CN113135953A - Preparation method and device of dimethyl germane - Google Patents
Preparation method and device of dimethyl germane Download PDFInfo
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- CN113135953A CN113135953A CN202110490716.4A CN202110490716A CN113135953A CN 113135953 A CN113135953 A CN 113135953A CN 202110490716 A CN202110490716 A CN 202110490716A CN 113135953 A CN113135953 A CN 113135953A
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- dimethyl
- dimethylgermane
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- germane
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- RUIGDFHKELAHJL-UHFFFAOYSA-N dimethylgermane Chemical compound C[GeH2]C RUIGDFHKELAHJL-UHFFFAOYSA-N 0.000 title claims abstract description 149
- 238000002360 preparation method Methods 0.000 title claims description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 75
- 239000002904 solvent Substances 0.000 claims abstract description 47
- YQECBLVSMFAWIZ-UHFFFAOYSA-N dichloro(dimethyl)germane Chemical compound C[Ge](C)(Cl)Cl YQECBLVSMFAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000007788 liquid Substances 0.000 claims abstract description 34
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 28
- 238000001816 cooling Methods 0.000 claims abstract description 18
- 239000012535 impurity Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 11
- 238000009833 condensation Methods 0.000 claims abstract description 10
- 230000005494 condensation Effects 0.000 claims abstract description 10
- 238000010992 reflux Methods 0.000 claims abstract description 7
- 238000001179 sorption measurement Methods 0.000 claims description 35
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000012279 sodium borohydride Substances 0.000 claims description 5
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 5
- 239000012280 lithium aluminium hydride Substances 0.000 claims description 3
- -1 lithium aluminum hydride Chemical compound 0.000 claims description 3
- 125000003158 alcohol group Chemical group 0.000 claims description 2
- 229910052732 germanium Inorganic materials 0.000 abstract description 12
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 abstract description 12
- 238000004519 manufacturing process Methods 0.000 abstract description 11
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 9
- 239000000243 solution Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 230000003247 decreasing effect Effects 0.000 description 4
- 239000003507 refrigerant Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000002309 gasification Methods 0.000 description 3
- 229910000078 germane Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 230000036632 reaction speed Effects 0.000 description 3
- 239000006096 absorbing agent Substances 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- 239000012295 chemical reaction liquid Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical group [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 238000005468 ion implantation Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910000104 sodium hydride Inorganic materials 0.000 description 1
- 239000012312 sodium hydride Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- PPMWWXLUCOODDK-UHFFFAOYSA-N tetrafluorogermane Chemical compound F[Ge](F)(F)F PPMWWXLUCOODDK-UHFFFAOYSA-N 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/30—Germanium compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
Abstract
The invention discloses a method and a device for preparing dimethyl germane, wherein the method for preparing the dimethyl germane comprises the following steps: step S1: respectively injecting a solvent, dimethyl germanium dichloride and a reducing agent into the closed reaction kettle, and reacting the dimethyl germanium dichloride and the reducing agent to generate dimethyl germane; step S2: cooling the gaseous dimethyl germane and the volatilized partial gaseous solvent, and refluxing the liquid solvent generated by condensation to the closed reaction kettle; step S3: rectifying the gaseous dimethylgermane; step S4: adsorbing impurities in the gaseous dimethyl germane; step S5: and collecting the dimethyl germane. According to the invention, dimethyl germanium dichloride and a reducing agent react in a closed reaction kettle to generate dimethyl germane, a part of solvent mixed in the dimethyl germane is removed through rectification, impurities in the dimethyl germane are adsorbed, and finally the dimethyl germane is collected to be used as a germanium source for manufacturing a chip.
Description
Technical Field
The invention relates to the technical field of preparation of semiconductor precursors, in particular to a method and a device for preparing dimethyl germane.
Background
The manufacture of large scale integrated circuit chips is the top technology with intense international competition, and germanium element needs to be implanted in an ion implantation manner in the chip manufacturing process. Commonly used germanium sources such as germane, germanium tetrafluoride, etc. often have flammable, explosive, and toxic hazardous properties.
Therefore, how to improve the security of the germanium source for manufacturing the chip is a technical problem to be solved urgently by those skilled in the art.
Disclosure of Invention
In view of the above, the first objective of the present invention is to provide a method for preparing dimethylgermane, which can produce high-purity dimethylgermane meeting the requirements of the integrated circuit industry, and improve the safety of germanium source manufacturing chips.
The second purpose of the invention is to provide a device for preparing the dimethyl germane.
In order to achieve the first object, the present invention provides the following solutions:
a method for preparing dimethylgermane, comprising:
step S1: respectively injecting a solvent, dimethyl germanium dichloride and a reducing agent into the closed reaction kettle, and reacting the dimethyl germanium dichloride and the reducing agent to generate dimethyl germane;
step S2: cooling the gaseous dimethyl germane and the volatilized partial gaseous solvent, and refluxing the liquid solvent generated by condensation to the closed reaction kettle;
step S3: rectifying the gaseous dimethylgermane;
step S4: adsorbing impurities in the gaseous dimethyl germane;
step S5: and collecting the dimethyl germane.
In a specific embodiment, between the step S4 and the step S5, a step S6 is further included: cooling the gaseous dimethylgermane so that the gaseous dimethylgermane liquefies into liquid dimethylgermane.
According to the preparation method of the dimethyl germane, dimethyl germanium dichloride and a reducing agent react in a closed reaction kettle to generate the dimethyl germane, a part of solvent mixed in the dimethyl germane is removed through rectification, impurities in the dimethyl germane are adsorbed again, and finally the dimethyl germane is collected to be used as a germanium source for manufacturing a chip.
In order to achieve the second object, the present invention provides the following solutions:
a preparation device of dimethyl germane comprises a closed reaction kettle, a rectification system, an adsorption system and a collecting tank;
dimethyl germanium dichloride, a reducing agent and a solvent are contained in the closed reaction kettle, and the dimethyl germanium dichloride and the reducing agent react to generate dimethyl germane;
the inlet of the rectification system is communicated with the outlet of the closed reaction kettle, and the rectification system is used for rectifying the dimethyl germane entering the rectification system;
the inlet of the adsorption system is communicated with the outlet of the rectification system, and the adsorption system is used for adsorbing impurities in the dimethyl germane entering the adsorption system;
the collecting tank is connected with the outlet of the adsorption system in a conduction mode and is used for collecting the dimethyl germane adsorbed and treated by the adsorption system.
In a specific embodiment, the apparatus for preparing dimethylgermane further comprises a cooler;
the cooler is arranged between the closed reaction kettle and the rectification system and is used for cooling gaseous dimethyl germane and gaseous solvent volatilized by the closed reaction kettle;
and the cooler is positioned above the closed reaction kettle, and the solvent condensed into liquid can flow back into the closed reaction kettle.
In another specific embodiment, the rectification system comprises a rectification column and a first condenser;
the inlet of the rectifying tower is communicated with the outlet of the cooler;
the export of rectifying column with the entry turn-on connection of first condenser, the export of first condenser respectively with adsorption system's entry reaches the liquid entry turn-on connection of rectifying column, first condenser is used for the gaseous state dimethyl germane that the condensation rectification came out.
In another specific embodiment, the apparatus for preparing dimethylgermane further comprises a first jacket and a second jacket;
the first jacket is coated outside the closed reaction kettle and used for heating or cooling the closed reaction kettle;
the second jacket is coated on the rectifying tower and used for heating or cooling the rectifying tower.
In another specific embodiment, the apparatus for preparing dimethylgermane further comprises a second condenser;
the second condenser is located the top of collection tank, just the entry of second condenser with the export turn-on connection of adsorber, the export of second condenser with the entry turn-on connection of collection tank for the condensation gaseous state dimethyl germane.
In another specific embodiment, the apparatus for preparing dimethylgermane further comprises a feed tank;
the number of the feeding tanks is 3, the feeding tanks are all in conduction connection with the closed reaction kettle and are respectively used for containing dimethyl germanium dichloride, a reducing agent and a solvent.
In another specific embodiment, the adsorption system comprises at least 1 adsorber, when the number of the adsorber is greater than or equal to 2, the adsorber is arranged in series, and the outlet of the former adsorber is lower than the inlet of the latter adsorber along the flow direction of the gaseous dimethylgermane.
In another specific embodiment, a stirrer is arranged in the closed reaction kettle;
the solvent is an alcohol ether solvent;
the reducing agent is sodium borohydride or lithium aluminum hydride.
The various embodiments according to the invention can be combined as desired, and the embodiments obtained after these combinations are also within the scope of the invention and are part of the specific embodiments of the invention.
When the device for preparing the dimethyl germane is used, dimethyl germanium dichloride and a reducing agent react in a closed reaction kettle to generate the dimethyl germane, the generated dimethyl germane and a part of solvent enter a rectification system for rectification, impurities in the dimethyl germane are adsorbed by an adsorption system, and finally the dimethyl germane is collected by a collection tank and is used as a germanium source for manufacturing a chip.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without novelty work.
Fig. 1 is a schematic structural diagram of a device for preparing dimethylgermane according to the present invention.
Wherein, in fig. 1:
the device comprises a closed reaction kettle 1, a rectification system 2, an adsorption system 3, a collection tank 4, a first jacket 5, a feeding tank 6, a cooler 7, a rectification tower 201, a first condenser 202, a second jacket 8 and a second condenser 9.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to fig. 1 in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the description of the present invention, it is to be understood that the terms "upper", "lower", "top", "bottom", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of describing the present invention and simplifying the description, but do not indicate or imply that the position or element referred to must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, are not to be construed as limiting the present invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
The invention provides a preparation method of dimethyl germane, which comprises the following steps:
step S1: and respectively injecting a solvent, dimethyl germanium dichloride and a reducing agent into the closed reaction kettle 1, and reacting the dimethyl germanium dichloride and the reducing agent to generate dimethyl germane.
Specifically, the closed reaction kettle 1 is in a vacuum state, so that impurities in the air are prevented from influencing the purity of the dimethyl germane.
After the solvent, the reducing agent and the dimethyl germanium dichloride are injected into the closed reaction kettle 1, the mixture is stirred by a stirrer so as to accelerate the reaction speed of the dimethyl germanium dichloride and the reducing agent.
Step S2: cooling the gaseous dimethyl germane and the volatilized partial gaseous solvent, and refluxing the condensed liquid solvent into the closed reaction kettle 1.
Specifically, the gaseous dimethylgermane and a part of the mixed gaseous solvent are cooled by the cooler 7, so that the solvent can flow back into the closed reaction vessel 1.
When the reaction is carried out in the closed reaction kettle 1, the reaction liquid is cooled by the first jacket 5 sleeved outside the closed reaction kettle 1, and after the reaction is finished, the residual dimethyl germane in the solvent is heated and evaporated by the first jacket 5, so that the yield of the batch product is improved.
Step S3: rectifying the gaseous dimethylgermane.
Specifically, the rectification of the dimethyl germane is realized through the rectifying tower 201 and the first condenser 202, the gaseous dimethyl germane discharged from the outlet of the rectifying tower 201 enters the first condenser 202, the gaseous dimethyl germane reacts with a low-temperature refrigerant in the first condenser 202, the dimethyl germane is condensed into liquid, one part of the liquid flows back to the rectifying tower 201, the other part of the liquid flows into the subsequent adsorption system 3, the liquid flowing back to the bottom of the rectifying tower 201 is heated and gasified through the second jacket 8 sleeved at the bottom of the rectifying tower 201, and the heating gasification of the rectifying tower 201 at the second jacket 8 and the condensation reflux of the first condenser 202 realize the rectification circulation process.
Step S4: adsorbing impurities in the gaseous dimethyl germane.
Specifically, the impurity removal of the gaseous dimethylgermane is achieved by the adsorption system 3. In particular, the adsorption system 3 comprises at least 1 adsorber. The number of adsorbers is not limited to 1, and may be increased or decreased as necessary. When the number of the adsorbers is more than or equal to 2, the adsorbers are arranged in series, and the outlet of the former adsorber is lower than the inlet of the latter adsorber along the flow direction of the gaseous dimethyl germane, so that the liquid solvent is prevented from entering the collection tank 4 through the adsorbers.
Step S5: and collecting the dimethyl germane.
Specifically, dimethylgermane is collected by the collection tank 4.
Further, the invention discloses that step S6 is further included between step S4 and step S5: cooling the gaseous dimethylgermane so that the gaseous dimethylgermane liquefies into liquid dimethylgermane.
Specifically, the gaseous dimethylgermane exiting from adsorption system 3 is condensed by second condenser 9.
According to the preparation method of the dimethyl germane, dimethyl germanium dichloride and a reducing agent react in a closed reaction kettle 1 to generate the dimethyl germane, a part of solvent mixed in the dimethyl germane is removed through rectification, impurities in the dimethyl germane are adsorbed again, and finally the dimethyl germane is collected to be used as a germanium source for manufacturing a chip.
As shown in fig. 1, another aspect of the present invention provides a dimethylgermane preparation apparatus for preparing high-purity dimethylgermane as a germanium source for an integrated circuit chip. Dimethyl germane is a low-pressure liquefied gas, the vapor pressure of the dimethyl germane is lower than that of germane at normal temperature, and the dimethyl germane is used for replacing germane as a germanium source for manufacturing a semiconductor integrated circuit chip, so that the burning and explosion risks in the processes of production, storage, transportation and use of the germanium source are reduced.
Wherein, the preparation device of the dimethyl germane comprises a closed reaction kettle 1, a rectification system 2, an adsorption system 3 and a collecting tank 4.
Dimethyl germanium dichloride, a reducing agent and a solvent are contained in the closed reaction kettle 1, and the dimethyl germanium dichloride and the reducing agent react to generate dimethyl germane. It should be noted that, the closed reaction kettle 1 is in a vacuum state, so as to prevent impurities in the air from entering the dimethyl germane to affect the purity of the dimethyl germane.
Compared with the prior art that the raw material dimethyl germanium dichloride has poor solubility, low reaction speed and low yield when water is used as a solvent for reaction, the alcohol ether solvent is adopted in the invention, so that the dimethyl germanium dichloride is convenient to dissolve in the alcohol ether solution, the solubility is high, the reaction speed is high, and the efficiency is high. Specifically, the alcohol ether solvent is methanol or diethyl ether. The reducing agent is sodium hydride or lithium aluminum hydride.
An inlet of the rectification system 2 is communicated with an outlet of the closed reaction kettle 1, and the rectification system 2 is used for rectifying the dimethyl germane entering the rectification system 2. Dimethyl germane generated by reaction in the closed reaction kettle 1 enters the rectification system 2, and the gaseous dimethyl germane is mixed with a gaseous solvent, so that the rectification system is required to rectify and the purity of the dimethyl germane is improved.
The inlet of the adsorption system 3 is connected with the outlet of the rectification system 2 in a conduction manner, and the adsorption system 3 is used for adsorbing impurities in the dimethyl germane entering the adsorption system 3, so that the purity of the dimethyl germane is further improved.
The collection tank 4 is connected with the outlet of the adsorption system 3 in a conduction manner and is used for collecting the dimethyl germane adsorbed by the adsorption system 3.
When the device for preparing the dimethyl germane is used, dimethyl germanium dichloride and a reducing agent react in a closed reaction kettle 1 to generate the dimethyl germane, the generated dimethyl germane and a part of solvent enter a rectification system 2 for rectification, impurities in the dimethyl germane are adsorbed through an adsorption system 3, and finally the dimethyl germane is collected through a collection tank 4 and serves as a germanium source for manufacturing a chip.
In some embodiments, the apparatus for preparing dimethylgermane further comprises a first jacket 5, wherein the first jacket 5 is wrapped outside the closed reaction kettle 1 and used for heating or cooling the closed reaction kettle 1. The first jacket 5 can cool the reaction liquid in the reaction process, and the residual dimethyl germane in the solvent can be heated and evaporated by the first jacket 5 after the reaction is finished, so that the yield of the batch product is improved.
The means for heating or cooling the closed reaction vessel 1 is not limited to the jacket, and may be any other means capable of increasing or decreasing the temperature.
Further, the invention discloses that a stirrer is arranged in the closed reaction kettle 1, the stirrer can fully mix materials to promote the reaction to be carried out by stirring, and the reaction efficiency of the dimethyl germanium dichloride and the reducing agent is improved. Specifically, the stirrer is any stirring device capable of uniformly mixing various liquids in the closed reaction kettle 1.
In some embodiments, the apparatus for preparing dimethylgermane further includes feeding tanks 6, and specifically, the number of the feeding tanks 6 is 3, and the feeding tanks are all in conductive connection with the closed reaction kettle 1 and are respectively used for containing dimethylgermanium dichloride, a reducing agent and a solvent.
In some embodiments, the apparatus for preparing dimethylgermane further comprises a cooler 7, wherein the cooler 7 is disposed between the closed reaction vessel 1 and the rectification system 2, and is used for cooling the dimethylgermane volatilized from the closed reaction vessel 1 and the solvent.
The cooler 7 is positioned above the closed reaction kettle 1, most of the solvent condensed into liquid state flows back into the closed reaction kettle 1 under the cooling effect of the cooler 7, the solvent does not need to be continuously supplemented in the reaction process, and the load of the subsequent purified part of the separated solvent is also reduced.
In some embodiments, rectification system 2 includes a rectification column 201 and a first condenser 202, and an inlet of rectification column 201 is in fluid communication with an outlet of cooler 7. The outlet of the rectifying tower 201 is in conduction connection with the inlet of the first condenser 202, the outlet of the first condenser 202 is in conduction connection with the inlet of the adsorption system 3 and the liquid inlet of the rectifying tower 201, and the liquid inlet of the rectifying tower 201 is arranged above the rectifying tower 201.
Further, the invention discloses a preparation device of dimethyl germane, which further comprises a second jacket 8, wherein the second jacket 8 is coated on the rectifying tower 201 and used for heating or cooling the distilling tower. The residual dimethyl germane in the solvent in the rectifying tower 201 is heated through the second jacket 8, so that the yield of the batch product is improved.
Gaseous dimethyl germane discharged from the outlet of the rectifying tower 201 enters the first condenser 202, and reacts with a low-temperature refrigerant in the first condenser 202, the dimethyl germane is condensed into liquid, a part of the liquid flows back into the rectifying tower 201, a part of the liquid enters the adsorption system 3, the liquid flowing back to the bottom of the rectifying tower 201 is gasified under the heating action of the second jacket 8, the heating gasification of the rectifying tower 201 at the second jacket 8 and the condensation reflux of the first condenser 202 realize the rectification circulation process.
It should be noted that the temperature of the rectifying column 201 is not limited to be increased or decreased by the jacket, and other devices for achieving heat conduction may be used.
In some embodiments, the adsorption system 3 includes at least 1 adsorber. The number of adsorbers is not limited to 1, and may be increased or decreased as necessary. When the number of the adsorbers is more than or equal to 2, the adsorbers are arranged in series, wherein the series arrangement refers to that the adsorbers are sequentially communicated end to end. The outlet of the previous adsorber is lower than the inlet of the following adsorber in the flow direction of the gaseous dimethylgermane, avoiding the liquid solvent from passing through the adsorber into the collection tank 4.
The invention directly obtains high-purity dimethyl germane by purifying the synthesis gas through the rectifying tower 201 and the absorber, and solves the problem of low purity of dimethyl germane prepared in a laboratory.
In some embodiments, the present invention discloses that the apparatus for preparing dimethylgermane further comprises a second condenser 9; the inlet of the second condenser 9 is connected with the outlet of the adsorber in a conduction way, and the outlet of the second condenser 9 is connected with the inlet of the collecting tank 4 in a conduction way. The rectified gaseous dimethyl germane enters an absorber for adsorption and purification, is condensed and liquefied by a second condenser 9, and enters a product collecting tank 4 for collection.
Example one
Methanol is added into the closed reaction kettle 1 through 1 feeding tank 6, sodium borohydride is added through another feeding tank 6 (after the addition is finished, the sodium borohydride powder can be washed into the closed reaction kettle 1 through the methanol), and dimethyl germanium dichloride is added into the 3 rd feeding tank 6. Continuously stirring the closed reaction kettle 1, vacuumizing the feeding tank 6 for containing the dimethyl germanium dichloride and the closed reaction kettle 1 to remove air, and slowly adding the dimethyl germanium dichloride into the reaction kettle. Dimethyl germane is generated by adding dimethyl germanium dichloride and reacting, the dimethyl germane and part of methanol steam volatilize and enter the cooler 7, the cooler 7 uses chilled water for heat exchange, the methanol steam is condensed and reflows, and the dimethyl germane enters the rectifying tower 201.
The dimethyl germane rises in the rectifying tower 201 and enters the first condenser 202, and is condensed into liquid under the action of a low-temperature refrigerant in the first condenser 202, one part of the liquid returns to the rectifying tower 201, and the other part of the liquid enters 2 adsorbers. The adsorber further removes impurities entrained in the dimethylgermane by an internally loaded adsorbent. The dimethyl germane after adsorption and purification enters a second condenser 9 to be condensed into liquid, and then enters a product collecting tank 4 to be collected.
Example two
Adding ethanol into the closed reaction kettle 1 through the feeding tank 6, adding a sodium borohydride aqueous solution through the feeding tank 6, and adding dimethyl germanium dichloride into the feeding tank 6. Continuously stirring the closed reaction kettle 1, and vacuumizing the feeding tank 6 for containing the dimethyl germanium dichloride and the closed reaction kettle 1 to remove air. Slowly adding dimethyl germanium dichloride in the feeding tank 6 into the closed reaction kettle 1. Dimethyl germane is generated by the reaction of the addition of dimethyl germanium dichloride, and the dimethyl germane, part of ethanol steam and water vapor are volatilized to enter a cooler 7. The cooler 7 uses chilled water for heat exchange, the ethanol steam and the water vapor are condensed and refluxed, and the dimethyl germane enters the rectifying tower 201.
The dimethyl germane rises in the rectifying tower 201 and enters the first condenser 202, and is condensed into liquid by the action of low-temperature refrigerant in the first condenser 202, and a part of the liquid returns to the rectifying tower 210, and a part of the liquid enters the adsorber. The liquid refluxed to the bottom of the rectifying tower 201 is gasified under the heating action of the second jacket 8, and the heating gasification at the second jacket 8 and the condensation reflux of the first condenser 202 realize the rectifying cycle process. The adsorber further removes impurities entrained in the dimethylgermane by the adsorbent loaded therein. The dimethyl germane after adsorption and purification enters a second condenser 9 to be condensed into liquid, and then enters a product collecting tank 4 to be collected.
It should be noted that the words indicating the orientation in this document, for example, the upper and lower, are set in the directions in which the apparatus for producing dimethylgermane is used, and are not intended to have other specific meanings for convenience of description.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise forms disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (10)
1. A method for preparing dimethylgermane, which is characterized by comprising the following steps:
step S1: respectively injecting a solvent, dimethyl germanium dichloride and a reducing agent into the closed reaction kettle, and reacting the dimethyl germanium dichloride and the reducing agent to generate dimethyl germane;
step S2: cooling the gaseous dimethyl germane and the volatilized partial gaseous solvent, and refluxing the liquid solvent generated by condensation to the closed reaction kettle;
step S3: rectifying the gaseous dimethylgermane;
step S4: adsorbing impurities in the gaseous dimethyl germane;
step S5: and collecting the dimethyl germane.
2. The method for preparing dimethylgermane according to claim 1, further comprising step S6 between step S4 and step S5: cooling the gaseous dimethylgermane so that the gaseous dimethylgermane liquefies into liquid dimethylgermane.
3. The preparation device of the dimethyl germane is characterized by comprising a closed reaction kettle, a rectification system, an adsorption system and a collection tank;
dimethyl germanium dichloride, a reducing agent and a solvent are contained in the closed reaction kettle, and the dimethyl germanium dichloride and the reducing agent react to generate dimethyl germane;
the inlet of the rectification system is communicated with the outlet of the closed reaction kettle, and the rectification system is used for rectifying the dimethyl germane entering the rectification system;
the inlet of the adsorption system is communicated with the outlet of the rectification system, and the adsorption system is used for adsorbing impurities in the dimethyl germane entering the adsorption system;
the collecting tank is connected with the outlet of the adsorption system in a conduction mode and is used for collecting the dimethyl germane adsorbed and treated by the adsorption system.
4. The apparatus for preparing dimethylgermane according to claim 3, further comprising a cooler;
the cooler is arranged between the closed reaction kettle and the rectification system and is used for cooling gaseous dimethyl germane and gaseous solvent volatilized by the closed reaction kettle;
and the cooler is positioned above the closed reaction kettle, and the solvent condensed into liquid can flow back into the closed reaction kettle.
5. The apparatus for preparing dimethylgermane according to claim 4, wherein the rectification system comprises a rectification column and a first condenser;
the inlet of the rectifying tower is communicated with the outlet of the cooler;
the export of rectifying column with the entry turn-on connection of first condenser, the export of first condenser respectively with adsorption system's entry reaches the liquid entry turn-on connection of rectifying column, first condenser is used for the gaseous state dimethyl germane that the condensation rectification came out.
6. The apparatus for preparing dimethylgermane according to claim 5, further comprising a first jacket and a second jacket;
the first jacket is coated outside the closed reaction kettle and used for heating or cooling the closed reaction kettle;
the second jacket is coated on the rectifying tower and used for heating or cooling the rectifying tower.
7. The apparatus for preparing dimethylgermane according to claim 6, further comprising a second condenser;
the second condenser is located the top of collection tank, just the entry of second condenser with the export turn-on connection of adsorber, the export of second condenser with the entry turn-on connection of collection tank for the condensation gaseous state dimethyl germane.
8. The apparatus for preparing dimethylgermane according to claim 3, further comprising a feed tank;
the number of the feeding tanks is 3, the feeding tanks are all in conduction connection with the closed reaction kettle and are respectively used for containing dimethyl germanium dichloride, a reducing agent and a solvent.
9. The apparatus for preparing dimethylgermane according to claim 3, wherein the adsorption system comprises at least 1 adsorber, and when the number of the adsorber is greater than or equal to 2, the adsorber is arranged in series, and the outlet of the former adsorber is lower than the inlet of the latter adsorber along the flow direction of the gaseous dimethylgermane.
10. The apparatus for preparing dimethylgermane according to any one of claims 3 to 9, wherein a stirrer is disposed in the closed reaction vessel;
the solvent is an alcohol ether solvent;
the reducing agent is sodium borohydride or lithium aluminum hydride.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014109463A1 (en) * | 2013-01-14 | 2014-07-17 | 대성산업가스 주식회사 | Method for producing high-purity germane and device therefor |
| TW201522229A (en) * | 2013-12-06 | 2015-06-16 | Gelest Technologies Inc | Method for producing high purity germane by a continuous or semi-continuous process |
| CN112546659A (en) * | 2020-12-08 | 2021-03-26 | 云南临沧鑫圆锗业股份有限公司 | Purification device and method for germanium tetrafluoride |
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2021
- 2021-05-06 CN CN202110490716.4A patent/CN113135953A/en active Pending
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| WO2014109463A1 (en) * | 2013-01-14 | 2014-07-17 | 대성산업가스 주식회사 | Method for producing high-purity germane and device therefor |
| TW201522229A (en) * | 2013-12-06 | 2015-06-16 | Gelest Technologies Inc | Method for producing high purity germane by a continuous or semi-continuous process |
| CN112546659A (en) * | 2020-12-08 | 2021-03-26 | 云南临沧鑫圆锗业股份有限公司 | Purification device and method for germanium tetrafluoride |
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Application publication date: 20210720 |