發(fā)布時(shí)間：2018-04-19 21:47

  本文選題：四氯化鈦 + 雜質(zhì)分析　； 參考：《北京理工大學(xué)》2015年博士論文

【摘要】：鈦具有密度小、比強(qiáng)度高、耐高溫以及耐腐蝕性能好等一系列優(yōu)異特性,從而被廣泛的應(yīng)用于化工、冶金、航空、航天、醫(yī)藥等領(lǐng)域。為了去除精TiCl_4中的雜質(zhì),需要對(duì)主要雜質(zhì)(氧、碳)進(jìn)行分析,對(duì)精TiCl_4質(zhì)量進(jìn)行嚴(yán)格控制。至今,我國(guó)鈦廠執(zhí)行的標(biāo)準(zhǔn)中,TiCl_4的雜質(zhì)檢測(cè)僅包括FeCl_3、SiCl_4、VOCl_3和色度這幾個(gè)分析指標(biāo),由于缺少有效的TiCl_4中主要雜質(zhì)(碳、氧)的分析,從而造成TiCl_4執(zhí)行標(biāo)準(zhǔn)較低,導(dǎo)致海綿鈦產(chǎn)品質(zhì)量受到較大影響,嚴(yán)重的影響我國(guó)鈦產(chǎn)業(yè)的發(fā)展。本研究課題來(lái)源于科技部創(chuàng)新方法專項(xiàng)項(xiàng)目(No.2011IM030700)資助,以國(guó)內(nèi)鈦企業(yè)對(duì)精TiCl_4中主要雜質(zhì)分析方法的迫切需求為導(dǎo)向,本研究的目的是建立主要雜質(zhì)的分析方法,研究成果應(yīng)用于企業(yè)控制精TiCl_4的質(zhì)量。以遵義鈦業(yè)股份有限公司提供的精Ti Cl_4為樣品,對(duì)含量較高的主要雜質(zhì)(碳、氧)進(jìn)行測(cè)定及控制分析,具體研究成果歸納如下:(1)針對(duì)精TiCl_4腐蝕性強(qiáng)的特性,以及紅外光譜分析的特點(diǎn),設(shè)計(jì)了一種密封性能良好、便于清洗和操作、可重復(fù)使用、不同光程的紅外吸收池測(cè)定裝置,通過(guò)紅外光譜法定量分析精TiCl_4中的雜質(zhì)。(2)選用TiOCl_2為紅外光譜研究目標(biāo)物,通過(guò)單標(biāo)法測(cè)得精TiCl_4中TiOCl_2含量為833.8±80.0mg/kg,相對(duì)標(biāo)準(zhǔn)偏差(RSD)在0.95%~1.94%之間;方法檢出限為26.7mg/kg,加標(biāo)回收率在88.5%~93.1%。折算成氧含量為98.8mg/kg,TiOCl_2是精TiCl_4中氧雜質(zhì)的主要提供者。(3)選用CO_2為紅外光譜研究目標(biāo)物,通過(guò)單標(biāo)法測(cè)得精TiCl_4中CO_2含量為1.53±0.11mg/kg,相對(duì)標(biāo)準(zhǔn)偏差(RSD)在0.53%~1.27%之間;方法檢出限為0.92mg/kg,加標(biāo)回收率在91.9%~94.7%。(4)選用有機(jī)雜質(zhì)為紅外光譜研究目標(biāo)物,通過(guò)標(biāo)準(zhǔn)加入法測(cè)得Ti Cl_4中CS_2、CH_2ClCOCl、CHCl_2COCl含量為6.6±0.1mg/kg、17.9±0.3mg/kg、2.2±0.4mg/kg;檢出限分別為0.1mg/kg、2.0mg/kg、1.0mg/kg;酰氯類峰有重疊,導(dǎo)致紅外分別定量分析難度較大,定量相對(duì)偏差較大。(5)選用CCl_3COCl為研究目標(biāo)物,通過(guò)離子色譜法測(cè)得TiCl_4中CCl_3COCl含量為41.3mg/kg,相對(duì)標(biāo)準(zhǔn)偏差(RSD)為7.7%;方法檢出限為0.6mg/kg,加標(biāo)回收率在84.1%~87.3%。折算成碳含量為5.4mg/kg,酰氯類雜質(zhì)是精TiCl_4中碳雜質(zhì)的主要提供者之一。(6)選取CCl_4為研究目標(biāo)物,通過(guò)氣相色譜法(ECD)測(cè)得精TiCl_4中CCl_4含量為0.17mg/kg,相對(duì)標(biāo)準(zhǔn)偏差(RSD)為2.4%;方法檢出限為0.001mg/kg,加標(biāo)回收率在95%~104%之間。
[Abstract]:Titanium has a series of excellent properties such as low density, high specific strength, high temperature resistance and good corrosion resistance, so it is widely used in chemical, metallurgical, aerospace, medical and other fields. In order to remove impurities in refined TiCl_4, it is necessary to analyze the main impurities (oxygen, carbon) and strictly control the quality of refined TiCl_4. Up to now, the impurity detection of TiClCO4 in the standard implemented by Chinese titanium plants only includes the analysis indexes of FeClS3SiCl4SiCl4VO Cl3 and chromaticity. Due to the lack of effective analysis of the main impurities (carbon, oxygen) in TiCl_4, the implementation standard of TiCl_4 is low. As a result, the quality of sponge titanium products is greatly affected, which seriously affects the development of China's titanium industry. This research project comes from the special project No. 2011IM030700 of the Ministry of Science and Technology. It is guided by the urgent need of domestic titanium enterprises to analyze the main impurity in TiCl_4. The purpose of this research is to establish the analytical method of the main impurity. The research results are applied to enterprises to control the quality of fine TiCl_4. Taking the refined Ti Cl_4 provided by Zunyi Titanium Industry Co., Ltd. as the sample, the main impurity (carbon, oxygen) with high content is determined and controlled. The concrete research results are summarized as follows: 1) the characteristic of high corrosivity of refined TiCl_4. As well as the characteristics of infrared spectrum analysis, a kind of infrared absorption cell measuring device with good sealing performance, easy cleaning and operation, reusability and different optical path is designed. The content of TiOCl_2 in refined TiCl_4 was 833.8 鹵80.0 mg / kg, the relative standard deviation was between 0.95mg / kg and 1.94%, the detection limit was 26.7 mg / kg and the recovery rate was 88.5mg / kg. The converted oxygen content of 98.8 mg / kg TiOCl2 is the main provider of oxygen impurity in refined TiCl_4. CO_2 is chosen as the target of infrared spectroscopy. The content of CO_2 in refined TiCl_4 is 1.53 鹵0.11 mg / kg, and the relative standard deviation is between 1.27% and 1.27% by single standard method. As a result, IR quantitative analysis is difficult, the relative deviation of quantitative analysis is large. CCl_3COCl is chosen as the research object. The content of CCl_3COCl in TiCl_4 is 41.3 mg / kg by ion chromatography, and the relative standard deviation is 7.7.The detection limit of the method is 0.6 mg / kg, and the recovery rate is 87.30.The detection limit of the method is 0.6 mg / kg. The carbon content is 5.4 mg / kg. Acyl chloride impurity is one of the main carbon impurities in refined TiCl_4. The content of CCl_4 in TiCl_4 was 0.17 mg / kg, the relative standard deviation (RSD) was 2.4%, the detection limit was 0.001 mg / kg and the recovery rate was between 95% and 104%.
【學(xué)位授予單位】：北京理工大學(xué)
【學(xué)位級(jí)別】：博士
【學(xué)位授予年份】：2015
【分類號(hào)】：TQ134.11

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