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Method for Producing Trichlorosilane Verfahren Zur Herstellung Von Trichlorosilan Procédé De Production De Trichlorosilane

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Method for Producing Trichlorosilane Verfahren Zur Herstellung Von Trichlorosilan Procédé De Production De Trichlorosilane (19) TZZ __T (11) EP 2 546 197 B1 (12) EUROPEAN PATENT SPECIFICATION (45) Date of publication and mention (51) Int Cl.: of the grant of the patent: C01B 33/107 (2006.01) B01D 3/00 (2006.01) 24.08.2016 Bulletin 2016/34 B01D 3/14 (2006.01) (21) Application number: 11753001.4 (86) International application number: PCT/JP2011/001189 (22) Date of filing: 01.03.2011 (87) International publication number: WO 2011/111335 (15.09.2011 Gazette 2011/37) (54) METHOD FOR PRODUCING TRICHLOROSILANE VERFAHREN ZUR HERSTELLUNG VON TRICHLOROSILAN PROCÉDÉ DE PRODUCTION DE TRICHLOROSILANE (84) Designated Contracting States: • TABATA, Masaki AL AT BE BG CH CY CZ DE DK EE ES FI FR GB Joetsu-shi GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO Niigata 942-8601 (JP) PL PT RO RS SE SI SK SM TR (74) Representative: Smaggasgale, Gillian Helen et al (30) Priority: 10.03.2010 JP 2010052548 WP Thompson 138 Fetter Lane (43) Date of publication of application: London EC4A 1BT (GB) 16.01.2013 Bulletin 2013/03 (56) References cited: (73) Proprietor: Shin-Etsu Chemical Co., Ltd. EP-A1- 0 146 148 EP-A2- 2 033 937 Tokyo 100-0004 (JP) EP-A2- 2 036 857 EP-A2- 2 036 859 JP-A- 7 089 709 JP-A- 2004 149 351 (72) Inventors: JP-A- 2007 269 679 JP-A- 2009 062 209 • TANAKA, Shuji JP-A- 2009 062 210 JP-A- 2009 062 212 Joetsu-shi Niigata 942-8601 (JP) Note: Within nine months of the publication of the mention of the grant of the European patent in the European Patent Bulletin, any person may give notice to the European Patent Office of opposition to that patent, in accordance with the Implementing Regulations. Notice of opposition shall not be deemed to have been filed until the opposition fee has been paid. (Art. 99(1) European Patent Convention). EP 2 546 197 B1 Printed by Jouve, 75001 PARIS (FR) EP 2 546 197 B1 Description Technical Field 5 [0001] The present invention relates to a method for producing trichlorosilane. In more detail, the present invention relates to a method for separating trichlorosilane from methyldichlorosilane more easily to obtain high-purity trichlorosi- lane. Background Art 10 [0002] Trichlorosilane (HSiCl3) has long been used as a raw material for high-purity polycrystalline silicon, which is used for the production of, for example, s ilicon wafers. As to the technique for obtaining trichlorosilane, many synthetic methods are known, and Japanese Patent Laid-Open No. 56-73617 (Patent Literature 1) discloses an invention relating to a method for producing trichlorosilane, advantageously characterized in that the by-product silicon tetrachloride is 15 efficiently converted into trichlorosilane in the production of trichlorosilane. [0003] Other known methods for producing trichlorosilane include a direct method in which metallurgical grade silicon is allowed to contact hydrogen chloride at a temperature of about 250°C or higher (refer to Japanese Patent Laid-Open No. 2-208217 (Patent Literature 2) and Japanese Patent Laid-Open No. 9-169514 (Patent Literature 3), and the like), a method for reducing silicon tetrachloride to trichlorosilane by reacting it with hydrogen in the presence of metallurgical 20 grade silicon (refer to Japanese Patent Laid-Open No. 60-36318 (Patent Literature 4)), and a method in which, using copper silicide in place of the metallurgical grade silicon, silicon tetrachloride is reduced to trichlorosilane by reacting it with hydrogen in the presence of the copper silicide (refer to Japanese Patent Laid-Open No. 10-29813 (Patent Literature 5)). [0004] Meanwhile, an impurity such as phosphorus or boron acts as a donor or acceptor in a silicon crystal. Thus, 25 when these dopant components are present in the raw material polycrystalline silicon used for the production of semi- conductor, they will be taken up in the final silicon wafer product. For this reason, for the production of semiconductor grade polycrystalline silicon, high-purity trichlorosilane obtained through precise distillation is used. [0005] In connection with the these manufacturing technologies for high-purity trichlorosilane, a method for separating and removing the aforementioned dopant components in advance before distillation of trichlorosilane by converting them 30 into an easily separable form with, for example, a getter is also proposed (for example, refer to Japanese Patent Laid- Open No. 2004-250317 (Patent Literature 6)). [0006] Further, carbon impurities in silicon crystals form an impurity level within the band gap and act as a carrier trap, and accelerate the formation of precipitation nuclei of oxygen in the crystals to induce defects in the production process of semiconductor devices. In view of the above, carbon impurity content is also a problem in semiconductor grade 35 polycrystalline silicon. [0007] Carbon impurities contaminating polycrystalline silicon may include carbon-containing compounds derived from a carbon member used in a CVD reactor which is employed for deposition of polycrystalline silicon, or carbon-containing compounds contained in trichlorosilane or hydrogen. However, it is not easy to produce trichlorosilane from which carbon- containing compounds have been sufficiently removed. 40 [0008] This is due to the following reasons: Because metal silicone used for direct synthesis of trichlorosilane is produced in an arc furnace using a carbon electrode, it has a purity of only about 99% and includes carbon as an impurity. Also, because the product for trichlorosilane synthesis flowing out of a CVD reactor contains methylchlorosilanes derived from the carbon member inside the CVD reactor, trichlorosilane purified by distillation still contains a trace amount of the aforementioned carbon-derived methylchlorosilanes. For example, when a carbon impurity-containing product pro- 45 duced in an arc furnace using a carbon electrode is used as the metallurgical grade silicon, lower boiling methylchlo- rosilanes will be mixed in an amount of about several tens of ppm in terms of weight ratio as the carbon impurity-derived by-product. [0009] Particularly, removal of methyldichlorosilane is difficult because it is not only the main component of methyl- chlorosilanes that are mixed in as described above but also its boiling point (41°C) is close to that of trichlorosilane 50 (32°C), which is a target product to be purified by distillation. [0010] EP203685, EP2036859 and EP2033937 disclose methods for making trichlorosilane, comprising the use of tetrachlorosilane and elemental chlorine. Citation List 55 Patent Literature [0011] 2 EP 2 546 197 B1 Patent Literature 1: Japanese Patent Laid-Open No. 56-73617 Patent Literature 2: Japanese Patent Laid-Open No. 2-208217 Patent Literature 3: Japanese Patent Laid-Open No. 9-169514 Patent Literature 4: Japanese Patent Laid-Open No. 60-36318 5 Patent Literature 5: Japanese Patent Laid-Open No. 10-29813 Patent Literature 6: Japanese Patent Laid-Open No. 2004-250317 Patent Literature 7: Japanese Patent Laid-Open No. 2004-149351 Summary of Invention 10 Technical Problem [0012] In view of these problems, Japanese Patent Laid-Open No. 2004-149351 (Patent Literature 7) discloses a method for purifying trichlorosilane capable of reducing-the concentration of carbon impurities at a relatively low cost. 15 This method employs a technique in which trichlorosilane is allowed to contact adsorbents such as silica gel and activated carbon so that carbon-containing silicon chloride compounds in the trichlorosilane are uniformly removed all at once, irrespective of the boiling points. [0013] However, removal of methyldichlorosilane whose boiling point is close to that of trichlorosilane is still difficult even with this method, and thus the burden on distillation is still unavoidably high. Aside from that, a burdensome task 20 will arise such that adsorbents after the adsorption treatment need to be processed accordingly as waste products. [0014] The present invention was completed in view of the foregoing problems, and an object of the present invention is to provide a technique that removes methyldichlorosilane more easily, which has been difficult to remove by conven- tional techniques, in the production of high-purity trichlorosilane without requiring a process of excessive distillation purification. 25 Solution to Problem [0015] In order to solve such problems, the method for producing trichlorosilane of the present invention is a method for obtaining high-purity trichlorosilane from a mixture comprising methyldichlorosilane (CH3HSiCl2), tetrachlorosilane 30 (SiCl4), and trichlorosilane (HSiCl3), comprising the steps of: (A) distilling the mixture to fractionate a fraction with a higher content of methyldichlorosilane than the mixture before distillation; (B) heating the fraction thus fractionated to disproportionate chlorine between methyldichlorosilane and tetrachlorosilane and thus convert the methyldichlorosilane into methyltrichlorosilane (CH3SiCl3); and (C) purifying the fraction after the disproportionation containing the methyl- trichlorosilane (CH 3SiCl3) by distillation to separate trichlorosilane, wherein the step (B) is carried out in the absence of Cl 2. 35 [0016] The disproportionation of chlorine in the step (B) is preferably carried out at a temperature range of 300 to 600°C. [0017] In thepresent invention, the disproportionation of chlorine inthe step (B)can alsobe carried outwithout a catalyst. [0018] In the present invention, the disproportionation of chlorine in the step (B) may be carried out in a heated vessel with a fluidized bed of silicon containing copper chloride as a catalyst under a hydrogen-containing.
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