本文選題：氫還原 + 流化床��； 參考：《內(nèi)蒙古大學(xué)》2017年碩士論文

【摘要】：硫化鈉作為一種強(qiáng)還原性、強(qiáng)堿性的無(wú)機(jī)化合物,在很多領(lǐng)域具有重要應(yīng)用。目前,我國(guó)的硫化鈉工業(yè)品大多采用煤粉還原法制備,環(huán)境負(fù)荷大且產(chǎn)物雜質(zhì)含量高,限制了硫化鈉高附加值產(chǎn)品的進(jìn)一步開(kāi)發(fā)利用。特別是硫化鈉作為近年興起的新型樹(shù)脂聚苯硫醚的生產(chǎn)原料,對(duì)其純度品相要求很高。因此,開(kāi)發(fā)新工藝制備高純硫化鈉具有重要意義。氣體一步法還原工業(yè)硫酸鈉制硫化鈉的研究已經(jīng)取得了很大進(jìn)展,其工藝簡(jiǎn)單,硫化鈉產(chǎn)物純度高。本實(shí)驗(yàn)室對(duì)該工藝過(guò)程及催化劑進(jìn)行了多年探索,但固相產(chǎn)物的純化及催化劑的分離仍是十分棘手的問(wèn)題。本論文首先用固相法制備了兩種不同的a-Fe203催化劑,研究其流化床中催化氫氣還原元明粉制高純硫化鈉粗產(chǎn)物反應(yīng)的催化性能,并提取粗產(chǎn)物中的催化劑進(jìn)行循環(huán)使用及催化機(jī)理初步探索。其次,分別以水和無(wú)水乙醇為溶劑對(duì)硫化鈉粗產(chǎn)物進(jìn)行純化實(shí)驗(yàn)探究,尋求高效的純化實(shí)驗(yàn)方案。最后,對(duì)乙醇提純法純化硫化鈉粗產(chǎn)物的實(shí)驗(yàn)條件進(jìn)行正交實(shí)驗(yàn)設(shè)計(jì)及優(yōu)化,得出最佳的純化實(shí)驗(yàn)條件。結(jié)果表明,反應(yīng)的催化機(jī)理可能為鐵氧化物混合相的共同催化作用,G-900-1型α-Fe203催化劑的催化性能最好,制得的硫化鈉粗產(chǎn)物中Na2S含量可高達(dá)95.2%。以無(wú)水乙醇為溶劑對(duì)硫化鈉粗產(chǎn)物進(jìn)行減壓旋蒸提純的效果遠(yuǎn)遠(yuǎn)優(yōu)于以水為溶劑的提純效果。對(duì)乙醇提純法進(jìn)行正交試驗(yàn)優(yōu)化,得到了最佳的實(shí)驗(yàn)條件,在此條件下獲得的純化產(chǎn)物為純相的Na2S·5H20,含量可達(dá)98.3%,雜質(zhì)Na2S03和Na2S203含量之和為1.4%,Fe含量0.0023%,均滿足國(guó)家標(biāo)準(zhǔn)要求。本工作基本解決了固相產(chǎn)物中催化劑的分離問(wèn)題,產(chǎn)品滿足生產(chǎn)聚苯硫醚所需高純硫化鈉原料的要求。
[Abstract]:Sodium sulphide, as an inorganic compound with strong reducibility and alkalinity, has important applications in many fields.At present, most of the industrial products of sodium sulfide in China are prepared by pulverized coal reduction method. The heavy environmental load and high impurity content limit the further development and utilization of high added value sodium sulfide products.Especially, sodium sulfide, as the raw material for the production of new resin polyphenylene sulfide (PPS) in recent years, requires high purity.Therefore, it is of great significance to develop a new process for the preparation of high purity sodium sulfide.Great progress has been made in the reduction of industrial sodium sulfate to sodium sulfide by one step gas reduction. The process is simple and the purity of sodium sulfide product is high.The process and catalyst have been explored in our laboratory for many years, but the purification of solid products and the separation of catalyst are still very difficult problems.In this paper, two kinds of a-Fe203 catalysts were prepared by solid phase method, and the catalytic performance of the catalyst in fluidized bed to produce high purity sodium sulphide was studied.The catalyst was extracted from the crude product for recycling and the mechanism of the catalyst was preliminarily explored.Secondly, the crude product of sodium sulfide was purified with water and anhydrous ethanol, respectively.Finally, the orthogonal design and optimization of the experimental conditions for the purification of crude sodium sulfide by ethanol purification method were carried out, and the optimum purification conditions were obtained.The results showed that the catalytic mechanism of the reaction was probably due to the co-catalysis of iron oxide mixed phase. The catalytic activity of G-900-1 偽 -Fe203 catalyst was the best, and the Na2S content in the crude product of sodium sulphide could be up to 95.2%.The purification of crude product of sodium sulfide with anhydrous ethanol as solvent is much better than that with water as solvent.The orthogonal experiment was carried out to optimize the ethanol purification method, and the optimum experimental conditions were obtained. Under this condition, the purified product was pure phase Na2S 5H20, the content of the purified product was 98.3 and the sum of the impurity Na2S03 and Na2S203 content was 1.4g Fe 0.0023, which met the requirements of the national standard.This work basically solves the problem of catalyst separation in solid product, and the product meets the requirement of high purity sodium sulfide raw material for the production of polyphenylene sulfide.
【學(xué)位授予單位】：內(nèi)蒙古大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類(lèi)號(hào)】：TQ131.12

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本文編號(hào)：1750316