WO2020179561A1 - クロロシラン類の製造方法 - Google Patents
クロロシラン類の製造方法 Download PDFInfo
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- WO2020179561A1 WO2020179561A1 PCT/JP2020/007622 JP2020007622W WO2020179561A1 WO 2020179561 A1 WO2020179561 A1 WO 2020179561A1 JP 2020007622 W JP2020007622 W JP 2020007622W WO 2020179561 A1 WO2020179561 A1 WO 2020179561A1
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- WIPO (PCT)
- Prior art keywords
- metallic silicon
- silicon
- sodium
- ppm
- fluidized bed
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
- C01B33/1071—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof
- C01B33/10715—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by reacting chlorine with silicon or a silicon-containing material
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
- C01B33/1071—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof
- C01B33/10742—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by hydrochlorination of silicon or of a silicon-containing material
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
Definitions
- the present invention relates to a novel method for producing chlorosilanes. Specifically, it provides a method capable of stably producing chlorosilanes by a chlorination reaction of metallic silicon.
- Chlorosilanes used for producing high-purity polysilicon represented by the Siemens method are produced by purifying chlorosilanes obtained by a chlorination reaction of metallic silicon.
- a method of supplying metallic silicon powder and hydrogen chloride to a fluidized bed in a reactor and producing chlorosilanes by a chlorination reaction of metallic silicon is common.
- a method is also known in which metallic silicon powder, tetrachlorosilane, and hydrogen, if necessary, are supplied to a fluidized bed to produce chlorosilanes by a chlorination reaction of metallic silicon.
- This reaction is expressed as the following formula. It is known that the reactions of the following formulas (1) and (2) occur at a reaction temperature of 300 to 360° C., and the reaction of the following formula (3) occurs at 500 to 550° C.
- the production of metallic silicon as a raw material uses a silicon raw material typified by silica stone and charcoal, coke, coal, wood chips, etc. as a reducing material, and a mixture of these is filled in an arc furnace as a raw material layer, 2300. It is carried out by heating at a high temperature of about 2800 K to reduce silica stone (see Non-Patent Document 1).
- the metallic silicon obtained by the above method is obtained as a large lump, but since the chlorination reaction of the metallic silicon is generally performed in a fluidized bed, the metallic silicon lump has a particle size having an average particle size of 400 ⁇ m or less. And subjected to the reaction in the form of metallic silicon powder.
- metallic silicon powder relatively low-purity silicon powder generally called metallurgical grade is used (Patent Document 1). Its purity is usually about 99%, and it is also called “2N (two-nine)" or crude metal silicon in this industry.
- the metallic silicon when the pulverized metallic silicon is fluidized in a fluidized bed type reactor to carry out a chlorination reaction, the metallic silicon aggregates or is produced as chlorosilanes and dimer (Si 2 HCl 5 , Si 2 Cl). 6 ) was sometimes included.
- dimers are also referred to in the art as "polymers".
- the agglomerates formed by the aggregation of metallic silicon may have a particle size of up to about 10 cm, which significantly impairs the fluidity of the fluidized bed and causes a decrease in yield.
- the formation of dimers requires purification of chlorosilanes, which causes a decrease in yield.
- Crude metallic silicon may also contain aluminum and sodium as impurities.
- aluminum and sodium are also chlorinated, and it is considered that NaAlCl 4 (hereinafter sometimes referred to as "double salt") having a low melting point is produced by the following reaction.
- the melting point of the double salt is about 185 ° C., and it is liquid at the above-mentioned reaction temperature for chlorosilane formation. Therefore, it is considered that the metallic silicon particles in the fluidized bed are fused to form a metallic silicon lump. Further, the liquid double salt adheres to the inner wall of the reactor together with the silicon particles. As a result, the fluidity of the fluidized bed deteriorates. The occurrence of poor flow induces erosion. Furthermore, heat spots are generated because it becomes difficult to remove heat from the reactor due to deposits. As a result, phenomena such as an increase in the amount of chlorosilane dimer produced and a runaway reaction occur, and in some cases, the chlorination reaction must be stopped.
- Patent Documents 2 and 3 Purification of metallic silicon has been carried out for various purposes. Also in the production of the above chlorosilanes, it is conceivable to purify the crude metallic silicon as a raw material to reduce the formation of silicon lumps and dimers. However, purification of metallic silicon, which is a raw material for producing chlorosilane, requires cost.
- an object of the present invention is that when chlorosilanes are produced by the reaction of metallic silicon and hydrogen chloride, when low-purity silicon generally called metallurgical grade is used as a raw material, metallic silicon is used in a fluidized bed type reaction apparatus. It is an object of the present invention to provide a method capable of stably producing chlorosilanes by preventing aggregation and adhesion to the reaction wall.
- the present inventors have made extensive studies on the causes of inducing phenomena such as aggregation and adhesion of silicon powder during the production of the chlorosilanes. It was known that crude metallic silicon, which is a raw material, contains a relatively large amount of aluminum component. This is thought to be derived from the raw material silica stone. However, there have been no reports of aluminum causing the above problems. However, it has been confirmed by the present inventors that the phenomenon occurs when a large amount of sodium is mixed in the crude metallic silicon manufacturing process.
- the impurity sodium contained in calcium carbonate may remain in the melting furnace without being separated, and sodium may be mixed in the crude metallic silicon produced in the next reaction.
- sodium silicate is often used as an adhesive for refractory bricks constituting the melting furnace, and the sodium concentration in the metallic silicon obtained immediately after starting the furnace is high. Rise.
- the sodium component contained in the crude metal silicon exceeds a specific amount, it reacts in the fluidized bed with the aluminum component originally contained in the crude metal silicon to form a double salt having a low melting point, and the crude metal It was found that it causes agglomeration of silicon powder and adhesion of metallic silicon to the inner wall of the fluidized bed type reactor. Based on the above findings, it has been found that all the above problems can be solved by controlling the sodium content of crude metallic silicon so as to be equal to or less than a specific value, and the present invention has been completed.
- chlorosilanes when chlorosilanes are produced by the chlorination reaction of metallic silicon, the content of sodium as the metallic silicon is 1 ppm or more and 90 ppm or less in terms of elements, and the content of aluminum is 1000 ppm or more in terms of elements.
- a method for producing chlorosilanes which comprises using metallic silicon of 4000 ppm or less.
- the metal silicon preferably has an average particle size of 150 to 400 ⁇ m from the viewpoint of facilitating formation of a fluidized bed.
- the chlorination reaction of metallic silicon is low due to the reaction between aluminum contained in crude metallic silicon and sodium. It is possible to suppress the formation of a compound salt having a melting point, and effectively prevent the aggregation of the silicon powder and the adhesion of metallic silicon to the inner wall of the fluidized bed type reactor. As a result, the formation of silicon lumps in the fluidized bed is suppressed, the formation of dimers (polymers) is reduced, and chlorosilanes can be stably produced.
- chlorosilanes For example, a method for producing chlorosilanes by supplying the crude metallic silicon powder and a chlorine source gas such as hydrogen chloride and tetrachlorosilane to the fluidized bed of a fluidized bed type reactor and performing a chlorination reaction of metallic silicon.
- chlorosilanes include monosilanes such as dichlorosilane, trichlorosilane, and tetrachlorosilane.
- the hydrogen chloride various industrially available hydrogen chlorides can be used. Further, the supply amounts of metallic silicon and hydrogen chloride are known as long as the metallic silicon and hydrogen chloride can be supplied at a rate that allows chlorination and a flow rate at which a fluidized bed can be formed. Conditions are adopted without any particular restrictions.
- the reaction temperature in the reaction is appropriately determined in consideration of the material and capacity of the reactor, the catalyst, etc., but is generally set in the range of 200 to 500 ° C, preferably 250 to 450 ° C.
- chlorosilanes there is also a method of supplying metallic silicon powder, tetrachlorosilane and hydrogen together with a catalyst typified by copper silicide to a fluidized bed to carry out a chlorination reaction of metallic silicon.
- the supply amount of metallic silicon, tetrachlorosilane, and hydrogen is a ratio that allows chlorination, and the metallic silicon, tetrachlorosilane, and hydrogen are supplied at a rate that allows the flow bed to be formed. If it can be supplied, known conditions are adopted without particular limitation.
- the reaction temperature in the reaction is appropriately determined in consideration of the material and capacity of the reaction apparatus, the catalyst and the like, but is generally set in the range of 400 to 700 ° C, preferably 450 to 600 ° C.
- the sodium content of crude metallic silicon used as a raw material in the above method is 1 ppm or more and 90 ppm or less, preferably 3 ppm or more and 50 ppm or less, and more preferably 5 ppm or more and 40 ppm or less in terms of elemental mass.
- the biggest feature is that.
- the content of aluminum in crude metallic silicon is the same as that of ordinary 2N grade metallic silicon, and is 1000 ppm or more and 4000 ppm or less, preferably 1500 ppm or more and 2500 ppm or less in terms of elemental mass.
- the purity of crude metallic silicon is preferably the same as that of ordinary 2N grade metallic silicon, and the silicon content is about 99% in terms of elemental mass, and more specifically, 98.5 to 99.4%. It may be 99.0 to 99.4%.
- silicon raw material typified by silica stone and charcoal, coke, coal, wood chips and the like are used as reducing materials, and a mixture thereof is filled in an arc furnace as a raw material layer, and 2300 Since it is produced by heating at a high temperature of about 2800 K and reducing silica stone, it can be obtained as a large lump having a mass of about 1000 to 2000 kg.
- chlorosilanes it is crushed into metallic silicon of a size suitable for the reaction.
- the method for reducing the sodium concentration in the silicon powder within the above range is not particularly limited, but the method for eliminating the above-mentioned pollution source is effective.
- a mold release agent for pouring metallic silicon obtained from a melting furnace a sodium-free mold release agent, for example, metallic silicon or carbon is used, and sodium carbonate is used as a heat insulating agent for the melting furnace.
- a low content is used, and further, after a new melting furnace is installed, the metal silicon is manufactured after being dry-heated until the influence of sodium derived from sodium silicate used as an adhesive disappears. Aspects are mentioned.
- the lower limit of the content of sodium contained in the raw material crude metal silicon is 1 ppm. Although it is technically easy to set the sodium content to less than 1 ppm, it causes an increase in cost as described above. Moreover, there is no difference in the effect obtained even when the sodium content is less than 1 ppm.
- the lower limit of the content of aluminum contained in the raw material crude metal silicon is 1000 ppm. Although it is technically easy to set the aluminum content to less than 1000 ppm, it causes an increase in cost as described above. Moreover, there is no difference in the effect obtained even when the aluminum content is less than 1000 ppm.
- the metallic silicon may be of any size that can be fluidized in a fluidized bed, and preferably has an average particle size of 150 to 400 ⁇ m, particularly 180 to 300 ⁇ m.
- the average particle size of silicon was measured according to the method described in Examples. By setting the average particle size of silicon within the above range, a stable fluidized bed can be obtained.
- sieves conforming to the test sieve specified in JIS Z 8801-1 and having a nominal opening of 500 ⁇ m, 355 ⁇ m, 250 ⁇ m, 212 ⁇ m, 150 ⁇ m, 106 ⁇ m, and 45 ⁇ m are stacked. Classify using the attached vibrating sieve.
- ⁇ Analysis method> The amount of dimers (Si 2 HCl 5 and Si 2 HCl 6 ) produced in all chlorosilanes was measured by gas chromatography (GC-TCD) using a thermal conductivity detector under the following conditions.
- Chlorosilane was produced by a fluidized bed reactor in the same manner as described above (amount of dimer produced). After operating for 30 days, the apparatus was stopped and the bottom plate under the fluidized bed was visually observed to confirm the presence or absence of a silicon mass (mass of 1 kg or more).
- Examples 1 to 4 Silica is reduced in a melting furnace to obtain a silicon melt.
- sodium-free one for example, metal silicon or carbon is used, and one having a low sodium content is used as calcium carbonate used as a heat-retaining agent for a melting furnace.
- the amount of sodium mixed in the manufacturing process is limited by methods such as performing empty heating until the effect of sodium derived from sodium silicate used as an adhesive disappears, and then manufacturing metallic silicon.
- metallic silicon whose sodium content was controlled as shown in Table 1 was obtained.
- the obtained metallic silicon was crushed to obtain crude metallic silicon having an average particle size shown in Table 1, and the above evaluation was performed. The results are shown in Table 1.
- Comparative Example 1 The above evaluation was performed using commercially available 2N grade crude metal silicon having the composition and average particle size shown in Table 1. The results are shown in Table 1.
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
Description
本発明者らは、上記の現象の要因について鋭意検討したところ、以下のような知見を得た。
50mlのテフロン(登録商標)製ビーカーにシリコン試料を0.5g~1.0g精秤した。その中に7N-HNO330mlを加えた。さらに、HF(50質量%)を徐々に加えて試料を分解した。それをホットプレート上に乗せ、温度140℃で2時間加熱させた後、ホットプレート温度160℃で1時間、さらにホットプレート温度140℃に調整し、残液が少量になるまで加熱した。その中に、回収試薬として、HCl(35質量%)を2ml添加し、さらに純水5mlを加え、ホットプレート温度140℃で5分間加熱した。ビーカーをホットプレートから降ろし、常温まで冷ました。ビーカー内の試料液をポリエチレン製漏斗とろ紙を用いて、ポリエチレン製100mlメスフラスコにろ過し、さらに純水にて、100mlまでメスアップした。この液をICP-OES装置として2波シーケンシャル形プラズマ発光分析装置に導入して分析した。
原料として用いた粗金属シリコン3~10gを乳鉢に採取する。採取したシリコンを乳棒ですり潰す。得られた粉状試料を蛍光X線専用の試料台に乗せ、蛍光X線分析装置(株式会社リガク製、ZSX PrimusII)でシリコン含量を測定する。
<採取方法>
1トンーフレキシブルコンテナに入った金属シリコンから約1kgをガラス容器に採取する。採取したサンプルを、よく撹拌した後、以下の分析に必要な量を採取する。
<分析方法>
金属シリコン粉約100gを、複数の篩を有する振動篩機を用いて分級し、各留分を最小留分から累積加算して50質量%となったときの累積径を平均粒径(メジアン径)とする。より具体的には、JIS Z 8801-1に規定される試験用篩に適合する篩であって、公称目開きが、500μm、355μm、250μm、212μm、150μm、106μm、45μmである篩を重ねて装着した振動篩機を用いて分級する。
<採取方法>
流動床方式反応装置に、金属シリコン粉と塩化水素(HCl)とを供給して反応させ、トリクロロシラン類を生成せしめ、トリクロロシラン類生成後の流動床方式反応装置の反応装置出口から生成したクロロシランガス及び金属シリコン粉を回収した。得られたクロロシランガスと金属シリコンをフィルターに通し、金属シリコンを除去した。クロロシランガスを熱交換器で冷却し、クロロシラン液を得て、ドラムに貯留した。ドラムから分析に必要な量のクロロシラン液を採取した。
<分析方法>
熱伝導度検出器を用いたガスクロマトグラフィー(GC-TCD)にて下記条件で測定し、全クロロシラン中の二量体(Si2HCl5及びSi2HCl6)生成量を調べた。
使用機器: 島津製作所 C-R8A
キャリア-ガス: 水素(G2)
二量体の生成量は反応装置内にヒートスポットが形成された際に増加するため、流動不良の評価方法として採用できる。
上記(二量体の生成量)と同様にして流動床方式反応装置によりクロロシランを製造した。30日運転した後に、装置を停止し、流動床下部の底板を目視にて観察し、シリコン塊(質量1kg以上)の有無を確認した。
珪石を溶融炉で還元し、シリコン融液を得る。得られる金属シリコンを流し込む型の離型剤として、ナトリウムフリーのもの、例えば、金属シリコンやカーボンを使用する、溶融炉の保温剤として使用される炭酸カルシウムとしてナトリウム含有量の低いものを使用する、溶融炉の新設後、接着剤として使用したケイ酸ソーダ由来のナトリウムの影響が無くなるまで空焚きを行った後、金属シリコンの製造を行う等の方法により、製造工程におけるナトリウムの混入量を制限して、表1に示すナトリウム含量に管理された金属シリコンを得た。
得られた金属シリコンを破砕し、表1に示す平均粒径の粗金属シリコンを得て、上記の評価を行った。結果を表1に示す。
表1に示す組成、平均粒径の市販の2Nグレードの粗金属シリコンを用いて上記の評価を行った。結果を表1に示す。
Claims (2)
- 金属シリコンの塩素化反応によりクロロシラン類を製造するに際し、上記金属シリコンとして、ナトリウムの含量が元素換算で1ppm以上90ppm以下、アルミニウムの含量が元素換算で1000ppm以上、4000ppm以下の金属シリコンを使用することを特徴とするクロロシラン類の製造方法。
- 前記金属シリコンの平均粒径が150~400μmである請求項1に記載のクロロシラン類の製造方法。
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
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KR1020217027637A KR20210130161A (ko) | 2019-03-05 | 2020-02-26 | 클로로 실란류의 제조방법 |
EP20766143.0A EP3919441B1 (en) | 2019-03-05 | 2020-02-26 | Chlorosilane producing method |
US17/435,056 US20220162079A1 (en) | 2019-03-05 | 2020-02-26 | Chlorosilane Producing Method |
JP2020532067A JP6811361B1 (ja) | 2019-03-05 | 2020-02-26 | クロロシラン類の製造方法 |
CN202080018385.8A CN113508091B (zh) | 2019-03-05 | 2020-02-26 | 氯硅烷类的制造方法 |
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US (1) | US20220162079A1 (ja) |
EP (1) | EP3919441B1 (ja) |
JP (1) | JP6811361B1 (ja) |
KR (1) | KR20210130161A (ja) |
CN (1) | CN113508091B (ja) |
TW (1) | TWI837316B (ja) |
WO (1) | WO2020179561A1 (ja) |
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- 2020-02-26 KR KR1020217027637A patent/KR20210130161A/ko unknown
- 2020-02-26 EP EP20766143.0A patent/EP3919441B1/en active Active
- 2020-02-26 WO PCT/JP2020/007622 patent/WO2020179561A1/ja unknown
- 2020-02-26 JP JP2020532067A patent/JP6811361B1/ja active Active
- 2020-02-26 CN CN202080018385.8A patent/CN113508091B/zh active Active
- 2020-02-26 US US17/435,056 patent/US20220162079A1/en active Pending
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"Current Situation and Issues of Small Arc Furnace", INDUSTRIAL HEATING, vol. 46, no. 3, 2009, pages 1 - 11 |
See also references of EP3919441A4 |
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JPWO2020179561A1 (ja) | 2021-03-11 |
CN113508091B (zh) | 2024-05-03 |
CN113508091A (zh) | 2021-10-15 |
KR20210130161A (ko) | 2021-10-29 |
EP3919441B1 (en) | 2023-07-26 |
EP3919441A4 (en) | 2022-11-09 |
TWI837316B (zh) | 2024-04-01 |
JP6811361B1 (ja) | 2021-01-13 |
US20220162079A1 (en) | 2022-05-26 |
TW202039365A (zh) | 2020-11-01 |
EP3919441A1 (en) | 2021-12-08 |
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