WO2011045880A1 - 水素ガス回収システムおよび水素ガスの分離回収方法 - Google Patents
水素ガス回収システムおよび水素ガスの分離回収方法 Download PDFInfo
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- Y02P20/156—Methane [CH4]
Definitions
- the present invention relates to a hydrogen gas recovery system and a hydrogen gas separation and recovery method, and more specifically, a technique for separating and recovering hydrogen from a reaction exhaust gas of a polycrystalline silicon production apparatus using trichlorosilane as a raw material, and using this separately.
- a hydrogen gas recovery system and a hydrogen gas separation and recovery method and more specifically, a technique for separating and recovering hydrogen from a reaction exhaust gas of a polycrystalline silicon production apparatus using trichlorosilane as a raw material, and using this separately.
- tetrachlorosilane and hydrogen by-produced according to Formula 2 can be converted to trichlorosilane by a reaction reverse to Formula 2, so that these by-products can be reused as a raw material gas for producing polycrystalline silicon. It is being used.
- the loss of the above-mentioned by-products is reduced and converted into trichlorosilane with high efficiency, that is, exhaust gas from the polycrystalline silicon manufacturing system is recovered and circulated with high efficiency. ⁇ Technology to reuse is required.
- the reaction exhaust gas from the polycrystalline silicon manufacturing system includes other As a by-product gas, a small amount of monochlorosilane (SiH 3 Cl) and dichlorosilane (SiH 2 Cl 2 ) are contained. In addition, as trace impurities, carbon monoxide (CO), methane (CH 4 ), monosilane (SiH 4 ), and nitrogen (N 2 ) are included.
- CO carbon monoxide
- CH 4 methane
- SiH 4 monosilane
- N 2 nitrogen
- chlorosilanes tetrachlorosilane, trichlorosilane, dichlorosilane, and monochlorosilane are collectively referred to as chlorosilanes, and the liquid is referred to as a chlorosilane liquid.
- the reaction exhaust gas from the polycrystalline silicon manufacturing apparatus is first separated into hydrogen and other components by a hydrogen recovery and circulation device directly connected to the polycrystalline silicon manufacturing apparatus, and the separated hydrogen is circulated and again returned to the polycrystalline silicon manufacturing apparatus.
- a hydrogen separation and recovery method is as follows: “New Energy Development Organization Commissioned Business Results Report, 1987-62, Development of Technology for Practical Use of Solar Power Generation System, Low-cost Silicon Experimental Refining Verification (Technology Development of Chlorsilane Hydrogen Reduction Process) It is publicly known by “Summary Version” (Non-Patent Document 1), Japanese Patent Laid-Open No. 2008-143775 (Patent Document 1), and the like.
- a gas absorption method using a chlorosilane solution is employed as a method for separating hydrogen chloride. Since the solubility of hydrogen chloride in a chlorosilane solution is not large, it is necessary to separate hydrogen chloride by a gas absorption method at a low temperature ( ⁇ 20 ° C. or lower), but it can be separated efficiently if sufficient heat recovery is performed.
- the separation method by adsorption utilizes the fact that the amount of impurities adsorbed on the surface of an adsorbent such as activated carbon increases at high pressure and low temperature, but decreases at low pressure and high temperature. This is a batch operation method in which adsorption operation and regeneration operation under low pressure and high temperature are performed alternately.
- a general activated carbon adsorption tower is composed of a plurality of activated carbon packed towers that are selectively used. Activated carbon loses its adsorption capacity after a certain period of time. This is called breakthrough, but it is switched to a regenerated activated carbon packed tower before breakthrough occurs.
- the used activated carbon is regenerated by releasing the adsorbed components by purging with a carrier gas under low pressure and high temperature. This is called adsorption component desorption.
- a carrier gas for regeneration of activated carbon is required to have a purity comparable to that of recovered hydrogen.
- recovered hydrogen purified by an activated carbon adsorption tower is used, or high purity hydrogen is replenished from the outside. And it is discharged
- Non-Patent Document 1 hydrogen as a carrier gas is newly supplied from the outside, and the desorption gas is sent to the conversion step of tetrachlorosilane to trichlorosilane and reused.
- the desorption gas is sent to the conversion step of tetrachlorosilane to trichlorosilane and reused.
- the present invention has been made in view of the above-mentioned problems, and its object is to effectively separate and reuse the desorption gas, and chlorosilanes, hydrogen chloride from the reaction exhaust gas of the polycrystalline silicon production apparatus,
- An object of the present invention is to provide a technique for producing polycrystalline silicon with low cost and high purity by reducing the replenishment amount of hydrogen gas used for separating nitrogen, carbon monoxide, methane, and monosilane as much as possible.
- a hydrogen gas recovery system of the present invention is a hydrogen gas recovery system used for separating and recovering hydrogen gas from reaction exhaust gas from an apparatus for producing polycrystalline silicon using trichlorosilane as a raw material.
- the condensation separation device for condensing and separating chlorosilanes from the reaction exhaust gas containing hydrogen from the polycrystalline silicon manufacturing process, the compression device for compressing the reaction exhaust gas containing hydrogen via the condensation separation device, and the compression device An absorption device that absorbs and separates hydrogen chloride by bringing a reaction exhaust gas containing hydrogen into contact with an absorbing solution, and adsorbs and removes methane, hydrogen chloride, and chlorosilanes contained in the reaction exhaust gas containing hydrogen that has passed through the absorption device.
- Each of the activated carbon packed towers is an activated carbon in the activated carbon packed tower.
- As a discharge line for hydrogen gas as a carrier used at the time of life it has a first line for discharging out of the system, and a second line for once circulating out of the adsorption device and circulating to the adsorption device.
- the second line includes a chlorosilane condensation / separation unit, a gas compression unit, and hydrogen chloride.
- the absorption separation part is provided in this order.
- the hydrogen chloride absorption / separation unit may be the absorption device.
- the gas compression unit may be the compression device, and the absorption / separation unit may be the absorption device.
- the condensation separation part of the chlorosilanes may be the condensation separation apparatus, the gas compression part may be the compression apparatus, and the absorption separation part may be the absorption apparatus.
- the hydrogen gas separation and recovery method of the present invention is a method of separating and recovering hydrogen gas from reaction exhaust gas from an apparatus for producing polycrystalline silicon using trichlorosilane as a raw material, and using the hydrogen gas recovery system of the present invention.
- At least one of the plurality of activated carbon packed towers performs adsorption removal of the methane, hydrogen chloride, and chlorosilanes, and at the same time, activated carbon regeneration in another activated carbon packed tower is performed. It includes operations (1) and (2).
- the operation (1) is an operation of lowering the pressure in the activated carbon packed tower and exhausting the activated carbon adsorbate from the first line with the hydrogen carrier gas
- the operation (2) is the operation ( After 1), the discharge line is switched to the second line, the adsorption device is heated to raise the activated carbon temperature, hydrogen chloride and chlorosilanes are desorbed and discharged out of the adsorption device with a hydrogen carrier gas. Then, hydrogen chloride and chlorosilanes are recovered from the exhaust gas, and the hydrogen gas is circulated to the adsorption device.
- liquid chlorosilanes can be used as the absorbing liquid.
- the adsorbed component when the adsorbed component is desorbed and regenerated from the activated carbon in which the reaction exhaust gas in the activated carbon packed tower is brought into contact and the components other than hydrogen are adsorbed, hydrogen is used as a carrier gas and desorption is performed in two stages. That is, the component to be desorbed by reducing the pressure inside the tower by extracting the hydrogen gas from the activated carbon packed tower is discharged out of the system together with the hydrogen and the carrier gas sent into the tower, and then the carrier gas is sent. The line is switched, the activated carbon packed tower is heated to desorb hydrogen chloride and chlorosilanes, and hydrogen chloride and chlorosilanes are recovered and hydrogen as a carrier gas is purified and recovered.
- FIG. 1 is a flowchart for explaining each step of the exhaust gas separation and recovery method of the present invention
- FIG. 2 is a schematic diagram showing an example of the configuration of the exhaust gas separation and recovery system of the present invention.
- reaction exhaust gas from the polycrystalline silicon manufacturing apparatus (100) is supplied to the first condensing apparatus (10), and chlorosilane is condensed and separated (S101).
- This condensation and separation step is performed so that chlorosilanes do not liquefy in the first pressurizer (20) used in the compression step (S102) and damage the pressurizer (20). It is provided to reduce the thermal load in the step (S103), and is for removing (part of) chlorosilanes in advance prior to compression of the reaction exhaust gas.
- the reaction exhaust gas from the polycrystalline silicon manufacturing apparatus is cooled to remove a part of the chlorosilanes from the reaction exhaust gas.
- the cooling temperature should just be below the temperature which chlorosilanes do not condense under the pressure after compression in a compression process (S102). Accordingly, the cooling temperature may be ⁇ 10 ° C. or lower, preferably ⁇ 20 ° C. or lower.
- the reaction exhaust gas after passing through the condensation and separation step (S101) is sent to the compression step (S102).
- a pressurizer (20) for separating, purifying, and recycling the reaction exhaust gas is used in the compression step (S102).
- This pressurizer (20) provides mechanical and chemical durability to the reaction exhaust gas. It can be used as long as it can be safely operated and does not change the composition of the reaction exhaust gas.
- the reaction exhaust gas compressed and pressurized in the compression step (S102) contains unseparated chlorosilanes, hydrogen chloride, hydrogen, nitrogen, carbon monoxide, methane, and monosilane. Therefore, the chlorosilanes and hydrogen chloride contained in the reaction exhaust gas are absorbed into the absorption liquid in the hydrogen chloride absorption step (S103).
- An absorption liquid mainly composed of liquid chlorosilanes is supplied from the hydrogen chloride distillation apparatus (40) to the hydrogen chloride absorption apparatus (30), and the reaction exhaust gas comes into gas-liquid contact with the absorption liquid, thereby causing reaction in the reaction exhaust gas. Chlorosilanes and hydrogen chloride are absorbed by the absorbent.
- the hydrogen chloride absorber (30) As the hydrogen chloride absorber (30), a packed tower, a plate tower, a spray tower, a wet wall tower, etc. can be used. However, since the solubility of hydrogen chloride in chlorosilanes is not large, the gas-liquid is efficiently and continuously. It must be a device that can be contacted.
- the hydrogen chloride absorption step (S103) is preferably performed at a low temperature and a high pressure. Specifically, a temperature range of ⁇ 30 ° C. to ⁇ 60 ° C. and a pressure range of 0.4 MPaG to 1.0 MPaG are selected.
- the absorbing solution in which hydrogen chloride is dissolved is led from the hydrogen chloride absorbing device (30) to the hydrogen chloride distillation device (40), where hydrogen chloride gas is separated at a temperature of 50 ° C. to 140 ° C. (S104).
- the hydrogen chloride gas separated here is recovered as a tower top component and can be reused in a synthesis process of trichlorosilane, a conversion process of tetrachlorosilane to trichlorosilane, or the like.
- the absorption liquid after separation of hydrogen chloride gas is cooled to ⁇ 30 ° C. to ⁇ 60 ° C. and then sent to the hydrogen chloride absorption device (30), where it is used again as the absorption liquid in the hydrogen chloride absorption step (S103).
- the reaction exhaust gas from which chlorosilanes and hydrogen chloride have been removed by the hydrogen chloride absorption device (30) is introduced into the adsorption device (50), and purified hydrogen is recovered (S105).
- the adsorption device (50) used in this step is filled with activated carbon, and while the hydrogen-based gas passes through the activated carbon packed bed, unseparated chlorosilanes, hydrogen chloride, and nitrogen contained in the gas Carbon monoxide, methane, and monosilane are adsorbed on the activated carbon and removed from the gas to obtain purified hydrogen.
- the adsorption device (50) shown in FIG. 2 includes a plurality (three) of activated carbon packed columns (50a to c) so that one or more columns can always perform the adsorption step (S105). .
- Each of these activated carbon packed towers functions as an adsorption tower. By providing a plurality of activated carbon packed towers, while another activated carbon packed tower is performing heat desorption regeneration, the other activated carbon packed towers are in the adsorption step (S105). Can be performed.
- the procedure for heat desorption regeneration of the activated carbon packed tower is performed in two stages as follows. First, the activated carbon packed tower to be heated and desorbed and regenerated is depressurized. This is because desorption proceeds more advantageously under low pressure conditions, and the pressure is reduced to 0.03 MPa or less. Following this pressure reduction, when a part of the hydrogen recovered by the adsorption device (50) is passed through the target activated carbon packed tower as a regeneration carrier gas, impurities such as nitrogen, carbon monoxide, methane, and monosilane are present. Discharged. Hydrogen containing these impurities is discharged out of the system. Of course, this hydrogen may be regenerated by a separate hydrogen purification / recovery line other than those described later.
- the activated carbon packed tower is heated from 140 ° C to 170 ° C.
- hydrogen chloride, chlorosilanes, and the like are desorbed from the surface of the activated carbon and are driven out of the activated carbon packed tower by hydrogen as a carrier gas to complete regeneration of the activated carbon.
- hydrogen containing hydrogen chloride and the like is recovered and purified as described later.
- regeneration can be again used as an active adsorption tower only by cooling and pressurizing to the temperature and pressure at the time of adsorption
- Each of the activated carbon packed towers (50a to 50c) is a discharge line (the first line) for discharging the desorption gas (impurities such as nitrogen, carbon monoxide, methane, monosilane) generated during the pressure reduction in the above-described activated carbon regeneration step.
- the desorption gas (hydrogen chloride and chlorosilanes) generated during the regeneration of the activated carbon that is executed following the above-mentioned pressure reduction are once discharged out of the adsorption device (50) and then recirculated to the adsorption device (50). 2, in FIG.
- a second condensing device (60) that is a condensation / separation part of chlorosilanes and a second pressurizer that is a gas compression part (70) and a second hydrogen chloride absorption device (90) which is an absorption separation part of hydrogen chloride are provided in this order.
- Each of the activated carbon packed towers has a function of selecting whether the hydrogen gas (exhaust gas containing) is sent to the first line or the second line.
- the above switching can be managed not by temperature but by the time from the start of regeneration. Therefore, the above-described two stages in the heat desorption regeneration of the activated carbon packed tower are a stage of selecting a discharge line for discharging the gas discharged from the packed tower according to the state of the activated carbon to the outside of the system, and hydrogen chloride. And after the process which collect
- the hydrogen gas recovery system of the present invention may have, for example, the mode illustrated in FIGS. 3 to 6 in addition to the mode illustrated in FIG.
- the first condensing device (10) is used as the condensing / separating unit for chlorosilanes
- the first pressurizer (20) is used as the gas compressing unit
- the hydrogen chloride absorbing device (30) is used as the absorbing / separating unit. ing. Accordingly, the desorption gas (hydrogen chloride and chlorosilanes) generated during the regeneration of the activated carbon discharged to the outside of the adsorption device (50) is removed from the first condensing device (10) and the first addition device provided in the second line. It will circulate through the pressure device (20) and the hydrogen chloride absorption device (30) sequentially to the adsorption device (50) again.
- the second condensing device (60) is used as the condensing / separating unit for chlorosilanes
- the first pressurizer (20) is used as the gas compressing unit
- the hydrogen chloride absorbing device (30) is used as the absorbing / separating unit. ing. Therefore, the desorption gas (hydrogen chloride and chlorosilanes) generated during the regeneration of the activated carbon discharged to the outside of the adsorption device (50) is discharged from the second condensing device (60) and the first addition device provided in the second line. It will circulate through the pressure device (20) and the hydrogen chloride absorption device (30) sequentially to the adsorption device (50) again.
- the second condensing device (60) is used as the condensing / separating unit for chlorosilanes
- the second pressurizer (70) is used as the gas compressing unit
- the hydrogen chloride absorbing device (30) is used as the absorbing / separating unit. ing. Accordingly, the desorption gas (hydrogen chloride and chlorosilanes) generated during the regeneration of the activated carbon discharged to the outside of the adsorption device (50) is removed from the second condensing device (60) and the second addition gas provided in the second line. It will circulate through the pressure device (70) and the hydrogen chloride absorption device (30) sequentially to the adsorption device (50) again.
- the third condenser (80) is provided between the second pressurizer (70) and the hydrogen chloride absorber (30) in the embodiment shown in FIG.
- separation of hydrogen chloride and chlorosilanes from other impurity components can be achieved only by adopting a simple configuration of separating the path of the desorption gas generated at the time of depressurization in the activated carbon regeneration step and the desorption gas generated at the time of heating the activated carbon. The reason is as follows.
- the adsorption state of each component on the activated carbon surface can be estimated from the relationship between the adsorption temperature (denoted as T ad ) and the critical temperature (T c ) of each component, and is as follows. Liquid: T ad ⁇ T c Liquid + compressed gas: T ad ⁇ T c Compressed gas: T ad > T c
- the adsorption state of the adsorption gas component of the adsorption tower on the activated carbon surface is as follows.
- nitrogen, carbon monoxide, methane, and monosilane are components that can be easily desorbed by reducing the pressure below the pressure during adsorption without requiring heat of vaporization because the adsorption state is compressed gas.
- hydrogen chloride and chlorosilanes are adsorbed in a liquid state, and it is necessary to give heat of vaporization during desorption.
- the activated carbon packed tower repeats the high-pressure / low-temperature adsorption process and the low-pressure / high-temperature regeneration process.
- the pressure reduction usually takes a short time.
- it takes a long time to raise the temperature by heating. This is because the packed bed of activated carbon has a low thermal conductivity and a large heat capacity.
- the desorption gas in the pressure reduction stage at the initial stage of the regeneration process containing impurities such as nitrogen, carbon monoxide, methane, and monosilane is released out of the system, while the desorption gas in the heat regeneration stage containing hydrogen chloride and chlorosilanes is released.
- a third condensing device (80) may be provided to increase the degree of condensation.
- the recovered hydrogen purified in the adsorption step (S105) is sent to the polycrystalline silicon production apparatus (100) through the circulation pipe and reused.
- This purified hydrogen does not contain boron chloride, phosphorus, arsenic, carbon compounds, etc., which are harmful impurities when incorporated into silicon crystals as well as hydrogen chloride, and has sufficient purity for producing high-purity polycrystalline silicon. Have.
- the compression step (S102) and the hydrogen chloride absorption step (S103) are provided after the condensation separation step (S101) for separating chlorosilanes. This is because hydrogen chloride is more easily absorbed at lower temperatures and higher pressures, but such low-temperature and high-pressure conditions are also suitable for condensation of chlorosilanes. (30) When passing through the interior, chlorosilanes are simultaneously separated and removed.
- the regeneration carrier gas can be reduced. It is also advantageous for reducing the amount of use.
- the pressure of the reaction exhaust gas recovery system is the polycrystalline silicon that is the cause of pressure increase.
- the amount of by-product hydrogen in the production equipment, the amount of exhaust gas outside the reaction exhaust gas recovery system that is the cause of pressure drop, the amount of hydrogen consumed in the polycrystalline silicon production equipment, dissolved in the chlorosilane solution and discharged out of the system Determined by the amount of hydrogen.
- the hydrogen gas can be taken out of the system as surplus hydrogen, and the effective use of the tetrachlorosilane to the trichlorosilane conversion device (200) is also possible. It becomes possible.
- the balance is negative, it is necessary to replenish high-purity hydrogen gas from outside the system as make-up hydrogen.
- the reaction temperature in the polycrystalline silicon production apparatus is 1060 ° C.
- the feed gas is 520 Nm 3 / hr of hydrogen and 1,150 kg / hr of trichlorosilane.
- the discharge amount of each component of the reaction exhaust gas is as shown in Table 2.
- the temperature of the condensation / separation step (S101) is ⁇ 20 ° C.
- the temperature in the hydrogen chloride absorption step (S103) is ⁇ 40 ° C. and the pressure is 0.8 MPa.
- the temperature of the adsorption step (S105) was 30 ° C.
- the pressure was 0.8 MPa
- the amount of hydrogen as a carrier gas used for regeneration was 62 Nm 3 / hr in terms of time average flow rate.
- the temperature in the second condensation step (S106) was ⁇ 40 ° C., and the desorption gas was discharged out of the system only for the initial 2 hours during regeneration.
- hydrogen purified by separating hydrogen chloride, chlorosilanes, and other trace impurities contained in the reaction exhaust gas generated from the production process of polycrystalline silicon using trichlorosilane as a raw material It is possible to minimize hydrogen to be supplied to the circulation system and hydrogen released to the outside of the system when the gas is recycled.
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Abstract
Description
HSiCl3 + H2 → Si + 3HCl ・・・(式1)
HSiCl3 + HCl → SiCl4 + H2 ・・・(式2)
液体: Tad<<Tc
液体+圧縮気体: Tad≒Tc
圧縮気体: Tad>Tc
実施例
20 第1加圧器
30 塩化水素吸収装置
40 塩化水素蒸留装置
50 吸着装置
60 第2凝縮装置
70 第2加圧器
80 第3凝縮装置
90 第2塩化水素吸収装置
100 多結晶シリコン製造装置
200 テトラクロロシランのトリクロロシランへの転換装置
Claims (6)
- トリクロロシランを原料として多結晶シリコンを製造する装置からの反応排ガスから水素ガスを分離回収するために用いる水素ガス回収システムであって、
多結晶シリコン製造工程からの、水素を含む反応排ガスからクロロシラン類を凝縮分離する凝縮分離装置と、
前記凝縮分離装置を経た、水素を含む反応排ガスを圧縮する圧縮装置と、
前記圧縮装置を経た、水素を含む反応排ガスを吸収液と接触させて塩化水素を吸収分離する吸収装置と、
前記吸収装置を経た、水素を含む反応排ガスに含まれる、メタン、塩化水素、およびクロロシラン類を吸着除去するための複数の活性炭充填塔からなる吸着装置を備え、
前記活性炭充填塔のそれぞれは、該活性炭充填塔内での活性炭再生時に用いるキャリアとしての水素ガスの排出ラインとして、系外に排出するための第1のラインと、前記吸着装置外に一旦排出した後に該吸着装置へと循環させる第2のラインとを有し、且つ、前記水素ガスを前記第1および第2のラインの何れに送るかを選択可能に構成されており、
前記第2のラインには、クロロシラン類の凝縮分離部とガス圧縮部と塩化水素の吸収分離部がこの順で設けられていることを特徴とする水素ガス回収システム。 - 前記塩化水素の吸収分離部は前記吸収装置である、請求項1に記載の水素ガス回収システム。
- 前記ガス圧縮部は前記圧縮装置であり、前記吸収分離部は前記吸収装置である、請求項1に記載の水素ガス回収システム。
- 前記クロロシラン類の凝縮分離部は前記凝縮分離装置であり、前記ガス圧縮部は前記圧縮装置であり、前記吸収分離部は前記吸収装置である、請求項1に記載の水素ガス回収システム。
- トリクロロシランを原料として多結晶シリコンを製造する装置からの反応排ガスから水素ガスを分離回収する方法であって、
請求項1乃至4の何れか1項に記載の水素ガス回収システムを用い、前記複数の活性炭充填塔の少なくとも1つに前記メタン、塩化水素、およびクロロシラン類の吸着除去を実行させると同時に、他の活性炭充填塔内の活性炭再生を実行し、該活性炭再生は、下記の操作(1)および(2)を含むことを特徴とする水素ガスの分離回収方法。
操作(1):前記活性炭充填塔内の圧力を下げ、水素キャリアガスにより、活性炭吸着物を前記第1のラインより系外排気する操作、および
操作(2):操作(1)の後、前記排出ラインを前記第2のラインに切替え、前記吸着装置を加熱して活性炭温度を上昇させ、塩化水素およびクロロシラン類を脱着すると共に水素キャリアガスにより前記吸着装置外へと排出し、該排出ガスから塩化水素およびクロロシラン類の回収を行い、水素ガスは前記吸着装置へ循環させる操作。 - 前記吸収液として液状のクロロシラン類を用いる、請求項5に記載の水素ガスの分離回収方法。
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