CN115140709A - Method for producing germane by fluidization through plasma synthesis method - Google Patents

Method for producing germane by fluidization through plasma synthesis method Download PDF

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CN115140709A
CN115140709A CN202210736607.0A CN202210736607A CN115140709A CN 115140709 A CN115140709 A CN 115140709A CN 202210736607 A CN202210736607 A CN 202210736607A CN 115140709 A CN115140709 A CN 115140709A
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tower
germane
plasma
hydrogen
germanium
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栗鹏伟
潘海涛
齐相前
赵懿斌
王敏华
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Suzhou Jinhong Gas Co Ltd
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Suzhou Jinhong Gas Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B6/00Hydrides of metals including fully or partially hydrided metals, alloys or intermetallic compounds ; Compounds containing at least one metal-hydrogen bond, e.g. (GeH3)2S, SiH GeH; Monoborane or diborane; Addition complexes thereof
    • C01B6/06Hydrides of aluminium, gallium, indium, thallium, germanium, tin, lead, arsenic, antimony, bismuth or polonium; Monoborane; Diborane; Addition complexes thereof
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/087Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
    • B01J19/088Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges

Abstract

The invention discloses a method for producing germane by plasma fluidization.A hydrogen gas enters a plasma hydrogen generator to generate plasma hydrogen, and the plasma hydrogen enters a fluidized bed; carrying out fluidization reaction with germanium powder to generate germane; condensing the reaction material flow after gas phase pressurization, enabling the middle upper part of the condensate tower to enter a light component removing tower for removing light component impurities, enabling the tower kettle material to enter a heavy component removing tower from the middle lower part of the tower kettle material for removing heavy component impurities, and enabling germane with the purity not lower than 5N obtained at the tower top to enter a germane product tank. Light component impurities extracted from the top of the light component removal tower and heavy component impurities extracted from the bottom of the heavy component removal tower enter a tail gas combustor to be incinerated to produce germanium dioxide powder, then hydrogen is used for reduction to produce germanium powder, and the obtained germanium powder enters a germanium powder tank for recycling. The invention solves the problems of low germane production efficiency, generation of byproducts and waste water and the like at present, does not generate waste water and byproducts which are difficult to separate and treat, and has high reaction efficiency and high product purity.

Description

Method for producing germane by fluidization through plasma synthesis method
Technical Field
The invention belongs to the technical field of electronic special gas production, and particularly relates to a method for producing germane by fluidization through a plasma synthesis method.
Background
Germane, an inorganic compound with the molecular formula GeH 4 The molecular weight is 76.63, and the product is colorless toxic gas with unpleasant odor. Germane is used as an important raw material for manufacturing high-purity germanium and various silicon-germanium alloys, and is mainly used in the aspects of semiconductors, infrared technology and the like. With the rapid development of the semiconductor industry, the demand for germane has increased in quality and supply. At present, although China has enterprise production, the scale is small, the stability is poor, the purity is low, and the method becomes one of the bottlenecks restricting the development of the semiconductor industry in China.
Germane is generally synthesized by a chemical reduction method, an electrochemical reaction method, and a plasma synthesis method.
Chemical reduction processes are generally prepared by reducing germanides with simple and complex metal hydrides. Generally, germanium-magnesium alloy, germanium dioxide and germanium tetrachloride can be used as the germanium-containing reagent, and lithium hydride, potassium hydride, lithium borohydride, sodium borohydride, lithium aluminum hydride and diisobutylaluminum oxide can be used as the reducing agent. The reduction reaction is carried out in an aqueous solution or an inorganic solvent and an organic solvent.
The electrochemical reduction method uses germanium as a cathode and molybdenum or cadmium as an anode. During the reaction, the cathode produces gereman and hydrogen and the anode produces molybdenum or cadmium oxide.
Plasma synthesis bombards elemental germanium with hydrogen atoms (H) generated by a high frequency plasma source to provide various reaction products, such as germanes in various states, such as germyle and the like.
The chemical reduction method and the electrochemical reduction method still have some problems in the aspects of comprehensive cost, purification, conversion rate and the like, for example, the content of byproducts is high, a large amount of wastewater is generated in the process, impurities are not easy to separate, and the like, and the purification is difficult. The plasma synthesis method generally uses a germanium target as a germanium source, the germanium target is expensive, the reaction efficiency is low, other germane impurities are more, and the utilization rate of germanium is low.
Disclosure of Invention
In order to solve the technical problems, the invention discloses a method for producing germane by plasma fluidization, which solves the problems of low germane production efficiency, generation of byproducts and wastewater and the like at present, does not generate wastewater and byproducts which are difficult to separate and treat, and has high reaction efficiency and high product purity.
The technical scheme of the invention is as follows: a process for plasma fluidized production of germane having the steps of:
1) Hydrogen enters a plasma hydrogen generator to generate plasma hydrogen, and the plasma hydrogen enters a fluidized bed;
2) Enabling the germanium powder to enter a fluidized bed, and carrying out a fluidization reaction with plasma hydrogen in the fluidized bed to generate germane;
3) Removing solid germanium powder carried by gas and solid from the reactant flow in the step 2) through a cyclone separator, and enabling the solid germanium powder to enter a germanium powder tank and enter a returning bed for secondary reaction; the gas phase enters a booster compressor for boosting, and condensation is carried out after boosting; returning the non-condensable gas hydrogen which is not condensed back to the hydrogen buffer tank for recycling;
4) The middle upper material of the condensate tower enters a light component removing tower to remove light component impurities; the material at the bottom of the tower is extracted, the heavy component impurities are removed by entering a heavy component removing tower from the middle lower part; germane with the purity not lower than 5N is obtained at the tower top, and a germane product enters a germane product tank;
5) Light component impurities extracted from the top of the light component removal tower and heavy component impurities extracted from the bottom of the heavy component removal tower enter a tail gas combustor for incineration treatment; burning germane, digermane and the like to produce germanium dioxide powder; and (3) enabling the germanium dioxide powder to enter a germanium dioxide reduction furnace, producing germanium powder by using hydrogen reduction, and enabling the obtained germanium powder to enter a germanium powder tank for recycling.
Wherein, the hydrogen entering the plasma hydrogen generator in the step 1) is 0.2-3 Bar; the discharge frequency of the plasma generator is 5-100KHz, and the discharge voltage is 10-50KV. Preferably, the hydrogen entering the plasma hydrogen generator is 0.3-1 Bar; the discharge frequency of the plasma generator is 40-80KHz, and the discharge voltage is 20-30KV.
Wherein, in the step 2), the granularity of the germanium powder entering the fluidized bed is 80-400 meshes. Preferably, the granularity of the germanium powder entering the fluidized bed is 120-200 meshes. Germanium powder enters the fluidized bed from the middle upper part of the fluidized bed.
Wherein, in the step 3), the gas phase is pressurized to 10-30Bar in a booster compressor, and the condensation temperature is lower than-20 ℃ after pressurization. Preferably, the gas phase is pressurized to 15-20 Bar in a booster compressor, and the condensation temperature is lower than-25 to-30 ℃ after pressurization.
Wherein, in the step 4), the operating temperature of the light component removing tower is-20 to-45 ℃, and the operating pressure is 6.1 to 11.6Bar. Preferably, the operating temperature of the light component removal tower is-30 to-35 ℃, and the operating pressure is 8.5-10Bar.
Wherein, in the step 4), light component impurities such as hydrogen, nitrogen, carbon monoxide and methane are removed by the light component removal tower, and the extracted amount of the light component on the top of the tower accounts for 3-10% of the total amount of the materials. Preferably, the extraction amount of the light components of the light component removal tower accounts for 5-6% of the total amount of the materials.
Wherein, in the step 4), the operation temperature of the de-weighting tower is-30 to-50 ℃, and the operation pressure is 5.2 to 10Bar. Preferably, the operation temperature of the de-weighting tower is-35 to-40 ℃, and the operation pressure is 7.2 to 8.5Bar.
Wherein, in the step 4), the heavy component impurities such as digermane, digermane and the like are removed from the tower kettle by the de-heavy tower, and the extraction amount of the heavy component in the tower kettle accounts for 10 to 40 percent of the total amount of the materials. Preferably, the extraction amount of heavy components in the tower bottom accounts for 15-20% of the total amount of the materials.
Wherein, in the step 5), the temperature of incineration treatment is 500-900 ℃. Preferably 570-700 degrees celsius.
Wherein, in the step 5), the germanium powder is produced by reducing the hydrogen in a germanium dioxide reducing furnace at the temperature of 600-700 ℃ for 30-9 min. Preferably, hydrogen is used for reduction in a germanium dioxide reduction furnace to produce germanium powder, the temperature is 650-675 ℃, and the reduction time is 45-60 min.
The invention also provides a plasma synthesis reaction system which comprises a V01 hydrogen buffer tank, an X01 plasma hydrogen generator, an R01 fluidized bed reactor, an F01 cyclone separator, a V02 germanium powder tank, a C01 booster compressor, an E01 deep cooler, a T01 lightness-removing tower, a T02 heavy-removing tower, a V03 germane product tank, an R02 tail gas combustor and an R03 germanium dioxide reduction furnace.
Wherein, the communication and the mutual relation of the reaction system are that hydrogen firstly enters a plasma hydrogen generator to generate plasma hydrogen which enters a fluidized bed R01; the germanium powder also enters a fluidized bed R01, and is subjected to a fluidization reaction with plasma hydrogen in the fluidized bed to generate germane; the reactant flow of fluidized bed R01 removes the solid germanium powder that the gas-solid was smugglied secretly through cyclone F01, and solid germanium powder gets into germanium powder jar V02, goes back to the bed from this and reacts once more, and the gaseous phase gets into booster compressor C01 and carries out the pressure boost, and deep cooler E01 condenses after the pressure boost, and noncondensable gas hydrogen that does not condense down returns at hydrogen buffer tank V01, recycles. The middle upper part of the condensate tower enters a light component removing tower T01 for removing light component impurities, the material collected from the tower bottom enters a heavy component removing tower T02 for removing heavy component impurities, and the germane with the purity not lower than 5N is obtained from the tower top and enters a germane product tank. And light component impurities extracted from the top of the light component removal tower T01 and heavy component impurities extracted from the bottom of the heavy component removal tower T02 enter a tail gas combustor R02 to be incinerated, germane, digermane and the like are incinerated to produce germanium dioxide powder, the germanium dioxide powder enters a germanium dioxide reduction furnace R03 to be reduced by hydrogen to produce germanium powder, and the obtained germanium powder enters a germanium powder tank to be recycled.
The method for producing germane by plasma fluidization solves the problems of low germane production efficiency, generation of byproducts and waste water and the like at present, and does not generate waste water and byproducts which are difficult to separate and treat. Germanium is recycled after being treated by adopting germanium-containing impurities, so that the utilization rate of germanium is improved. The plasma synthesis reaction system adopted by the invention improves the reaction efficiency, and the obtained germane product has high purity.
Drawings
FIG. 1 is a schematic diagram of a plasma synthesis reaction system of the present invention, wherein V01 is a hydrogen buffer tank, X01 is a plasma hydrogen generator, R01 is a fluidized bed reactor, F01 is a cyclone separator, V02 is a germanium powder tank, C01 is a booster compressor, E01 is a deep cooler, T01 is a light component removal tower, T02 is a heavy component removal tower, V03 is a germane product tank, R02 is a tail gas combustor, and R03 is a germanium dioxide reduction furnace.
Detailed Description
The technical solution of the present invention will be further described with reference to the following specific examples, but the present invention is not limited to these examples.
A process for producing germane by plasma fluidization having the steps of:
1) Hydrogen enters a plasma hydrogen generator to generate plasma hydrogen, and the plasma hydrogen enters a fluidized bed;
2) Enabling germanium powder to enter the fluidized bed from the middle upper part of the fluidized bed, and carrying out a fluidization reaction with plasma hydrogen in the fluidized bed to generate germane;
3) Removing solid germanium powder carried by gas and solid from the reactant flow in the step 2) through a cyclone separator, and enabling the solid germanium powder to enter a germanium powder tank and enter a returning bed for secondary reaction; the gas phase enters a booster compressor for boosting, and condensation is carried out after boosting; returning the non-condensable gas hydrogen which is not condensed back to the hydrogen buffer tank for recycling;
4) The middle upper material of the condensate tower enters a light component removing tower to remove light component impurities; extracting materials at the bottom of the tower, and removing heavy component impurities in a heavy component removing tower from the middle lower part; germane with the purity not lower than 5N is obtained at the tower top, and a germane product enters a germane product tank;
5) Light component impurities extracted from the top of the light component removal tower and heavy component impurities extracted from the bottom of the heavy component removal tower enter a tail gas combustor to be incinerated; burning germane, digermane and the like to produce germanium dioxide powder; and (3) enabling the germanium dioxide powder to enter a germanium dioxide reduction furnace, producing germanium powder by using hydrogen reduction, and enabling the obtained germanium powder to enter a germanium powder tank for recycling.
Example 1
Hydrogen with 0.5Bar enters a plasma hydrogen generator, the discharge frequency of the plasma generator is 50KHz, the discharge voltage is 40KV, and the generated plasma hydrogen enters a fluidized bed R01; germanium powder with the granularity of 150 meshes enters the fluidized bed from the middle upper part of the fluidized bed, and the germane is generated by the fluidization reaction in the fluidized bed. The reactant flow is removed with solid germanium powder carried by gas and solid through a cyclone separator F01, the solid germanium powder enters a germanium powder tank V02, the reactant flow returns to the bed for reaction again, the gas phase enters a booster compressor C01 for boosting, the boosting is at 20bar, a booster aftercooler E01 carries out condensation, the condensation temperature is lower than-30, and the uncondensed gas hydrogen which is not condensed returns to a hydrogen buffer tank V01 for recycling. The middle upper part of the condensate tower enters a light component removal tower T01 to remove light component impurities, the operating temperature of the tower is-30 ℃, the operating pressure is 10Bar, the light component impurities of hydrogen, nitrogen, carbon monoxide and methane are thoroughly removed from the top of the tower, and the extracted amount of the light components at the top of the tower accounts for 5 percent of the total amount of the materials; extracting materials from the tower kettle, feeding the materials into a de-weighting tower T02 from the middle lower part for removing heavy component impurities, wherein the operating temperature of the tower is-35 ℃, the operating pressure is 8.5Bar, the heavy component impurities such as digermane, digermane and the like are completely removed from the tower kettle, and the extraction amount of the heavy components in the tower kettle accounts for 20 percent of the total amount of the materials; the germane with the purity not lower than 5N is obtained at the tower top, and the germane product enters a germane product tank.
Light component impurities extracted from the top of the light component removal tower T01 and heavy component impurities extracted from the bottom of the heavy component removal tower T02 enter a tail gas combustor R02 to be incinerated, and germane, digermane and the like are incinerated at the temperature of 600 ℃ to produce germanium dioxide powder. And (3) enabling the germanium dioxide powder to enter a germanium dioxide reduction furnace R03, reducing the germanium dioxide powder by using hydrogen to produce germanium powder, wherein the temperature is 650 ℃, the reduction time is 60min, and the obtained germanium powder enters a germanium powder tank for recycling.
Example 2
1Bar hydrogen enters a plasma hydrogen generator, the discharge frequency of the plasma generator is 60KHz, the discharge voltage is 60KV, and the generated plasma hydrogen enters a fluidized bed R01; germanium powder with the granularity of 200 meshes enters the fluidized bed from the middle upper part of the fluidized bed, and is subjected to a fluidization reaction with plasma hydrogen in the fluidized bed to generate germane. The reactant flow is removed with solid germanium powder carried by gas and solid through a cyclone separator F01, the solid germanium powder enters a germanium powder tank V02, the reactant flow returns to the bed for reaction again, the gas phase enters a booster compressor C01 for boosting, the boosting is at 20bar, a booster aftercooler E01 carries out condensation, the condensation temperature is lower than-30, and the uncondensed gas hydrogen which is not condensed returns to a hydrogen buffer tank V01 for recycling. The middle upper part of the condensate tower enters a lightness-removing tower T01 to remove light component impurities, the operating temperature of the tower is-30 ℃, the operating pressure is 10Bar, the light component impurities such as hydrogen, nitrogen, carbon monoxide and methane are thoroughly removed from the top of the tower, and the extracted amount of the light components at the top of the tower accounts for 5 percent of the total amount of materials; the material extracted from the tower kettle enters a de-heavy tower T02 from the middle lower part for removing heavy component impurities, the operating temperature of the tower is-35 ℃, the operating pressure is 8.5Bar, the heavy component impurities such as digermane, gerane and the like are completely removed from the tower kettle, and the extracted amount of the heavy component in the tower kettle accounts for 15 percent of the total amount of the material; the germane with the purity not lower than 5N is obtained at the tower top, and a germane product enters a germane product tank.
And (3) introducing light component impurities extracted from the top of the light component removal tower T01 and heavy component impurities extracted from the bottom of the heavy component removal tower T02 into a tail gas combustor R02 for incineration treatment, wherein the incineration temperature is 650 ℃, and incinerating germane, digermane and the like to produce germanium dioxide powder. And (3) enabling the germanium dioxide powder to enter a germanium dioxide reduction furnace R03, reducing the germanium dioxide powder by using hydrogen to produce germanium powder at the temperature of 675 for 50min, and enabling the obtained germanium powder to enter a germanium powder tank for recycling.
Example 3
Hydrogen of 0.8Bar enters a plasma hydrogen generator, the discharge frequency of the plasma generator is 60KHz, the discharge voltage is 50KV, and the generated plasma hydrogen enters a fluidized bed R01; germanium powder with the granularity of 200 meshes enters the fluidized bed from the middle upper part of the fluidized bed, and is subjected to a fluidization reaction with plasma hydrogen in the fluidized bed to generate germane. The reactant flow is removed with solid germanium powder carried by gas and solid through a cyclone separator F01, the solid germanium powder enters a germanium powder tank V02, the reactant flow returns to the bed for reaction again, the gas phase enters a booster compressor C01 for boosting, the boosting is at 15bar, a booster aftercooler E01 condenses, the condensation temperature is lower than-35, and the uncondensed gas hydrogen which is not condensed returns to a hydrogen buffer tank V01 for recycling. The middle upper part of the condensate tower enters a lightness-removing tower T01 to remove light component impurities, the operating temperature of the tower is-30 ℃, the operating pressure is 10Bar, the light component impurities such as hydrogen, nitrogen, carbon monoxide and methane are thoroughly removed from the top of the tower, and the extracted amount of the light components at the top of the tower accounts for 3 percent of the total amount of materials; the material extracted from the tower kettle enters a de-weighting tower T02 from the middle lower part to remove heavy component impurities, the operating temperature of the tower is-35 ℃, the operating pressure is 8.5Bar, the heavy component impurities such as digermane, digermane and the like are completely removed from the tower kettle, and the extracted amount of the heavy component in the tower kettle accounts for 25 percent of the total amount of the material; the germane with the purity not lower than 5N is obtained at the tower top, and the germane product enters a germane product tank.
And (3) introducing light component impurities extracted from the top of the light component removal tower T01 and heavy component impurities extracted from the bottom of the heavy component removal tower T02 into a tail gas combustor R02 for incineration treatment at the incineration temperature of 750 ℃, and incinerating germane, digermane and the like to produce germanium dioxide powder. And (3) enabling the germanium dioxide powder to enter a germanium dioxide reduction furnace R03, reducing the germanium dioxide powder by using hydrogen to produce germanium powder at the temperature of 670 for 50min, and enabling the obtained germanium powder to enter a germanium powder tank for recycling.
The method for producing germane by plasma fluidization solves the problems of low germane production efficiency, generation of byproducts and wastewater and the like at present, and does not generate wastewater and byproducts which are difficult to separate and treat. Germanium is recycled after being treated by adopting germanium-containing impurities, so that the utilization rate of germanium is improved. The plasma synthesis reaction system adopted by the invention improves the reaction efficiency, and the obtained germane product has high purity.
The above-described embodiments are only preferred embodiments of the present invention, and it should be noted that those skilled in the art can make various changes and modifications without departing from the inventive concept, and these changes and modifications are all within the scope of the present invention.

Claims (10)

1. A process for plasma fluidized production of germane, characterized in that the process has the steps of:
1) Hydrogen enters a plasma hydrogen generator to generate plasma hydrogen, and the plasma hydrogen enters a fluidized bed;
2) Enabling the germanium powder to enter a fluidized bed, and carrying out a fluidization reaction with plasma hydrogen in the fluidized bed to generate germane;
3) Removing solid germanium powder carried by gas and solid from the reactant flow in the step 2) through a cyclone separator, and enabling the solid germanium powder to enter a germanium powder tank and enter a returning bed for secondary reaction; the gas phase enters a booster compressor for boosting, and condensation is carried out after boosting; returning the non-condensable gas hydrogen which is not condensed back to the hydrogen buffer tank for recycling;
4) The middle-upper material of the condensate tower enters a lightness-removing tower to remove light component impurities; extracting materials at the bottom of the tower, and removing heavy component impurities in a heavy component removing tower from the middle lower part; germane with the purity not lower than 5N is obtained at the tower top, and a germane product enters a germane product tank;
5) Light component impurities extracted from the top of the light component removal tower and heavy component impurities extracted from the bottom of the heavy component removal tower enter a tail gas combustor for incineration treatment; burning germane, digermane and the like to produce germanium dioxide powder; and (3) enabling the germanium dioxide powder to enter a germanium dioxide reduction furnace, producing germanium powder by using hydrogen reduction, and enabling the obtained germanium powder to enter a germanium powder tank for recycling.
2. The method for producing germane by plasma fluidization according to claim 1, wherein the hydrogen gas entering the plasma hydrogen generator in the step 1) is 0.2 to 3Bar; the discharge frequency of the plasma generator is 5-100KHz, and the discharge voltage is 10-50KV.
3. The method for producing germane by plasma fluidization according to claim 1, wherein the granularity of germanium powder entering the fluidized bed in the step 2) is 80-400 meshes.
4. The method for producing germane by plasma fluidization according to claim 1, wherein in the step 3), the gas phase is pressurized to 10-30Bar in a booster compressor, and the condensation temperature after pressurization is lower than-20 ℃.
5. The method for producing germane by plasma fluidization according to claim 1, wherein in the step 4), the operating temperature of the lightness-removing tower is-20 to-45 ℃, and the operating pressure is 6.1 to 11.6Bar.
6. The method for producing germane by plasma fluidization according to claim 1, wherein in the step 4), light component impurities such as hydrogen, nitrogen, carbon monoxide and methane are removed by a light component removal tower, and the extracted amount of light components at the top of the tower accounts for 3% -10% of the total amount of materials.
7. The method for producing germane by plasma fluidization according to claim 1, wherein in the step 4), the operation temperature of the de-weighting tower is-30 to-50 ℃, and the operation pressure is 5.2 to 10Bar.
8. The method for producing germane by plasma fluidization according to claim 1, wherein in the step 4), the de-weighting tower removes the heavy component impurities such as digermane and digermane from the tower kettle, and the extraction amount of the heavy component in the tower kettle accounts for 10-40% of the total amount of the materials.
9. The method for producing germane by plasma fluidization according to claim 1, wherein the incineration temperature in the step 5) is 500-900 ℃.
10. The method for producing germane by plasma fluidization according to claim 1, wherein in the step 5), the germanium powder is produced by reducing with hydrogen in a germanium dioxide reducing furnace at 600-700 ℃ for 30-9 min.
CN202210736607.0A 2022-06-27 2022-06-27 Method for producing germane by fluidization through plasma synthesis method Pending CN115140709A (en)

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CN111957064A (en) * 2020-09-10 2020-11-20 天津中科拓新科技有限公司 Method and device for synthesizing and refining optical fiber-grade germanium tetrachloride
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JP2015174800A (en) * 2014-03-14 2015-10-05 国立大学法人大阪大学 monosilane generator
CN111957064A (en) * 2020-09-10 2020-11-20 天津中科拓新科技有限公司 Method and device for synthesizing and refining optical fiber-grade germanium tetrachloride
CN114524413A (en) * 2022-03-02 2022-05-24 沧州华宇特种气体科技有限公司 System and method for preparing germane

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