the leaching rate can reach 96.29%. by X ray diffraction (XRD) detection, calcined samples for Magnesium Sulfate.
On the basis of the hydrolysis of different metal ions when the pH value of the difference in the purification of crude Magnesium Sulfate with ammonia solution, strictly control the pH value of the 6,60 constant temperature water bath, the removal of iron, aluminum and other impurities, and then adjust the pH value is about 8.5, heated to boiling filtered, Magnesium Sulfate solution after purification by evaporation, crystallization and calcination. The purity of more than 99.93%.
Through the experimental study on the purification of Magnesium Sulfate solution concentration, reaction temperature, ammonia dosage, stirring speed on the yield of magnesium hydroxide, the optimum experimental conditions for synthesis of magnesium hydroxide: Magnesium Sulfate was 1.5mol - L-1, the reaction temperature is 50 DEG C, the reaction time is 50min, ammonia and magnesium ratio is 3:1, the speed was 450R the product is min-1. card the magnesium hydroxide aggregates, the apparent average particle size of 24.55 m, reached a purity of more than 99.9%, the yield of anionic 90.16%., cationic, nonionic and compound effects of various types of additives on the magnesium hydroxide, did not change the crystal shape and morphology of magnesium hydroxide, but will cause changes in polarity and crystal the degree, probably because the counter ion of Magnesium Sulfate has played a major role.
Through the experimental study on the effect of hydrothermal modification of magnesium hydroxide crystal and morphology of synthesized under the optimum conditions, the optimum conditions of magnesium hydroxide hydrothermal modification of hydrothermal time 12h, hydrothermal temperature is 220 DEG C, the concentration of sodium hydroxide 6.0mol L-1. samples from polar small, regular shape, good dispersion, crystallization high degree of thermal stability, apparent average particle size of 2.16 m, reached a purity of more than 99.94%, the yield was 88.13%.

【學(xué)位授予單位】:沈陽(yáng)工業(yè)大學(xué)
【學(xué)位級(jí)別】:碩士
【學(xué)位授予年份】:2015
【分類號(hào)】:TQ132.2

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