CN105524101A - Silicon tetrafluoride complex preparation method and device adopted by method - Google Patents
Silicon tetrafluoride complex preparation method and device adopted by method Download PDFInfo
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- CN105524101A CN105524101A CN201510945826.XA CN201510945826A CN105524101A CN 105524101 A CN105524101 A CN 105524101A CN 201510945826 A CN201510945826 A CN 201510945826A CN 105524101 A CN105524101 A CN 105524101A
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- China
- Prior art keywords
- complexing agent
- tower
- storage tank
- complex
- silicon tetrafluoride
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title description 21
- 239000008139 complexing agent Substances 0.000 claims abstract description 70
- 238000006243 chemical reaction Methods 0.000 claims abstract description 61
- 230000018044 dehydration Effects 0.000 claims abstract description 23
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 23
- 230000000536 complexating effect Effects 0.000 claims abstract description 12
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 8
- 239000010959 steel Substances 0.000 claims abstract description 8
- 239000002808 molecular sieve Substances 0.000 claims abstract description 5
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 5
- 150000001875 compounds Chemical class 0.000 claims description 40
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 10
- 239000003507 refrigerant Substances 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 6
- 238000010668 complexation reaction Methods 0.000 abstract 5
- 229910004014 SiF4 Inorganic materials 0.000 abstract 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 14
- 229910052710 silicon Inorganic materials 0.000 description 14
- 239000010703 silicon Substances 0.000 description 14
- 239000000126 substance Substances 0.000 description 10
- 239000004065 semiconductor Substances 0.000 description 6
- 239000002994 raw material Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 3
- 230000000155 isotopic effect Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000005372 isotope separation Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000002210 silicon-based material Substances 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- YSBQKZZHQPPKEL-UHFFFAOYSA-N ethanol;tetrafluorosilane Chemical compound CCO.F[Si](F)(F)F YSBQKZZHQPPKEL-UHFFFAOYSA-N 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- JDIZLMCIIFJNSY-UHFFFAOYSA-N methanol;tetrafluorosilane Chemical compound OC.F[Si](F)(F)F JDIZLMCIIFJNSY-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000009377 nuclear transmutation Methods 0.000 description 1
Classifications
-
- 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
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/12—Organo silicon halides
- C07F7/121—Preparation or treatment not provided for in C07F7/14, C07F7/16 or C07F7/20
- C07F7/126—Preparation or treatment not provided for in C07F7/14, C07F7/16 or C07F7/20 by reactions involving the formation of Si-Y linkages, where Y is not a carbon or halogen atom
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
Abstract
The invention discloses a silicon tetrafluoride complex preparation method and a device thereof. The preparation method comprises the following steps: (1) allowing a complexing agent to enter a dehydration tower loaded with molecular sieve from the bottom of the dehydration tower loaded with the molecular sieve and outflow from the top of the dehydration tower, and collecting the complexing agent to an anhydrous complexing agent storage tank, wherein the content of water in the complexing agent is dropped to 50 ppm or less; and (2) adding the anhydrous complexing agent to a complexation reaction tower from the top of the complexation reaction tower; adding silicon tetrafluoride gas into the complexation reaction tower from the bottom of the complexation reaction tower; and collecting a silicon tetrafluoride complex to a complex storage tank. The device comprises a complexing agent storage tank (1), a complexing agent conveying pump (2), the dehydration tower (3), the anhydrous complexing agent storage tank (4), an anhydrous complexing agent conveying pump (5), a SiF4 steel cylinder (6), the complexation reaction tower (7), the complex storage tank (8) and a vacuum pump (9). The preparation method has the advantages of easy control, no pollution, complete reaction and the like; and the prepared silicon tetrafluoride complex has the advantages of high complexing degree and extremely low water content.
Description
Technical field
The present invention relates in hyundai electronics and semi-conductor industry, silicon isotope separation field, particularly a kind of preparation method of silicon tetrafluoride complex compound and equipment, it is applicable to prepare silicon tetrafluoride complex compound, supplies raw materials for follow-up silicon isotope is separated.
Background technology
In hyundai electronics and semi-conductor industry, silicon materials obtain a wide range of applications, and the semiconductor components and devices more than 90% is all made up of silicon.Natural silicon contains three kinds of stable isotropic substances
28si,
29si,
30si, its content is respectively 92.23%, and 4.67%, 3.10%.In recent years, the silicon materials of isotopic pure start with its excellent characteristic the concern being subject to scientists.
Along with the development of modern information industry and electronic computer industry, the volume of semi-conductor chip becomes less, integration degree is higher.But semi-conductor chip volume is less, circuit integrated level is higher, and current density will increase gradually, and unit volume internal heat generation amount increases, such will make components and parts operationally temperature raise, chip temperature is too high will cause performance of semiconductor element device and life-span to be declined to a great extent.Use isotopic pure
28si(99.85%) semiconducter device made, the comparable natural silicon of the thermal conductivity under room temperature increases by 10% ~ 60%, and what increase at some specific temperature is more.Isotopic pure
28the diode reverse breakdown voltage that Si makes can improve more than 80% than the natural silicon diode of same process.Enrichment
29si is a kind of potential material for storing and operate quantum computerized information.Contain
30the silicon ingot of Si is the novel material realizing neutron transmutation doping (NDT), and NDT is a kind of technology adopting the way of neutron irradiation to adulterate to material, and its maximum advantage is exactly that the impurities concentration distribution of mixing is very even.
At present, the method realizing silicon isotope separation mainly contains cryogenic rectification method, gas centrifuge process, laser method, chemical exchange method etc.Wherein, chemical exchange method, owing to having the advantages such as separation factor is high, treatment capacity is large, has become the method being hopeful most to realize silicon isotope industrial separation.Domestic chemical exchange method divided silicon isotropic substance is in the desk study stage, and the company that there is no produces silicon tetrafluoride complex compound, and the preparation method that the present invention proposes and equipment will be separated the silicon tetrafluoride complex compound raw material providing qualified for silicon isotope.
Summary of the invention
The object of this invention is to provide a kind of preparation method and equipment of silicon tetrafluoride complex compound, for subsequent chemistry exchange process divided silicon isotropic substance provides qualified silicon tetrafluoride complex compound raw material.The method has and is easy to control, and the feature such as pollution-free and react completely, obtained silicon tetrafluoride complex compound complexing degree is high, and water content is extremely low.
For solving the problems of the technologies described above, the present invention realizes like this.
A preparation method for silicon tetrafluoride complex compound, comprises the steps.
(1) complexing agent dehydration: complexing agent is entered bottom the dehydration tower of filling molecular sieve, top is flowed out, and is collected into anhydrous complexing agent storage tank; In complexing agent, moisture content is down to below 50ppm.
(2) complex reaction: anhydrous complexing agent is added to complex reaction tower from top; Silicon tetrafluoride gas adds complex reaction tower from bottom; Collect silicon tetrafluoride complex compound to complex compound storage tank, detect its complexing degree; If complexing is spent low, then complex compound is delivered to again complex reaction tower and react.
As a kind of preferred version, in step of the present invention (2), tower bottom pressure controls between absolute pressure 0.2 ~ 0.4Mpa.
Further, of the present invention have complexing agent to be one in the carbon alcohol such as methyl alcohol, ethanol or n-propyl alcohol.
Further, refrigerant cooling is passed in the chuck in step of the present invention (2) outside complex reaction tower; Complex reaction temperature is controlled between 0 ~ 10 DEG C.
The equipment that above-mentioned silicon tetrafluoride complexes preparation method adopts, comprises complexing agent storage tank, complexing agent transferpump, dehydration tower, anhydrous complexing agent storage tank, anhydrous complexing agent transferpump, SiF
4steel cylinder, complex reaction tower, complex compound storage tank and vacuum pump; The lower transport port of described complexing agent storage tank communicates with dehydration tower lower transport port through complexing agent transferpump; The top transmit port of described dehydration tower communicates with the top transmit port of anhydrous complexing agent storage tank; The lower transport port of described anhydrous complexing agent storage tank communicates with the top transmit port of complex reaction tower through anhydrous complexing agent transferpump; Described SiF
4the top transmit port of steel cylinder communicates with the lower transport port of complex reaction tower; Described complex reaction tower bottom complex compound collection port communicates with the top transmit port of complex compound storage tank; The working port of described vacuum pump communicates with the top transmit port of complex reaction tower.
As a kind of preferred version, the present invention is provided with chuck outside described complex reaction tower.
Further, the present invention is respectively equipped with the tensimeter that range is-0.1MPa ~ 1.0MPa at the bottom of described complex reaction column overhead and tower.
Further, the present invention is provided with at described complex reaction tower bottom the thermometer that range is-50 ~ 200 DEG C.
The silicon tetrafluoride complex compound complexing degree that the present invention obtains is high, and water content is extremely low, and for adopting chemical exchange method divided silicon isotropic substance to provide the qualified raw material of high-quality further, the inventive method has and is easy to control, and pollution-free, the feature such as react completely.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the invention will be further described.Protection scope of the present invention is not only confined to the statement of following content.
Fig. 1 is silicon tetrafluoride complexes preparation device structure schematic diagram of the present invention.
In figure: 1, complexing agent storage tank; 2, complexing agent transferpump; 3, dehydration tower; 4, anhydrous complexing agent storage tank; 5, anhydrous complexing agent transferpump; 6, SiF
4steel cylinder; 7, complex reaction tower; 8, complex compound storage tank; 9 is vacuum pump; 10, chuck.
Embodiment
As shown in the figure, the preparation method of silicon tetrafluoride complex compound, it comprises the steps.
(1) complexing agent dehydration: complexing agent is entered bottom the dehydration tower of filling molecular sieve, top is flowed out, and is collected into anhydrous complexing agent storage tank; In complexing agent, moisture content is down to below 50ppm; Described complexing agent is the one in the carbon alcohol such as methyl alcohol, ethanol or n-propyl alcohol.
(2) complex reaction: anhydrous complexing agent is added to complex reaction tower from top; Silicon tetrafluoride gas adds complex reaction tower from bottom; Collect silicon tetrafluoride complex compound to complex compound storage tank, detect its complexing degree; Complexing degree is qualified about 100%, if complexing is spent low, then complex compound is delivered to again complex reaction tower and reacts.Tower bottom pressure of the present invention controls between absolute pressure 0.2 ~ 0.4Mpa; Refrigerant cooling is passed in chuck outside described complex reaction tower; Complex reaction temperature is controlled between 0 ~ 10 DEG C.
The equipment that above-mentioned silicon tetrafluoride complexes preparation method adopts, comprises complexing agent storage tank 1, complexing agent transferpump 2, dehydration tower 3, anhydrous complexing agent storage tank 4, anhydrous complexing agent transferpump 5, SiF
4steel cylinder 6, complex reaction tower 7, complex compound storage tank 8 and vacuum pump 9; The lower transport port of described complexing agent storage tank 1 communicates with dehydration tower 3 lower transport port through complexing agent transferpump 2; The top transmit port of described dehydration tower 3 communicates with the top transmit port of anhydrous complexing agent storage tank 4; The lower transport port of described anhydrous complexing agent storage tank 4 communicates with the top transmit port of complex reaction tower 7 through anhydrous complexing agent transferpump 5; Described SiF
4the top transmit port of steel cylinder 6 communicates with the lower transport port of complex reaction tower 7; Bottom described complex reaction tower 7, complex compound collection port communicates with the top transmit port of complex compound storage tank 8; The working port of described vacuum pump 9 communicates with the top transmit port of complex reaction tower 7.The present invention is provided with chuck 10 outside described complex reaction tower 7.The present invention is respectively equipped with the tensimeter that range is-0.1MPa ~ 1.0MPa at the bottom of described complex reaction tower 7 tower top and tower.The present invention is provided with at described complex reaction 7 tower bottom the thermometer that range is-50 ~ 200 DEG C.
embodiment 1
The present embodiment makes complexing agent with methyl alcohol, with SiF
4silicon tetrafluoride methanol complex is prepared in gas reaction.
Detailed process is as follows.
1, start complexing agent transferpump 2 and methyl alcohol is squeezed into dehydration tower 3 from complexing agent storage tank 1, enter anhydrous complexing agent storage tank 4 after dehydration to store, detect anhydrous complexing agent water content, be qualified lower than 50ppm, if higher than this value, then the complexing agent in anhydrous complexing agent storage tank 4 is squeezed into dehydration tower 3 again to dewater, to qualified.
2, need to vacuumize process to whole complex reaction Tower System before reaction, when after the numerical value that pressure gauge reading is stabilized in close to-0.1Mpa, stop vacuumizing, and keep vacuum.
3, by purity higher than 99.99% SiF
4gas passes in complex reaction tower 7, reaches 0.2Mpa to pressure gauge reading.Pass into refrigerant to complex reaction tower chuck simultaneously.
4, open anhydrous complexing agent transferpump, add anhydrous complexing agent with the flow velocity of 50L/h to complex reaction tower 7 tower top, complexing agent and SiF
4gas carries out complex reaction in complex reaction tower 7, keep the temperature of complex compound at the bottom of tower to be 5 DEG C, tower bottom pressure gauge pressure at about 0.2MPa, along with the carrying out of reaction progressively adds SiF in complex reaction tower
4gas.
5, the silicon tetrafluoride complex compound that reaction produces enters complex compound storage tank 8 and stores, and detects its complexing degree, reaches about 100% for qualified, if too low, again return complex reaction top of tower and carry out complex reaction.
embodiment 2.
The present embodiment makes complexing agent with ethanol, with SiF
4silicon tetrafluoride ethanol complex is prepared in gas reaction.
Detailed process is as follows.
Preparation process reaction conditions keeps the temperature of complex compound at the bottom of tower to be 0 DEG C, tower bottom pressure gauge pressure is at about 0.25MPa.
All the other operation stepss are identical with embodiment 1.
embodiment 3.
The present embodiment makes complexing agent with n-propyl alcohol, with SiF
4silicon tetrafluoride n-propyl alcohol complex compound is prepared in gas reaction.
Detailed process is as follows.
Preparation process reaction conditions keeps the temperature of complex compound at the bottom of tower to be 2 DEG C, tower bottom pressure gauge pressure is at about 0.3MPa.
All the other operation stepss are identical with embodiment 1.
From above-mentioned example 1,2,3, the silicon tetrafluoride complex compound complexing degree that present method obtains is high, after testing about 100%, water content is extremely low, after testing lower than 50ppm, for adopting chemical exchange method divided silicon isotropic substance to provide the qualified raw material of high-quality further, present method have be easy to control, pollution-free, the feature such as react completely.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (8)
1. a preparation method for silicon tetrafluoride complex compound, is characterized in that, comprises the steps:
(1) complexing agent dehydration: complexing agent is entered bottom the dehydration tower of filling molecular sieve, top is flowed out, and is collected into anhydrous complexing agent storage tank; In complexing agent, moisture content is down to below 50ppm;
(2) complex reaction: anhydrous complexing agent is added to complex reaction tower from top; Silicon tetrafluoride gas adds complex reaction tower from bottom; Collect silicon tetrafluoride complex compound to complex compound storage tank, detect its complexing degree; If complexing is spent low, then complex compound is delivered to again complex reaction tower and react.
2. the preparation method of silicon tetrafluoride complex compound according to claim 1, is characterized in that: in described step (2), tower bottom pressure controls between absolute pressure 0.2 ~ 0.4Mpa.
3. the preparation method of silicon tetrafluoride complex compound according to claim 2, is characterized in that: described in have complexing agent to be one in the carbon alcohol such as methyl alcohol, ethanol or n-propyl alcohol.
4. the preparation method of silicon tetrafluoride complex compound according to claim 3, is characterized in that: pass into refrigerant cooling in the chuck in described step (2) outside complex reaction tower; Complex reaction temperature is controlled between 0 ~ 10 DEG C.
5. as Claims 1 to 4 arbitrary as described in silicon tetrafluoride complexes preparation method the equipment that adopts, it is characterized in that: comprise complexing agent storage tank (1), complexing agent transferpump (2), dehydration tower (3), anhydrous complexing agent storage tank (4), anhydrous complexing agent transferpump (5), SiF
4steel cylinder (6), complex reaction tower (7), complex compound storage tank (8) and vacuum pump (9); The lower transport port of described complexing agent storage tank (1) communicates with dehydration tower (3) lower transport port through complexing agent transferpump (2); The top transmit port of described dehydration tower (3) communicates with the top transmit port of anhydrous complexing agent storage tank (4); The lower transport port of described anhydrous complexing agent storage tank (4) communicates with the top transmit port of complex reaction tower (7) through anhydrous complexing agent transferpump (5); Described SiF
4the top transmit port of steel cylinder (6) communicates with the lower transport port of complex reaction tower (7); Described complex reaction tower (7) bottom complex compound collection port communicates with the top transmit port of complex compound storage tank (8); The working port of described vacuum pump (9) communicates with the top transmit port of complex reaction tower (7).
6. the equipment that adopts of silicon tetrafluoride complexes preparation method according to claim 5, is characterized in that: outside described complex reaction tower (7), be provided with chuck (10).
7. the equipment that adopts of silicon tetrafluoride complexes preparation method according to claim 6, is characterized in that: at the bottom of described complex reaction tower (7) tower top and tower, be respectively equipped with the tensimeter that range is-0.1MPa ~ 1.0MPa.
8. the equipment that adopts of silicon tetrafluoride complexes preparation method according to claim 7, is characterized in that: be provided with at described complex reaction (7) tower bottom the thermometer that range is-50 ~ 200 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510945826.XA CN105524101B (en) | 2015-12-17 | 2015-12-17 | Ocratation complex compound preparation method and its used equipment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510945826.XA CN105524101B (en) | 2015-12-17 | 2015-12-17 | Ocratation complex compound preparation method and its used equipment |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105524101A true CN105524101A (en) | 2016-04-27 |
| CN105524101B CN105524101B (en) | 2019-01-04 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201510945826.XA Expired - Fee Related CN105524101B (en) | 2015-12-17 | 2015-12-17 | Ocratation complex compound preparation method and its used equipment |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116832615A (en) * | 2023-08-29 | 2023-10-03 | 天津天和盛新材料科技有限公司 | Continuous production process method for silicon isotopes |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000048941A1 (en) * | 1999-02-16 | 2000-08-24 | Eagle-Picher Industries, Inc. | Enrichment of silicon or germanium isotopes |
| CN101257964A (en) * | 2005-09-08 | 2008-09-03 | 斯泰拉化工公司 | Isotopic enrichment process |
| CN102774845A (en) * | 2012-07-06 | 2012-11-14 | 天津大学 | Device and method for producing boron trifluoride-11 electronic specific gas |
| CN204447690U (en) * | 2014-12-19 | 2015-07-08 | 中国石油天然气股份有限公司 | Molecular sieve water separation tower |
-
2015
- 2015-12-17 CN CN201510945826.XA patent/CN105524101B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000048941A1 (en) * | 1999-02-16 | 2000-08-24 | Eagle-Picher Industries, Inc. | Enrichment of silicon or germanium isotopes |
| CN101257964A (en) * | 2005-09-08 | 2008-09-03 | 斯泰拉化工公司 | Isotopic enrichment process |
| CN102774845A (en) * | 2012-07-06 | 2012-11-14 | 天津大学 | Device and method for producing boron trifluoride-11 electronic specific gas |
| CN204447690U (en) * | 2014-12-19 | 2015-07-08 | 中国石油天然气股份有限公司 | Molecular sieve water separation tower |
Non-Patent Citations (2)
| Title |
|---|
| A. V. KHOROSHILOV等，: "Separation of Silicon Isotopes by Chemical Exchange between Silicon Tetrafluoride and Its Complex Compounds with Aliphatic Alcohols", 《THEORETICAL FOUNDATIONS OF CHEMICAL ENGINEERING》 * |
| J. P. GUERTIN等，: "THE INTERACTION OF SILICON TETRAFLUORIDE WITH METHANOL", 《CANADIAN JOURNAL OF CHEMISTRY》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116832615A (en) * | 2023-08-29 | 2023-10-03 | 天津天和盛新材料科技有限公司 | Continuous production process method for silicon isotopes |
| CN116832615B (en) * | 2023-08-29 | 2023-11-21 | 天津天和盛新材料科技有限公司 | Continuous production process method for silicon isotopes |
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