四氯化硅氫化制備三氯氫硅生產(chǎn)工藝研究
發(fā)布時間：2018-09-10 13:36
【摘要】：近年來,位于光伏上游的多晶硅產(chǎn)業(yè),因產(chǎn)能過剩遭遇寒潮,國內(nèi)多晶硅產(chǎn)業(yè)受到嚴(yán)重的沖擊,除了國外多晶硅生產(chǎn)巨頭沖擊國內(nèi)市場的因素外,其根本原因還是自身核心技術(shù)不夠成熟,導(dǎo)致生產(chǎn)成本過高。降低產(chǎn)業(yè)能耗,實現(xiàn)副產(chǎn)物循環(huán)利用,成了國內(nèi)多晶硅行業(yè)健康持續(xù)發(fā)展的關(guān)鍵。改良西門子法是生產(chǎn)多晶硅的主流工藝,每生產(chǎn)1 t多晶硅副產(chǎn)約15 t四氯化硅,如何處理數(shù)量龐大的四氯化硅,成為制約多晶硅行業(yè)發(fā)展的巨大瓶頸。利用四氯化硅氫化技術(shù)制備三氯氫硅,實現(xiàn)物料的閉路循環(huán),大幅降低生產(chǎn)成本,開始得到越來越多業(yè)內(nèi)人士的關(guān)注。現(xiàn)有的高溫氫化工藝和冷氫化工藝中的高能耗和反應(yīng)轉(zhuǎn)化率低的問題亟待解決。怎么提高四氯化硅轉(zhuǎn)化率,節(jié)能降耗成了氫化技術(shù)的研究熱點。針對該問題,本文對四氯化硅DBD等離子體氫化工藝進(jìn)行了探索,并將鎳基催化劑用于高溫氫化反應(yīng)進(jìn)行實驗研究。主要的研究工作內(nèi)容和結(jié)果如下:(1)提出了DBD等離子體放電用于四氯化硅的氫化反應(yīng),并設(shè)計等離子體發(fā)生器和石英套管反應(yīng)器,搭建專業(yè)實驗平臺,對DBD等離子體放電條件和四氯化硅氫化反應(yīng)進(jìn)行小試試驗探索。在DBD低溫等離子體中,四氯化硅發(fā)生氫化反應(yīng)生成三氯氫硅,而且在試驗功率范圍內(nèi),隨著等離子體電源功率的增大,三氯氫硅收率增大,實驗條件下得到三氯氫硅的最大收率為12.1%。(2)DBD等離子體氫化過程中反應(yīng)進(jìn)度不易控制,四氯化硅等離子體還原沒有停留在生成三氯氫硅這一步,而是繼續(xù)還原生成了單質(zhì)硅。高溫四氯化硅氣體夾帶著不定型硅粉,形成導(dǎo)電性的煙霧,改變了原有的放電結(jié)構(gòu),放電間距大大變小,放電均勻性不好控制。(3)采用浸漬法制備不同的負(fù)載鎳催化劑,對比了四種催化劑對四氯化硅氫化反應(yīng)的催化效果,結(jié)果表明,Ni/HZSM-5催化性能最佳。最佳反應(yīng)條件為:鎳負(fù)載量為10%,反應(yīng)溫度850℃,反應(yīng)壓力0.3 MPa,進(jìn)料比H_2:SiCl_4為4,空速為5000 h~(-1),在最佳反應(yīng)條件下,四氯化硅的轉(zhuǎn)化率可以達(dá)到16.69%。
[Abstract]:In recent years, the polycrystalline silicon industry located in the upper reaches of photovoltaic has suffered a severe shock due to the cold wave of overcapacity. In addition to the factors that the foreign polysilicon production giants have impacted the domestic market, The fundamental reason is that its core technology is not mature enough, leading to high production costs. Reducing industry energy consumption and realizing recycling of by-products have become the key to the healthy and sustainable development of domestic polysilicon industry. The modified Siemens method is the mainstream process for the production of polysilicon. How to deal with the large quantity of silicon tetrachloride for every 1 ton polysilicon by-product about 15 tons of silicon tetrachloride has become a huge bottleneck restricting the development of polycrystalline silicon industry. The production of trichlorosilicon by hydrogenation of hydrochlorinated tetrachloride can realize the closed-circuit circulation of the material and reduce the production cost greatly. It has been paid more and more attention to by the industry. The problems of high energy consumption and low reaction conversion in the existing high temperature hydrogenation process and cold hydrogenation process need to be solved. How to improve the conversion rate of silicon tetrachloride and save energy and reduce consumption has become the research hotspot of hydrogenation technology. In order to solve this problem, the plasma hydrogenation process of silicon tetrachloride (DBD) was investigated, and the nickel-based catalyst was used in the hydrogenation at high temperature. The main contents and results are as follows: (1) DBD plasma discharge is proposed for hydrogenation of silicon tetrachloride, and plasma generator and quartz casing reactor are designed to build a professional experimental platform. The discharge conditions of DBD plasma and the hydrogenation of silicon tetrachloride were investigated. In DBD low temperature plasma, silicon tetrachloride is hydrogenated to produce trichlorosilicon. In the range of test power, the yield of trichlorosilicon increases with the increase of plasma power. Under the experimental conditions, the maximum yield of trichlorosilicon is 12.1. (2) the reaction progress is not easy to control during the hydrogenation of DBD plasma. The plasma reduction of silicon tetrachloride does not stop at the step of producing trichlorosilicon, but continues to reduce to form elemental silicon. High temperature silicon tetrachloride gas entrainment of amorphous silica fume to form conductive smoke, changed the original discharge structure, discharge spacing greatly smaller, discharge uniformity is not easy to control. (3) different nickel catalysts were prepared by impregnation method. The catalytic effects of four kinds of catalysts for hydrogenation of silicon tetrachloride were compared. The results showed that Ni / HZSM-5 had the best catalytic performance. The optimum reaction conditions are as follows: nickel loading 10, reaction temperature 850 鈩，
本文編號：2234599
[Abstract]:In recent years, the polycrystalline silicon industry located in the upper reaches of photovoltaic has suffered a severe shock due to the cold wave of overcapacity. In addition to the factors that the foreign polysilicon production giants have impacted the domestic market, The fundamental reason is that its core technology is not mature enough, leading to high production costs. Reducing industry energy consumption and realizing recycling of by-products have become the key to the healthy and sustainable development of domestic polysilicon industry. The modified Siemens method is the mainstream process for the production of polysilicon. How to deal with the large quantity of silicon tetrachloride for every 1 ton polysilicon by-product about 15 tons of silicon tetrachloride has become a huge bottleneck restricting the development of polycrystalline silicon industry. The production of trichlorosilicon by hydrogenation of hydrochlorinated tetrachloride can realize the closed-circuit circulation of the material and reduce the production cost greatly. It has been paid more and more attention to by the industry. The problems of high energy consumption and low reaction conversion in the existing high temperature hydrogenation process and cold hydrogenation process need to be solved. How to improve the conversion rate of silicon tetrachloride and save energy and reduce consumption has become the research hotspot of hydrogenation technology. In order to solve this problem, the plasma hydrogenation process of silicon tetrachloride (DBD) was investigated, and the nickel-based catalyst was used in the hydrogenation at high temperature. The main contents and results are as follows: (1) DBD plasma discharge is proposed for hydrogenation of silicon tetrachloride, and plasma generator and quartz casing reactor are designed to build a professional experimental platform. The discharge conditions of DBD plasma and the hydrogenation of silicon tetrachloride were investigated. In DBD low temperature plasma, silicon tetrachloride is hydrogenated to produce trichlorosilicon. In the range of test power, the yield of trichlorosilicon increases with the increase of plasma power. Under the experimental conditions, the maximum yield of trichlorosilicon is 12.1. (2) the reaction progress is not easy to control during the hydrogenation of DBD plasma. The plasma reduction of silicon tetrachloride does not stop at the step of producing trichlorosilicon, but continues to reduce to form elemental silicon. High temperature silicon tetrachloride gas entrainment of amorphous silica fume to form conductive smoke, changed the original discharge structure, discharge spacing greatly smaller, discharge uniformity is not easy to control. (3) different nickel catalysts were prepared by impregnation method. The catalytic effects of four kinds of catalysts for hydrogenation of silicon tetrachloride were compared. The results showed that Ni / HZSM-5 had the best catalytic performance. The optimum reaction conditions are as follows: nickel loading 10, reaction temperature 850 鈩，
本文編號：2234599
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