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WO2010128743A1 - Réacteur vertical pour la production de silane et son emploi pour l'extraction de silane en continu - Google Patents

Réacteur vertical pour la production de silane et son emploi pour l'extraction de silane en continu Download PDF

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Publication number
WO2010128743A1
WO2010128743A1 PCT/KR2009/006928 KR2009006928W WO2010128743A1 WO 2010128743 A1 WO2010128743 A1 WO 2010128743A1 KR 2009006928 W KR2009006928 W KR 2009006928W WO 2010128743 A1 WO2010128743 A1 WO 2010128743A1
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Prior art keywords
reaction
silane
raw material
vertical reactor
temperature
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Ceased
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PCT/KR2009/006928
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English (en)
Korean (ko)
Inventor
뻬뜨로비치 엔도빈유리
발렌티노비치 뻬레르바올렉
니꼴라예브나 체크리엘레나
아르카지예비치 스토로젠코파벨
니꼴라예비치 폴리바노프알렉산드르
강경훈
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
KCC Corp
FSUE GNIICHTEOS
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KCC Corp
FSUE GNIICHTEOS
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Filing date
Publication date
Priority claimed from RU2009117349/05A external-priority patent/RU2414421C2/ru
Application filed by KCC Corp, FSUE GNIICHTEOS filed Critical KCC Corp
Publication of WO2010128743A1 publication Critical patent/WO2010128743A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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
    • C01B33/04—Hydrides of silicon
    • C01B33/043—Monosilane
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity

Definitions

  • the present invention relates to a vertical reactor for producing silane and a continuous recovery method of silane using the same.
  • MGS metallurgical silicon
  • the metal silicon is converted into volatile silicon compounds, and the volatile silicon compounds are subjected to various steps of purification, and then the purified volatile silicon compounds are recovered into semiconductor silicon.
  • a halogen compound of silicon such as silicon tetrahalide is produced in large quantities as a byproduct in the production of titanium, magnesium, and trichlorosilane.
  • fertilizer production generates a large amount of silicon tetrafluoride, which, if discarded as is, can cause great environmental problems, but when used in the recovery process of silicon, It can be usefully used as a cheap raw material.
  • Initial raw materials typically contain a mixture of various halides such as chloride, fluoride, free hydrogen halide, element impurities, moisture or oxygen in the silicon halide compound. Compound, etc.) and impurities in the metal hydride (eg, NaAlH 2 Et 2 ). Accordingly, reaction products may include byproducts such as hydrocarbons, hydrogen, and aluminum metal.
  • various halides such as chloride, fluoride, free hydrogen halide, element impurities, moisture or oxygen in the silicon halide compound. Compound, etc.
  • impurities in the metal hydride eg, NaAlH 2 Et 2
  • reaction products may include byproducts such as hydrocarbons, hydrogen, and aluminum metal.
  • US Pat. No. 4,632,816 discloses a method for recovering monosilane from excess metal hydride contained in one reactor.
  • the reaction apparatus may be rapidly contaminated due to the contamination by the metal halide containing hydrogen and the aluminum metal produced as a by-product thereof, thereby reducing the function of producing and recovering monosilane. have.
  • U.S. Patent No. 4,847,061 discloses a method for recovering monosilane in two reactors formed in the opposite direction to the movement of the reaction stream to reduce contamination by hydrogen containing metal halides.
  • this type of solution also has a problem that it does not completely solve the problem of contamination due to the metal halide containing hydrogen.
  • US Patent No. 5,075,092 discloses a method for the continuous recovery of monosilane through a prototype consisting of three devices.
  • the two reactors flow in the opposite direction to the reaction flow for ideal mixing, and the third reactor is designed to react in contact with several chemical reaction processes in the gas phase. This allows the third reactor to ideally mix the two processes and serve to separate the gas and liquid phases.
  • silicon halide is fed to the first reactor, and reacted with the remainder of the metal hydride to convert almost all of the silicon halide to monosilane.
  • a mixture comprising unreacted silicon halide and monosilane is fed to the second reactor.
  • the metal hydride is fed to the second reactor, reacted with the monosilane supplied from the first reactor, and then transferred to the first reactor for final release.
  • the stoichiometric ratio of the feed is adjusted by minimizing heat release inside the second reactor.
  • the stoichiometric ratio of the reactants approaches an approximation, and in particular, it is possible to prevent the metal halides which do not react with the metal hydrides from leaking in a contaminated state.
  • the second reactor in which excessive reaction of silicon halides and metal hydrides (there is no excess because both materials are used for almost 100% bonding), is a controlled reactor that stoichiometrically controls the feed of the mixing reactor and raw material reactants. Depending on the reaction characteristics in the mixing reactor, there may be raw materials remaining in the reaction product which are relatively small but not always able to react. Thus, an ideal mixing reactor equipped with a mechanical mixing device is provided. There is a problem in that it must be used.
  • the present invention was created in order to solve the above problems, and an object of the present invention is to perform a stoichiometric reaction for producing silane using silicon halide with only one reactor, and includes a reaction section including a plurality of reaction zones. At the stop, the silicon halide flowing from the bottom is reacted with the metal hydride flowing from the top to produce monosilane and metal halides, and the monosilane and metal halides generated are continuously separated and recovered to the upper and lower outlets, respectively. It is to provide a vertical reactor for producing silane and a continuous recovery method of silane using the same.
  • a device comprising: a reaction unit including a plurality of reaction zones in which a first raw material in a liquid phase including a metal hydride and a second raw material in a gas phase including silicon halides are reacted; A first inlet formed on an upper side of the reaction part and introducing a first raw material into the reaction part; A second inlet formed on one side of the lower portion of the reaction part and introducing a second raw material into the reaction part; A first outlet formed at an upper end of the reaction part and discharging silane gas generated in the reaction part; And a second outlet formed at a lower end of the reaction part and discharging the liquid metal halide generated in the reaction part.
  • the present invention provides a continuous recovery method of silane to recover the silane using a vertical reactor for producing silane according to the present invention.
  • the process since the process is performed using only one reactor, the process can be simplified, the connection part can be shortened, the loss due to the movement of the initial reaction product can be reduced, and the derived reaction product can be efficiently used. As a result, production costs can be greatly reduced.
  • FIG. 1 schematically illustrates a vertical reactor for producing silane according to an embodiment of the present invention and a method for recovering monosilane from silicon halide using metal hydride using the same.
  • the present invention comprises: a reaction part including a plurality of reaction zones in which a first raw material in a liquid phase including a metal hydride and a second raw material in a gas phase including silicon halides are reacted; A first inlet formed on an upper side of the reaction part and introducing a first raw material into the reaction part; A second inlet formed on one side of the lower portion of the reaction part and introducing a second raw material into the reaction part; A first outlet formed at an upper end of the reaction part and discharging silane gas generated in the reaction part; And a second outlet formed at a lower end of the reaction part to discharge the liquid metal halide produced in the reaction part.
  • the silane manufacturing vertical reactor 100 introduces a liquid metal hydride into the upper portion of the reaction unit 110 through the first inlet 120, and the second inlet 130.
  • the gaseous silicon halide is introduced into the lower portion of the reaction unit 110 through the.
  • the term "vertical reactor” refers to a reactor in which a reaction part is formed along a vertical direction, and the shape and shape thereof are not particularly limited.
  • the vertical reactor may have a relatively long height compared to the diameter.
  • the branch may be a column-type reactor.
  • reaction zone is not particularly limited, but may include, for example, a reaction rack formed so that the first liquid of the introduced liquid phase reacts for a predetermined time and then overflows.
  • reaction shelf is a contact type device to prevent the accumulation of solids
  • liquid phase ex. NaAlH 4 solution
  • gaseous compound ex. SiF 4
  • the metal halide (ex. NaAlF 4 ) generated through the reaction with the liquid metal hydride (ex. NaAlH 4 ) may have a slurry form, and the metal halide in the slurry form may not accumulate. It may be configured to flow over the outside of the reaction shelf so as not to.
  • reaction unit may further include a liquid transport device, thereby allowing a smoother flow.
  • the reaction unit includes a plurality of reaction zones for reacting the first raw material and the second raw material to generate the high value-added monosilane and the metal halide generated as all the reactions are performed at the stop of the reaction part. If the separation can be recovered, and the number of stages is not particularly limited, for example, the reaction zone may be formed in three to 30 stages in the vertical direction from the top to the bottom.
  • the reaction part includes a plurality of reaction zones so that the first raw material of the liquid phase and the second raw material of the gaseous phase respectively introduced into the upper part and the lower part of the reaction part can perform the reaction at various heights along the vertical direction. I can regulate it.
  • reaction zone when the reaction zone is formed in less than three stages, it may be difficult to control the reaction so that the reaction occurs mainly at the stop of the reaction portion, and if it exceeds 30 stages, there is a fear that the efficiency is reduced due to the excess equipment. .
  • reaction unit may further include a stirring device for mixing the first raw material and the second raw material introduced.
  • the stirring device serves to uniformly mix the first raw material and the second raw material so that sufficient contact can be made between the reacting raw materials, and the number thereof is not particularly limited. It can be installed separately for each reaction zone so that it can be mixed well, and one stirring device can be installed to operate simultaneously with blades for each reaction zone.
  • the form of the stirring device is not particularly limited, but, for example, the first raw material and the second inside of the reaction unit are attached to the stirring shaft and the stirring shaft formed along the vertical direction from the upper part to the lower part of the reaction part. It may be to include at least one blade for mixing the raw materials. That is, in the stirring device as described above, as the stirring shaft rotates, the blade attached to the stirring shaft rotates along the stirring shaft to uniformly mix the raw materials in the reaction unit, and the blade may be provided in each reaction zone. have.
  • the vertical reactor for producing silane according to the present invention may further include a heat sensing unit for measuring the temperature inside the reaction unit.
  • the heat sensing unit senses a temperature inside the reaction unit and measures a temperature to predict at which point the reaction occurs in the reaction unit. Accordingly, when the reaction unit includes at least two reaction zones, each reaction zone By measuring the heat of reaction in the reaction zone when the main reaction occurs in the reaction zone formed in the upper and lower portions of the reaction portion, it can be induced to occur in the middle portion of the reaction portion.
  • the heat sensing unit when the temperature of the inside of the reaction unit is measured by the heat sensing unit, when the heat of reaction in the reaction zone formed at the upper or lower portion of the reaction unit appears to be high, it flows into the first inlet or the second inlet to control this. Inflow of the first raw material and / or the second raw material can be controlled.
  • the main reaction when the main reaction appears in the reaction zone formed at the bottom of the reaction section, it means that the metal hydride is oversupplied and the main reaction occurs in the reaction zone on the lower side, thereby reducing the inflow of metal hydride or reducing the inflow of silicon halide. If the main reaction occurs in the reaction zone formed at the top of the reaction section, it means that the silicon halide is oversupplied, so that the inflow of silicon halide or the inflow of metal hydride can be increased.
  • the vertical reactor for producing silane according to the present invention may further include a heat exchanger for absorbing heat in the reaction zone or supplying heat to the reaction zone according to the temperature of the reaction zone measured by the heat sensing unit.
  • the heat exchanger serves to adjust the temperature in each reaction zone according to the temperature measured from the heat sensing unit.
  • the heat exchanger functions as a heat exchanger by adjusting the amount of raw material introduced according to the measured reaction heat. It may be possible, however, when the heat exchanger is further included, separate heating and cooling means may be used to adjust the temperature of the reaction zone.
  • the heat exchanger may include all of heat exchangers that may be commonly used in the art, and may include, for example, a heating device for supplying heat to the reaction part and a cooling device for absorbing heat from the reaction part.
  • the vertical reactor for producing silane according to the present invention may further include a third inlet formed on one side of the lower part of the reaction part to re-introduce the liquid metal halide discharged through the second outlet into the reaction part.
  • the vertical reactor for producing silane according to the present invention includes the third inlet, the residue remaining in the liquid phase may be reintroduced through the third inlet so that the slurry remaining in the lower portion of the reaction portion is stagnant to cause precipitation. The flow can be smoothed to prevent it.
  • it may further include a pump unit for transferring the residue to the first inlet or the third inlet so that the liquid metal halide discharged through the second outlet to the reaction unit.
  • the material of the vertical reactor for producing silane according to the present invention is not particularly limited, but may be made of a material commonly used in the art, but may be made of a material such as carbon steel.
  • the vertical reactor for producing silane according to the present invention does not need to move gas and liquid to another device because the reaction is performed in one device, so that a compressor or a pump may not be used.
  • first step and the second step are not specified in a time-series order, but may be performed simultaneously, respectively, and the time-series propagation relationship is not greatly limited.
  • the first step is a step of introducing a liquid first raw material containing a metal hydride through the first inlet to the upper portion of the reaction unit. That is, the liquid metal hydride is introduced into the reaction part through the first inlet formed in the upper part of the reaction part to react with the gaseous silicon halide introduced in the second step to be described later.
  • the type of the metal hydride used in the first step is not particularly limited, for example, it may be a compound represented by the following formula (1) or (2).
  • A is lithium, sodium or potassium.
  • the liquid metal hydride may include an alkali metal hydride (ex. NaH or LiH), or an aluminum hydride (LiAlH 4 , NaAlH 4 or KAlH 4 ).
  • the solvent may further include a hydrocarbon.
  • the type of the hydrocarbon is not particularly limited, and may include all hydrocarbons of various forms that may be used in admixture with ethers or cyclic ethers, but for example, one selected from the group consisting of toluene, toluene derivatives, and other hydrocarbon compounds. The above may be included, and more specifically, toluene, xylene, hexane, heptane and the like may be used.
  • any known method may be used to recover the solvent evaporating from the monosilane, for example using a dephlegmator or cold to reduce the loss of the solvent into the gaseous reaction product.
  • the cooled sodium aluminum hydride solution can be fed to the top of the device.
  • silicon halide is also not particularly limited in kind, for example, may be a compound represented by the following formula (3) or (4).
  • X and Y are each independently fluorine, chlorine or bromine, n is an integer of 1 to 4,
  • X is fluorine, chlorine or bromine, n is an integer of 1 to 3.
  • silicon halide may be SiF 4 , SiCl 4 , SiBr 4 , SiI 4 , and the like, and various halogens, such as SiBr 2 Cl 2 , SiF 2 Cl 2 , SiFCl 3 , EtSiF3, Et 2 SiF 2, and the like, may be used. Silicon halides in which organohalogenated silicon is mixed may be used.
  • the third step is a step of reacting the first raw material and the second raw material introduced into the reaction unit in the first step and the second step.
  • the reaction takes place mainly at the stop of the reaction section, and the monosilane and metal halides thus produced can be separately discharged to the top and the bottom, respectively.
  • the reaction contact time between the gaseous silicon halide in the reaction zone and the liquid metal hydride in each reaction zone prevents the increase of heat release in one reactor, and according to the object of the present invention, the main reaction is carried out at the stop of the reaction section to achieve high purity.
  • the monosilane and the metal halide can be controlled within an appropriate time range so as to separate and discharge, and are not particularly limited.
  • the pressure of the reaction unit in the third step is also not particularly limited, for example, can be carried out at atmospheric pressure (atmospheric pressure) or more, for example, a pressure of 1 atm (absolute) to 10 atm (absolute) It may be carried out under the conditions, specifically, it can be carried out under pressure conditions of 1.2 atm (absolute) to 1.4 atm (absolute).
  • the reaction may be carried out, for example, at a temperature of 10 ° C. to 110 ° C., specifically, in the case where the liquid metal hydride of the first step includes diethylene glycol dimethyl ether, 30 It may be carried out at a temperature of °C to 70 °C, more specifically, the pressure of the reaction unit may be carried out under the conditions of 1.2 atm (absolute), the temperature is 80 °C to 110 °C.
  • the load may be applied to the stirring device, when the reaction temperature exceeds 110 °C silicon halide to the solvent It may melt and react and vaporize as it is.
  • the third step the step of measuring the temperature of the reaction unit; And (2) controlling the inflow amount of the metal hydride and the silicon halide flowing into the reaction unit according to the temperature measured in the step (1).
  • the third step the step (A) of measuring the temperature of the reaction unit; And supplying or recovering heat to the reaction part according to the measured temperature.
  • the effects that can be obtained by controlling the inflow amount of the metal hydride and silicon halide flowing into the reaction part or supplying or recovering heat supplied to the reaction part by measuring the temperature inside the reaction part are as described above.
  • the cooling means for recovering heat from the reaction portion it is possible to cool the reaction portion using an external cooling flow (ex. In the form of rotating water), more specifically, the cooling means for each reaction zone
  • the temperature in the reaction zone can be adjusted so that the heat of reaction does not appear high at the top or bottom of the reaction section.
  • the fourth step in the present invention is the step of separating and discharging the silane gas and the liquid metal halide generated in the third step.
  • the silane gas and the liquid metal halide are generated through the third step, the gaseous silane is discharged through the upper part of the reaction part, and the liquid metal halide flowing down to the lower part of the reaction part reacts. Can be discharged through the bottom of the unit.
  • the continuous recovery method of the silane according to the present invention may further include the step of re-introducing the liquid metal halide discharged to the bottom of the reaction section to the top or bottom of the reaction section.
  • the reaction may be performed by reflowing the liquid metal halide in which the unreacted metal hydride remains to the upper part of the reaction part, or flowing into the lower part of the reaction part to facilitate the flow of the lower part of the reaction part. It may also provide flowability.
  • the gaseous silicon halide and the liquid metal hydride are reacted in the reaction unit 110 to generate a monosilane gas and a liquid metal halide
  • the monosilane gas is formed on the upper portion of the reaction unit 110. It can be discharged through the first outlet 140 (3).
  • the pump unit 170 After discharging the liquid metal halide to the second outlet 150 formed at the lower end of the reaction unit 110 by using the pump unit 170, it is recovered or to the outside of the reactor for the preparation of a new process thereafter. It may leak (4).
  • the residue of the liquid phase may be re-introduced through the third inlet 160 to facilitate the flow of the lower portion of the reaction unit (5), and the metal hydride that has not reacted in the residue may be used according to process requirements. By transferring the metal hydride to the upper portion of the reaction unit 110 so that the reaction can be carried out again (6).
  • silicon halides such as tetrafluoro silane can react with the liquid metal hydride while uniformly passing through all the reaction zones from the lower part of the reaction part to the upper part.
  • the monosilane gas may be discharged through the first outlet formed at the top of the reaction unit.
  • the monosilane discharged accordingly is a high-purity monosilane containing almost no impurities, and can be usefully used, and an extremely small amount of impurities contained in the monosilane gas can be purified through an additional purification process if necessary. have.
  • the metal hydride (ex. NaAlH 4 ) solution dissolved in the hydrocarbon or ether solvent passes through all the reaction zones uniformly through the first inlet formed on the upper side of the reaction part, and almost all of them are converted into metal halides. Some trace metal hydride may be collected at the bottom of the reaction section.
  • the reaction product in a gaseous state is separated from the lower part of the reaction part, and the liquid part may be discharged to the outside through a second outlet formed at the bottom of the reaction part through a pump part for later processing or recovery.
  • the residue of the liquid phase discharged from the vertical reactor for producing silane according to the present invention may be discharged at an appropriate speed within a range in which a certain amount of liquid can be maintained at the bottom of the apparatus.
  • the outflow rate of the liquid is too slow may precipitate the solid phase, in order to prevent the precipitation of the solid phase may be further provided with a separate stirring device at the bottom of the reactor.
  • the reaction is first started by dissolving the introduced silicon halide in the solvent of the metal hydride, and then reacting with the metal hydride, which is not established, that is, at the initial reaction start-up There is a fear that the silicon halide and the metal hydride may not completely complete the reaction.
  • the silicon halide flowing from the second inlet formed at the lower side of the reaction unit may be introduced into the first inlet formed at the upper side of the reaction unit by using the pump unit, thereby reducing the loss of reactants due to the insufficient initial reaction conditions.
  • the continuous recovery method of silane according to the present invention such a process may be performed until the reactor is operated normally.
  • the stoichiometric relationship of the sample is destroyed, it can be adjusted to change the amount of raw material flowing into the reaction part or to control the reaction at the stop part of the reaction part by controlling the heat of reaction using a heat exchanger or the like. have.
  • Hydrogenation exothermic reaction of silicon halide proceeds in the reaction section, and a large amount of heat is released, and in particular, various cooling means known in the art may be applied to remove the reaction heat of each reaction section.
  • the cooling means may be arranged on one side of the reaction part to adjust the cooling flow flowing into the cooling means while controlling the temperature of each reaction zone.
  • the method of controlling the emission of the heat of reaction and controlling the main reaction zone to occur at the stop of the reaction section may vary, for example, the stoichiometric reaction can be secured using the following two methods.
  • a proper amount of cooling liquid can be supplied to the reaction unit so that the preset temperature is maintained accurately.
  • Such a cooling liquid is supplied sufficiently so that a given device does not exceed the maximum hot spot temperature, and the resulting temperature change graph shows how the reaction is flowing inside the reaction part according to the height of the reaction part, and the current device. Show where the reaction is concentrated.
  • the temperature of the reaction section can be controlled by changing the cooling liquid consumption regardless of the excess capacity of the reaction section.
  • the enthalpy of the cooling liquid at the outlet and inlet of the reactor is controlled in each reaction zone.
  • the graph of the change in heat emission in each reaction zone located along the height of the reactor allows you to determine how the reaction is flowing and what part of the reactor is currently concentrated.
  • heat carriers may be used as the cooling liquid; Preferably water can be used.
  • reaction temperature is maintained in the range of approximately 10 °C to 80 °C under a reaction pressure of 1 atm (absolute) to 1.2 atm (absolute), when using a monosilane or a compound having a boiling point similar to monosilane as a solvent, 20 It can hold
  • the reaction temperature can be maintained between 30 °C and 70 °C.
  • the pressure is increased to 10 atm (absolute)
  • the heat of reaction rises in proportion to the vapor density pressure of the solvent, but cannot exceed 110 ° C.
  • a heat exchanger may be installed that condenses and recovers the vaporized solvent at temperatures above the lowest permissible temperature of the process (not more than 10 ° C.).
  • Such heat exchangers can be considered to manage spatial placement in the main reaction zones within the reactor, and the installation of heat exchangers can control the rate of reaction. For example, when the reaction is slow (when the reaction temperature is low), the heater can be heated to increase the reaction rate or cool down to reduce the reaction rate.
  • the reaction section of the reactor ensures effective contact between the gas and the liquid, and at the same time any form known as long as it can accommodate the required amount of liquid in the reaction section.
  • loss of gas flow energy can occur. That is, for example, when using a reactor to react a small amount of reactants in a low power device, the gas flow energy is not sufficient to maintain the device size.
  • silicon halides may be introduced into the reaction section to produce metal halides of the same type as Na 2 SiF 6 and to reduce the addition reactions that lead to loss of raw materials with the generation of waste. Not all of the silicon halides are introduced through the bottom of the apparatus, but may be introduced through inlets separated into several parts by height.
  • the number of additional inlets of silicon halide introduced into the reaction unit may be 2 to 5, specifically 1 or 2 inlets may be further formed.
  • the amount of silicon halide flowing into the lower part of the reaction part may be 25 parts by weight to 40 parts by weight based on 100 parts by weight of total silicon halide flowing into the reaction part, and the excess may be additionally introduced through another inlet formed at one side of the reaction part.
  • the amount of silicon halide (extra amount of silicon halide) introduced into the device A separately without flowing through the bottom may be 10% to 80% based on 100 parts by weight of the total silicon halide as described above. Can be.
  • the initial sample flow does not need to be purified metal hydride and silicon halide, it is possible to recover monosilane and metal halide using various mixtures composed of various components.
  • the reactor was installed as described above, and the sodium aluminum hydride solution was supplied at a composition ratio as shown in Table 1 below.
  • tetrafluoro silane gas was supplied in an amount of 2.88 kg / hr through the lower one side of the reaction unit.
  • the process was carried out in a continuous manner at a temperature of 20 ° C. and a pressure of 1.1 atm (absolute), and at the same time, the reaction mixture of Table 2 as a gas product was recovered through the top of the reaction section.
  • the slurry containing the metal fluoride was continuously discharged through the bottom of the apparatus to the ingredients and contents shown in Table 3 below.
  • the initial concentration of the sodium aluminum hydride was adjusted to 8.6% by weight.
  • the toluene solution containing the same industrial sodium aluminum hydride as Example 1 was mixed with an ethylene glycol dimethyl ether (monoglyme / dimethoxyethane) solvent and used as a first raw material containing metal hydride.
  • Example 1 purified tetrafluoro silicon was used, while in Example 2, contaminated conventional industrial impurities were chlorine hydride, fluorine hydride, hexafluoro. Tetrafluorosilicon containing disiloxane and a small amount of water was used.
  • the reactor was used in the same manner as in Example 1, and the sodium aluminum hydride solution was supplied in the composition ratio as shown in Table 4.
  • composition ratio of the tetrafluoro silane (silicon tetrafluoride / silicon tetrafluoride) in the gas form flowing into the bottom of the device is shown in Table 5.
  • the process was carried out under a temperature of 60 ° C. and a pressure of 1.2 atm (absolute), through which a reaction product in gaseous form was produced with the components and contents shown in Table 6 below.
  • Example 1 due to the high pressure and high temperature process of saturated steam monosilane compared with the case of using diethylene glycol dimethyl ether, together with the reaction product in gaseous form under the conditions described above The loss of solvent was great.
  • the slurry containing the metal halide was continuously discharged at the bottom of the apparatus, and the amount is shown in Table 7 below.

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Abstract

Réacteur vertical pour la production de silane et son emploi pour l'extraction de silane en continu. Cette invention permet d'isoler et d'extraire du silane et des halogénures de métal d'une grande pureté produits séquentiellement par la réaction d'un hydrure de métal liquide tel qu'un hydrure de sodium aluminium (NaAlH4) avec un halogénure de silicium gazeux tel qu'un tétrafluorure de silicium (SiF4)dans un seul et même réacteur. L'invention permet d'ajuster automatiquement le rapport stoïchiométrique des composants entrant dans la réaction, d'isoler et d'évacuer un composé initial ne participant pas à la réaction afin d'empêcher qu'il ne soit introduit dans le produit de réaction, et d'ajuster en permanence la température interne de l'unité de réaction pour que les processus se déroulent de façon stoïchiométrique.
PCT/KR2009/006928 2009-05-07 2009-11-24 Réacteur vertical pour la production de silane et son emploi pour l'extraction de silane en continu Ceased WO2010128743A1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
RU2009117349 2009-05-07
RU2009117349/05A RU2414421C2 (ru) 2009-05-07 2009-05-07 Способ непрерывного получения моносилана
KR1020090098481A KR101101972B1 (ko) 2009-05-07 2009-10-15 실란 제조용 수직형 반응기 및 이를 이용한 실란의 연속적 회수방법
KR10-2009-0098481 2009-10-15

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WO2010128743A1 true WO2010128743A1 (fr) 2010-11-11

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09194489A (ja) * 1996-01-12 1997-07-29 Shin Etsu Chem Co Ltd シラン類の製造方法
JP2003012677A (ja) * 2001-02-26 2003-01-15 General Electric Co <Ge> シラン中に炭素−ケイ素結合を形成する方法及び装置
US20080095691A1 (en) * 2004-09-17 2008-04-24 Degussa Gmbh Apparatus and Process for Preparing Silanes
US20080319214A1 (en) * 2007-06-20 2008-12-25 Wacker Chemie Ag Process For Preparing Si-H-Containing Silanes

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09194489A (ja) * 1996-01-12 1997-07-29 Shin Etsu Chem Co Ltd シラン類の製造方法
JP2003012677A (ja) * 2001-02-26 2003-01-15 General Electric Co <Ge> シラン中に炭素−ケイ素結合を形成する方法及び装置
US20080095691A1 (en) * 2004-09-17 2008-04-24 Degussa Gmbh Apparatus and Process for Preparing Silanes
US20080319214A1 (en) * 2007-06-20 2008-12-25 Wacker Chemie Ag Process For Preparing Si-H-Containing Silanes

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