WO2011025091A1 - Procédé de purification d'hydrogène à très haute pureté - Google Patents

Procédé de purification d'hydrogène à très haute pureté Download PDF

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Publication number
WO2011025091A1
WO2011025091A1 PCT/KR2009/006926 KR2009006926W WO2011025091A1 WO 2011025091 A1 WO2011025091 A1 WO 2011025091A1 KR 2009006926 W KR2009006926 W KR 2009006926W WO 2011025091 A1 WO2011025091 A1 WO 2011025091A1
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Prior art keywords
hydrogen
adsorbent
impurities
purification
powder
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PCT/KR2009/006926
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English (en)
Korean (ko)
Inventor
아르카지예비치 스토로젠코파벨
그리고리예브나 슈토바올가
뻬뜨로비치 엔도빈유리
보리소비치 오신베체슬라브
강경훈
Original Assignee
주식회사 케이씨씨
에프에스유이 그니테오스
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Publication date
Priority claimed from RU2009132181/05A external-priority patent/RU2415075C1/ru
Application filed by 주식회사 케이씨씨, 에프에스유이 그니테오스 filed Critical 주식회사 케이씨씨
Publication of WO2011025091A1 publication Critical patent/WO2011025091A1/fr

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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
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/50—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
    • C01B3/56—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by contacting with solids; Regeneration of used solids
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C14/00—Alloys based on titanium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/10—Inorganic adsorbents
    • B01D2253/112—Metals or metal compounds not provided for in B01D2253/104 or B01D2253/106
    • B01D2253/1122—Metals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2256/00—Main component in the product gas stream after treatment
    • B01D2256/16—Hydrogen
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/10—Single element gases other than halogens
    • B01D2257/102—Nitrogen
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/55—Compounds of silicon, phosphorus, germanium or arsenic
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2259/00—Type of treatment
    • B01D2259/40—Further details for adsorption processes and devices
    • B01D2259/414—Further details for adsorption processes and devices using different types of adsorbents
    • B01D2259/4141—Further details for adsorption processes and devices using different types of adsorbents within a single bed
    • B01D2259/4145—Further details for adsorption processes and devices using different types of adsorbents within a single bed arranged in series
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
    • C01B2203/042—Purification by adsorption on solids
    • C01B2203/043—Regenerative adsorption process in two or more beds, one for adsorption, the other for regeneration
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
    • C01B2203/0465—Composition of the impurity

Definitions

  • the present invention relates to a high purity hydrogen purification method, and more particularly, to a hydrogen purification method for removing various impurities contained in hydrogen obtained through pyrolysis of silane.
  • Hydrogen generated through the reaction as described above may be reused in the silicon deposition process after the purification process, but if impurities remain at a certain concentration or more in the hydrogen, there is a fear that the quality of the semiconductor silicon.
  • the above method is a method of purifying industrial hydrogen used for hydrogenation and hydrocracking of petroleum derivatives, and the purified hydrogen is difficult to be applied to electronic engineering and electronic technology.
  • the low temperature method has a problem in that energy consumption is high and the hydrogen purification process is complicated to perform.
  • Such conventional methods may be easy to remove boron-containing impurities, but have a problem in that hydrogen of higher purity cannot be obtained by removing nitrogen or phosphorus impurities.
  • US Patent No. 4871524 discloses a method for removing boron-containing impurities and phosphorus-containing impurities from hydrogen by using activated carbon at a low temperature.
  • the present invention was created to solve the above-mentioned problems of the prior art, and an object of the present invention is to provide a high-purity hydrogen purification method for removing impurities such as boron, nitrogen, and phosphorus from hydrogen generated during pyrolysis of monosilane. .
  • the present invention as a means for solving the above problems, comprising the step of purifying by passing hydrogen containing impurities through a purifying bed filled with an adsorbent comprising at least one selected from the group consisting of magnesium, aluminum, titanium and titanium alloys. It provides a hydrogen purification method.
  • Hydrogen produced in the pyrolysis process of monosilane contains impurities such as boron, nitrogen, and phosphorus, and according to the present invention, the hydrogen containing impurities is passed through a purified bed filled with an adsorbent having excellent adsorption efficiency.
  • the phosphorus content is 10 ppb or less
  • the boron content is 10 ppb or less
  • the ethylene content is 1 ppm or less
  • the nitrogen content is reduced to 100 ppm or less. Hydrogen can be obtained.
  • the purification can be performed in a relatively easy temperature range without performing the purification in a cryogenic environment, there is an advantage in terms of energy efficiency.
  • FIG. 1 is a process schematic diagram schematically showing a process for performing a hydrogen purification method according to an embodiment of the present invention.
  • the present invention relates to a method for purifying hydrogen, comprising the step of purifying hydrogen containing impurities through a purifying bed filled with an adsorbent comprising at least one selected from the group consisting of magnesium, aluminum, titanium and titanium alloys.
  • the adsorbent packed in the purification layer to efficiently adsorb and remove various impurities contained in the hydrogen under easier process conditions to obtain a high purity hydrogen, as described above, the adsorbent, magnesium, At least one selected from the group consisting of aluminum, titanium and titanium alloys.
  • the adsorbent may be used by combining the above-described materials in various forms, and the use form is not particularly limited, but may include, for example, magnesium, aluminum, titanium, and titanium alloys. More specifically, magnesium, aluminum, a mixture of magnesium and aluminum, and a material in which titanium or a titanium alloy is mixed with the metal or the metal mixture may be used.
  • titanium is not particularly limited to form the titanium alloy, for example, it may contain one or more selected from the group consisting of iron, nickel, cobalt and the like.
  • composition of the metal and titanium alloy used as the adsorbent and the mixing ratio thereof are not particularly limited, and may be used in various compositions and mixing ratios, for example, the composition and mixing ratio of the components contained in hydrogen Various adjustments can be made depending on the composition and content of impurities.
  • the hydrogen purification method according to the present invention is also not particularly limited in the form of the adsorbent filled in the purification layer, for example, it may be made in the form of powder, chip, foil (foil) or sponge form, specifically It may be made in the form of a powder.
  • the size of the adsorbent is not particularly limited, and may be adjusted to an appropriate size according to various conditions such as use capacity and content of impurities contained in hydrogen to be supplied.
  • the adsorbent may be 0.1 ⁇ m to 5000 ⁇ m. It may be in the form of a powder having an average particle diameter of, specifically, may be in the form of a powder having an average particle diameter of 10 ⁇ m to 500 ⁇ m.
  • the adsorbent when the adsorbent is in the form of a powder having an average particle diameter of less than 0.1 ⁇ m, the hydrogen to be purified does not pass through the purification layer, or a flying phenomenon due to fine powder may occur, which may cause difficulties in the process, due to static electricity There is a risk of explosion.
  • the adsorbent when the adsorbent is in the form of a powder having an average particle diameter of more than 5000 ⁇ m, there is a fear that the effective surface area of the adsorbent is reduced by reducing the specific surface area of the adsorbent. It may be difficult.
  • the adsorbent having the form as described above may be filled in a constant reactor to form a purification layer.
  • the tablet layer filled with the adsorbent is not particularly limited in form, and may be composed of a fixed bed or a fluidized bed.
  • the adsorbent may be mixed and dispersed through stirring, and thus the mixture obtained may be filled in a tube through which hydrogen gas passes so as to react with impurities contained in hydrogen passing through the purification layer, thereby forming a fixed bed, It may be used in the form of a fluidized bed to further improve contact between the impurities and the adsorbent.
  • the impurities may include boron, phosphorus, nitrogen, and the like, and specifically, may include boron impurities, phosphorus impurities, nitrogen impurities, and other impurities such as ethylene, monosilane, and the like.
  • the boron impurity may include BH 3 and B 2 H 6, etc.
  • the nitrogen impurity may include N 2 , and the like
  • the phosphorous impurity may include PH 3 .
  • the adsorbent used in the present invention can be removed by solidifying the impurities contained in hydrogen (ex. Boron, nitrogen, phosphorus, ethylene, monosilane, etc.) with a metal carbide compound, as shown in Scheme 2 below.
  • the process conditions are not particularly limited at the time of purification, for example, the purification is 500 °C It may be carried out in a temperature range of to 1000 °C, specifically, may be carried out in a temperature range of 600 °C to 900 °C.
  • the hydrogen purification is carried out at a temperature range of less than 500 °C, the reaction rate of the impurities and the adsorbent is lowered, there is a fear that the removal efficiency of impurities relative to the process time is lowered, if carried out at a temperature range exceeding 1000 °C, It may be difficult to select a reaction vessel to be filled and there is a fear that the energy efficiency is lowered.
  • the hydrogen purification method according to the present invention it is possible to perform the purification process only under the conventional cryogenic temperature because it uses an adsorbent that can efficiently purify hydrogen at a temperature condition that is relatively easy to perform the purification process even if the purification is not performed under cryogenic temperatures. Compared to the case of using activated carbon as an adsorbent, it may have advantages in terms of energy efficiency.
  • the hydrogen purification method according to the present invention can easily separate the hydrogen gas and the impurities by solidifying the impurities as the purification process is performed within a relatively low energy consumption temperature range.
  • the amount of impurities that can be removed per hour through the hydrogen purification method according to the present invention is not particularly limited, and sufficient reaction is performed between the impurities and the adsorbent according to the object of the present invention, the impurities can be separated from the hydrogen gas Appropriate purification rates may be employed.
  • the pressure conditions at the time of purification are not particularly limited, for example, it can be carried out under air pressure, specifically, the purification can be carried out under pressure conditions of 1 atm to 10 atm.
  • the hydrogen purification method according to the present invention is a device capable of performing the process as described above, the type and configuration is not particularly limited, for example, it includes a grid for dispersing, an electric stove and a temperature controller This can be done using a device.
  • the lattice for dispersing means a hollow tube capable of filling metal powder and titanium alloy powder.
  • the lattice for dispersing may also be used as the term "refining layer tube or reactor," and the electric furnace may increase the temperature of the refining layer. Serves to supply heat.
  • a supply unit and a recovery unit through which hydrogen gas flows in and out may be provided at the top and bottom of the device, respectively.
  • the reactor provided inside the apparatus may be filled with the adsorbent as described above, and may supply hydrogen contaminated by micro impurities.
  • the temperature inside the reactor can be controlled within the temperature range of 500 °C to 1000 °C, and the purified hydrogen obtained by passing the hydrogen containing impurities through the purification layer can be discharged to the outlet provided in the upper portion of the device have.
  • the purified hydrogen may move to a waste heat recoverer at a high temperature to transfer heat to hydrogen including impurities present in the waste heat recoverer. Accordingly, hydrogen containing impurities heated by the purified hydrogen may be supplied into the reactor at a high temperature.
  • a more effective way to purify hydrogen from finely sized impurities is to use a fluidized bed reactor containing the adsorbent described above.
  • the size of the device is not particularly limited, but may be determined based on the amount and linear speed of the adsorbent, for example.
  • At least two or more reactors may be interconnected, and a device configured in the form of the above-described adsorbent may be used in the reactor.
  • chained devices in which at least two reactors are provided parallel to one another so as to carry out a continuous hydrogen purification operation.
  • the purification process may be performed several times using all the reactors, and in some reactors, the hydrogen gas is not supplied in a stopped state. Then, when a problem occurs in the reactor to perform the purification process, the reaction may be carried out continuously through the reactor in the air.
  • FIG. 1 is a process schematic diagram schematically showing a process of performing a hydrogen purification method according to an embodiment of the present invention.
  • the contaminated hydrogen may be transferred to a reactor by passing through a heat exchanger 50.
  • the reactor includes two first reactors 10 and 20 installed in parallel; And two second reactors 30, 40 also installed in parallel.
  • the first reactor (10, 20) is filled with at least one adsorbent selected from the group consisting of magnesium powder, aluminum powder, titanium powder and titanium alloy powder, the second reactor (30, 40), magnesium powder, Among one or more adsorbents selected from the group consisting of aluminum powder, titanium powder and titanium alloy powder, the same or different kinds of adsorbents as those charged in the first reactors 10 and 20 may be charged.
  • the contaminated hydrogen, heated to thermal temperature may be supplied to either one of the two first reactors 10 and 20 installed in parallel, or may be supplied to both sides as necessary.
  • Hydrogen may be supplied to another first reactor 20. Accordingly, while the purification process is performed to the first reactor 20, a process of regenerating the adsorbent in the other first reactor 10 may be performed to perform a continuous process.
  • the first purified hydrogen through the first reactors 10 and 20 may be supplied to the second reactors 30 and 40 to be secondarily purified.
  • the operating state of the second reactors 30 and 40 may be similar to that of the first reactors 10 and 20.
  • the primary and secondary purified hydrogen may be transferred to the filtration unit 60 to remove impurities of the metal powder, thereby obtaining high purity hydrogen.
  • the content of impurities contained in the purified hydrogen is 10 ppb or less, and boron 10 ppb so as to be suitable for the silicon deposition process. Or less, nitrogen may be removed below 100 ppm, more specifically phosphorus below 1 ppb, boron below 1 ppb, and nitrogen below 1 ppm.
  • Hydrogen purification used equipment equipped with a gas dispersion grid (reactor) having a height of 1000 mm and an inner diameter of 150 mm, a supply part, a recovery part, an electric stove, and a temperature controller.
  • a gas dispersion grid reactor having a height of 1000 mm and an inner diameter of 150 mm
  • a supply part a recovery part
  • an electric stove a temperature controller.
  • the reactor was filled with magnesium powder having a particle diameter of 10 ⁇ m to 200 ⁇ m with an adsorbent. Thereafter, by heating the hydrogen in the reactor for 3 hours using an electric stove, the temperature was raised to 700 °C. Hydrogen was passed through the purification layer to remove impurities under this temperature.
  • the pressure of the reactor was atmospheric pressure
  • the rate of hydrogen flow was 150 L (liter) / h (hour)
  • the gas (hydrogen) flow was analyzed every 50 hours.
  • Impurity content in hydrogen according to Example 1 is shown in Table 1.
  • Example 2 In the same manner as in Example 1, a powder mixture of magnesium powder and titanium powder in a ratio of 1: 4 was used as the adsorbent. At this time, the particle diameter of magnesium powder was 10 micrometers-500 micrometers, the particle diameter of aluminum powder was 70 micrometers-350 micrometers, and the internal temperature of the reactor was 500 degreeC.
  • Impurity content in hydrogen according to Example 2 is shown in Table 2.
  • Example 2 In the same manner as in Example 1, a powder mixture having a 1: 1 ratio of magnesium powder and titanium powder was used as an adsorbent. At this time, the particle diameter of magnesium powder was 70 micrometers-350 micrometers, the particle diameter of titanium powder was 20 micrometers-500 micrometers, and the internal temperature of the reactor was 850 degreeC.
  • Example 2 In the same manner as in Example 1, a powder mixture of magnesium powder and titanium alloy powder having a TiFe 2 formula of 1: 4 was used as the adsorbent. At this time, the particle size of the magnesium powder was 70 ⁇ m to 350 ⁇ m, the particle diameter of the titanium alloy powder was 20 ⁇ m to 500 ⁇ m, the internal temperature of the reactor was 850 °C.
  • Impurity content in hydrogen according to Example 4 is shown in Table 4.
  • the powder mixture was performed in the same manner as in Example 1 except that the titanium alloy powder containing magnesium powder and cobalt 5% as a sorbent was 1: 10. At this time, the particle size of the magnesium powder was 20 ⁇ m to 250 ⁇ m, the particle diameter of the titanium alloy powder was 20 ⁇ m to 500 ⁇ m, the internal temperature of the reactor was 1000 °C.
  • Impurity content in hydrogen according to Example 5 is shown in Table 5.
  • Example 2 The same method as in Example 1 was used, but an apparatus in which three reactors were structurally coupled in advance was used.
  • the adsorbent is a magnesium powder in the first reactor, a powder mixture in which the ratio of magnesium powder and titanium powder is 1: 4, and in the third reactor, the ratio of magnesium powder and titanium (TiFe2) alloy powder is 1: A powder mixture of 10 was used.
  • the particle size of the magnesium powder used in the first and / or second reactor was 70 ⁇ m to 350 ⁇ m
  • the particle size of the titanium powder was 20 ⁇ m to 500 ⁇ m
  • the particle size of the magnesium powder used in the third reactor was 20 ⁇ m to 250 ⁇ m.
  • the particle size of the titanium alloy powder was 20 ⁇ m to 500 ⁇ m.
  • the internal temperature of the first reactor was 650 ° C
  • the internal temperature of the second reactor was 750 ° C
  • the internal temperature of the third reactor was 900 ° C.
  • Impurity content in hydrogen according to Example 6 is shown in Table 6.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
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  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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Abstract

La présente invention concerne un procédé de purification d'hydrogène comprenant l'étape consistant à faire passer de l'hydrogène contenant des impuretés à travers une couche de purification dans laquelle est placé un adsorbant comprenant au moins un élément choisi dans le groupe constitué du magnésium, de l'aluminium, du titane et d'alliages de titane, ce qui permet ainsi de purifier ledit hydrogène. Selon la présente invention, l'hydrogène contenant des impuretés telles que bore, azote, phosphore, et analogues traverse une couche de purification dans laquelle est placé un adsorbant métallique spécifique, ce qui permet l'élimination plus efficace des impuretés, ainsi que la réduction de la consommation d'énergie inutile puisque la purification n'a pas besoin d'être effectuée à une température extrêmement basse.
PCT/KR2009/006926 2009-08-27 2009-11-24 Procédé de purification d'hydrogène à très haute pureté WO2011025091A1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
RU2009132181 2009-08-27
RU2009132181/05A RU2415075C1 (ru) 2009-08-27 2009-08-27 Способ глубокой очистки водорода
KR1020090098632A KR101101968B1 (ko) 2009-08-27 2009-10-16 고순도의 수소 정제 방법
KR10-2009-0098632 2009-10-16

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WO2011025091A1 true WO2011025091A1 (fr) 2011-03-03

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4749558A (en) * 1978-02-02 1988-06-07 Studiengesellschaft Kohle Mbh Method of separating and purifying hydrogen
KR20020013060A (ko) * 2000-08-10 2002-02-20 이택홍 수소 정제 방법 및 정제 장치
JP2005200252A (ja) * 2004-01-14 2005-07-28 Nippon Telegr & Teleph Corp <Ntt> 水素精製装置
US20060254425A1 (en) * 2002-12-24 2006-11-16 Baksh Mohamed Safdar A Process and apparatus for hydrogen purification

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4749558A (en) * 1978-02-02 1988-06-07 Studiengesellschaft Kohle Mbh Method of separating and purifying hydrogen
KR20020013060A (ko) * 2000-08-10 2002-02-20 이택홍 수소 정제 방법 및 정제 장치
US20060254425A1 (en) * 2002-12-24 2006-11-16 Baksh Mohamed Safdar A Process and apparatus for hydrogen purification
JP2005200252A (ja) * 2004-01-14 2005-07-28 Nippon Telegr & Teleph Corp <Ntt> 水素精製装置

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