CN105524101B - Ocratation complex compound preparation method and its used equipment - Google Patents
Ocratation complex compound preparation method and its used equipment Download PDFInfo
- Publication number
- CN105524101B CN105524101B CN201510945826.XA CN201510945826A CN105524101B CN 105524101 B CN105524101 B CN 105524101B CN 201510945826 A CN201510945826 A CN 201510945826A CN 105524101 B CN105524101 B CN 105524101B
- Authority
- CN
- China
- Prior art keywords
- tower
- complexing agent
- storage tank
- complex reaction
- complex
- Prior art date
- 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.)
- Expired - Fee Related
Links
- 150000001875 compounds Chemical class 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000008139 complexing agent Substances 0.000 claims abstract description 104
- 238000006243 chemical reaction Methods 0.000 claims abstract description 101
- 230000000536 complexating effect Effects 0.000 claims abstract description 27
- 229910004014 SiF4 Inorganic materials 0.000 claims abstract description 26
- 230000018044 dehydration Effects 0.000 claims abstract description 14
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 12
- 239000010959 steel Substances 0.000 claims abstract description 12
- 230000005540 biological transmission Effects 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 24
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- 238000012797 qualification Methods 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 9
- 235000019441 ethanol Nutrition 0.000 claims description 8
- 239000002826 coolant Substances 0.000 claims description 6
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims 2
- 239000002808 molecular sieve Substances 0.000 abstract description 3
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 abstract description 3
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 abstract description 3
- 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
- 239000004065 semiconductor Substances 0.000 description 7
- 238000000926 separation method Methods 0.000 description 6
- 239000002994 raw material Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 4
- 238000005372 isotope separation Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000011017 operating method Methods 0.000 description 2
- 239000002210 silicon-based material Substances 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification 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 present invention discloses the preparation method and equipment of a kind of ocratation complex compound, and preparation method includes that (1) enters complexing agent from the dehydration tower bottom of filling molecular sieve, and top outflow is collected to anhydrous complexing agent storage tank；Moisture content is down to 50ppm or less in complexing agent；(2) anhydrous complexing agent is added from top to complex reaction tower；Complex reaction tower is added from bottom in silicon tetrafluoride gas；Ocratation complex compound is collected to complex compound storage tank.Equipment includes complexing agent storage tank (1), complexing agent delivery pump (2), dehydrating tower (3), anhydrous complexing agent storage tank (4), anhydrous complexing agent delivery pump (5), SiF4Steel cylinder (6), complex reaction tower (7), complex compound storage tank (8) and vacuum pump (9).The present invention has the features such as easily controllable, pollution-free and fully reacting, and ocratation complex compound complexing degree obtained is high, and water content is extremely low.
Description
Technical field
The present invention relates in hyundai electronics and semi-conductor industry, silicon isotope separation field, especially a kind of ocratation
The preparation method and equipment of complex compound provide raw material it is suitable for preparing ocratation complex compound for the separation of subsequent silicon isotope.
Background technique
In hyundai electronics and semi-conductor industry, silicon materials are had been widely used, the semiconductor components and devices more than 90%
All it is made of silicon.Natural silicon is containing there are three types of stable isotopes28Si、29Si、30Si, content are respectively 92.23%,
4.67%, 3.10%.In recent years, the silicon materials of isotopically pure start the concern by scientists with its excellent characteristic.
With the development of modern information industry and electronic computer industry, the volume of semiconductor chip becomes smaller, integrated
Change degree is higher.But semiconductor chip volume is smaller, and route integrated level is higher, and current density will be gradually increased, in unit volume
Calorific value increases, in this way will be so that component temperature raising at work, chip temperature is excessively high will to will lead to semiconductor components and devices
Performance and service life decline to a great extent.Use isotopically pure28Si(99.85% semiconductor devices made of), thermal conductivity at room temperature is than day
Right silicon increases by 10%~60%, increased more at certain specific temperature.Isotopically pure28Diode reverse breakdown made of Si
Voltage can be improved 80% or more than the natural silicon diode of same process.Enrichment29Si is a kind of potentially for storage and operating quantity
The material of sub- computerized information.Contain30The silicon ingot of Si is the new material for realizing neutron transmutation doping (NDT), and NDT is using neutron
The method of irradiation is come a kind of technology being doped to material, and the biggest advantage is to the impurities concentration distribution of incorporation is very equal
It is even.
Currently, the method for realizing silicon isotope separation mainly has cryogenic rectification method, gas centrifugation, laser method, chemistry to hand over
Change method etc..Wherein, chemical exchange method is due to having many advantages, such as that separation is high, treating capacity is big, it has also become is most hopeful to realize silicon
The method of isotope industrial separation.Domestic chemical exchange method separation silicon isotope is in the desk study stage, there is no company raw
Ocratation complex compound is produced, preparation method and equipment proposed by the present invention will provide qualified ocratation for silicon isotope separation
Raw material is complexed.
Summary of the invention
The object of the present invention is to provide the preparation methods and equipment of a kind of ocratation complex compound, are subsequent chemistry exchange process
It separates silicon isotope and qualified ocratation complexing raw material is provided.This method has easily controllable, pollution-free and fully reacting
The features such as, ocratation complex compound complexing degree obtained is high, and water content is extremely low.
In order to solve the above technical problems, the invention is realized in this way.
A kind of preparation method of ocratation complex compound, includes the following steps.
(1) complexing agent is dehydrated: complexing agent being entered from the dehydration tower bottom of filling molecular sieve, top outflow is collected to nothing
Water complexing agent storage tank；Moisture content is down to 50ppm or less in complexing agent.
(2) complex reaction: anhydrous complexing agent is added from top to complex reaction tower；Silicon tetrafluoride gas is added from bottom
Complex reaction tower；Ocratation complex compound is collected to complex compound storage tank, detects its complexing degree；If complexing spend it is low, will complexing
Object, which is sent again to complex reaction tower, to be reacted.
As a preferred embodiment, in step (2) of the present invention tower bottom pressure control 0.2~0.4Mpa of absolute pressure it
Between.
Further, of the present invention to have complexing agent for one of carbon alcohol such as methanol, ethyl alcohol or normal propyl alcohol.
Further, coolant cooling is passed through in the collet in step (2) of the present invention outside complex reaction tower；It will complexing
Reaction temperature controls between 0~10 DEG C.
Equipment used by above-mentioned ocratation complex compound preparation method, including it is complexing agent storage tank, complexing agent delivery pump, de-
Water tower, anhydrous complexing agent storage tank, anhydrous complexing agent delivery pump, SiF4Steel cylinder, complex reaction tower, complex compound storage tank and vacuum pump；
The lower transport port of the complexing agent storage tank is communicated through complexing agent delivery pump with dehydrating tower lower transport port；The dehydrating tower
Top transmission port communicated with the top transmission port of anhydrous complexing agent storage tank；The lower transport of the anhydrous complexing agent storage tank
Port is communicated through anhydrous complexing agent delivery pump with the top transmission port of complex reaction tower；The SiF4The top transmission end of steel cylinder
Mouth is communicated with the lower transport port of complex reaction tower；The complex reaction tower bottom complex compound collection port and complex compound storage tank
Top transmission port communicate；The working port of the vacuum pump is communicated with the top transmission port of complex reaction tower.
As a preferred embodiment, the present invention is externally provided with collet in the complex reaction tower.
Further, the present invention the complex reaction column overhead and tower bottom be respectively equipped with range be -0.1MPa~
The pressure gauge of 1.0MPa.
Further, the present invention is equipped with the thermometer that range is -50~200 DEG C in the complex reaction tower bottom.
Ocratation complex compound complexing degree produced by the present invention is high, and water content is extremely low, further to use chemical exchange method
Separation silicon isotope provides the raw material of high-quality qualification, and the method for the present invention has easily controllable, pollution-free, the spies such as fully reacting
Point.
Detailed description of the invention
Present invention will be further explained below with reference to the attached drawings and specific embodiments.Protection scope of the present invention not only office
It is limited to the statement of following content.
Fig. 1 is ocratation complex compound Preparation equipment structural schematic diagram of the present invention.
In figure: 1, complexing agent storage tank；2, complexing agent delivery pump；3, dehydrating tower；4, anhydrous complexing agent storage tank；5, anhydrous complexing
Agent delivery pump；6,SiF4Steel cylinder；7, complex reaction tower；8, complex compound storage tank；9 be vacuum pump；10, collet.
Specific embodiment
As shown, the preparation method of ocratation complex compound, it includes the following steps.
(1) complexing agent is dehydrated: complexing agent being entered from the dehydration tower bottom of filling molecular sieve, top outflow is collected to nothing
Water complexing agent storage tank；Moisture content is down to 50ppm or less in complexing agent；The complexing agent is the carbon such as methanol, ethyl alcohol or normal propyl alcohol
One of alcohol.
(2) complex reaction: anhydrous complexing agent is added from top to complex reaction tower；Silicon tetrafluoride gas is added from bottom
Complex reaction tower；Ocratation complex compound is collected to complex compound storage tank, detects its complexing degree；Complexing degree in 100% or so qualification,
If complexing is spent low, complex compound is sent again to complex reaction tower and is reacted.Tower bottom pressure control of the present invention is in absolute pressure 0.2
Between~0.4Mpa；Coolant cooling is passed through in collet outside the complex reaction tower；Complex reaction temperature is controlled 0~10
Between DEG C.
Equipment used by above-mentioned ocratation complex compound preparation method, including complexing agent storage tank 1, complexing agent delivery pump 2,
Dehydrating tower 3, anhydrous complexing agent storage tank 4, anhydrous complexing agent delivery pump 5, SiF4Steel cylinder 6, complex reaction tower 7, complex compound storage tank 8 and
Vacuum pump 9；The lower transport port of the complexing agent storage tank 1 is through complexing agent delivery pump 2 and 3 lower transport port phase of dehydrating tower
It is logical；The top transmission port of the dehydrating tower 3 is communicated with the top transmission port of anhydrous complexing agent storage tank 4；The anhydrous complexing
The lower transport port of agent storage tank 4 is communicated through anhydrous complexing agent delivery pump 5 with the top transmission port of complex reaction tower 7；It is described
SiF4The top transmission port of steel cylinder 6 is communicated with the lower transport port of complex reaction tower 7；The 7 bottom network of complex reaction tower
Object collection port is closed to communicate with the top transmission port of complex compound storage tank 8；The working port and complex reaction tower of the vacuum pump 9
7 top transmission port communicates.The present invention is externally provided with collet 10 in the complex reaction tower 7.The present invention is in the complex reaction
It is -0.1MPa~1.0MPa pressure gauge that 7 tower top of tower and tower bottom, which are respectively equipped with range,.The present invention is in 7 tower of complex reaction
Bottom is equipped with the thermometer that range is -50~200 DEG C.
Embodiment 1
The present embodiment makees complexing agent with methanol, with SiF4Gas reaction prepares ocratation methanol complex.
Detailed process is as follows.
1, methanol is squeezed into dehydrating tower 3 from complexing agent storage tank 1 by starting complexing agent delivery pump 2, and anhydrous complexing is entered after dehydration
Agent storage tank 4 stores, and detects anhydrous complexing agent water content, is qualification lower than 50ppm, if storing up anhydrous complexing agent higher than the value
Complexing agent in tank 4 squeezes into the dehydration of dehydrating tower 3 again, until qualified.
2, it needs to carry out vacuumize process to entire complex reaction Tower System before reacting, when pressure gauge reading is stablized close
After the numerical value of -0.1Mpa, stop vacuumizing, and keep vacuum.
3, purity is higher than to 99.99% SiF4Gas is passed through in complex reaction tower 7, until pressure gauge reading reaches 0.2Mpa.
Coolant is passed through to complex reaction tower collet simultaneously.
4, anhydrous complexing agent delivery pump is opened, anhydrous complexing agent is added to 7 tower top of complex reaction tower with the flow velocity of 50L/h,
Complexing agent and SiF4Gas carries out complex reaction in complex reaction tower 7, and keeping the temperature of tower bottom complex compound is 5 DEG C, tower bottom pressure
Power meter pressure is in 0.2MPa or so, as gradually SiF is added into complex reaction tower in the progress of reaction4Gas.
5, the ocratation complex compound that reaction generates enters the storage of complex compound storage tank 8, detects its complexing degree, reaches 100% left side
The right side is qualification, returns complex reaction top of tower again if too low and carries out complex reaction.
Embodiment 2.
The present embodiment makees complexing agent with ethyl alcohol, with SiF4Gas reaction prepares ocratation ethanol complex.
Detailed process is as follows.
It is 0 DEG C that preparation process reaction condition, which keeps the temperature of tower bottom complex compound, tower bottom pressure meter pressure is left in 0.25MPa
It is right.
Remaining operating procedure is same as Example 1.
Embodiment 3.
The present embodiment makees complexing agent with normal propyl alcohol, with SiF4Gas reaction prepares ocratation normal propyl alcohol complex compound.
Detailed process is as follows.
It is 2 DEG C, tower bottom pressure meter pressure in 0.3MPa or so that preparation process reaction condition, which keeps the temperature of tower bottom complex compound,.
Remaining operating procedure is same as Example 1.
As examples detailed above 1,2,3 it is found that ocratation complex compound complexing degree made from this method is high, through detecting 100%
Left and right, water content is extremely low, is lower than 50ppm through detection, high-quality further to use chemical exchange method separation silicon isotope to provide
Qualified raw material, this method have it is easily controllable, it is pollution-free, the features such as fully reacting.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (3)
1. a kind of preparation method of ocratation complex compound, which is characterized in that make complexing agent with methanol, with SiF4Gas reaction, packet
Include following steps:
(1) methanol is squeezed into dehydrating tower from complexing agent storage tank by starting complexing agent delivery pump, and anhydrous complexing agent storage tank is entered after dehydration
Storage, detects anhydrous complexing agent water content, is qualification lower than 50ppm, if being higher than the value, by the network in anhydrous complexing agent storage tank
Mixture squeezes into dehydrating tower dehydration again, until qualified；
(2) react before need to entire complex reaction Tower System carry out vacuumize process, when pressure gauge reading stablize close to-
After the numerical value of 0.1Mpa, stop vacuumizing, and keep vacuum；
(3) purity is higher than to 99.99% SiF4Gas is passed through in complex reaction tower, until pressure gauge reading reaches 0.2Mpa；Simultaneously
Coolant is passed through to complex reaction tower collet；
(4) anhydrous complexing agent delivery pump is opened, anhydrous complexing agent, complexing are added to complex reaction column overhead with the flow velocity of 50L/h
Agent and SiF4Gas carries out complex reaction in complex reaction tower, and keeping the temperature of tower bottom complex compound is 5 DEG C, tower bottom pressure gauge pressure
Power is in 0.2MPa or so, as gradually SiF is added into complex reaction tower in the progress of reaction4Gas；
(5) the ocratation complex compound that reaction generates enters the storage of complex compound storage tank, detects its complexing degree, reaching 100% or so is
Qualification, water content are lower than 50ppm, return complex reaction top of tower again if too low and carry out complex reaction；
Equipment used by the ocratation complex compound preparation method, including complexing agent storage tank (1), complexing agent delivery pump (2),
Dehydrating tower (3), anhydrous complexing agent storage tank (4), anhydrous complexing agent delivery pump (5), SiF4Steel cylinder (6), complex reaction tower (7), network
Close object storage tank (8) and vacuum pump (9)；The lower transport port of the complexing agent storage tank (1) is through complexing agent delivery pump (2) and dehydration
Tower (3) lower transport port communicates；The top of the top transmission port of the dehydrating tower (3) and anhydrous complexing agent storage tank (4) passes
Defeated port communicates；The lower transport port of the anhydrous complexing agent storage tank (4) is anti-through anhydrous complexing agent delivery pump (5) and complexing
The top transmission port of tower (7) is answered to communicate；The SiF4The top transmission port of steel cylinder (6) and the bottom of complex reaction tower (7)
Transmission port communicates；The top transmission end of complex reaction tower (7) the bottom complex compound collection port and complex compound storage tank (8)
Mouth communicates；The working port of the vacuum pump (9) is communicated with the top transmission port of complex reaction tower (7)；It is anti-in the complexing
Tower (7) is answered to be externally provided with collet (10)；Complex reaction tower (7) tower top and tower bottom be respectively equipped with range be -0.1MPa~
The pressure gauge of 1.0MPa；The thermometer that range is -50~200 DEG C is equipped in the complex reaction (7) tower bottom.
2. a kind of preparation method of ocratation complex compound, which is characterized in that make complexing agent with ethyl alcohol, with SiF4Gas reaction, packet
Include following steps:
(1) ethyl alcohol is squeezed into dehydrating tower from complexing agent storage tank by starting complexing agent delivery pump, and anhydrous complexing agent storage tank is entered after dehydration
Storage, detects anhydrous complexing agent water content, is qualification lower than 50ppm, if being higher than the value, by the network in anhydrous complexing agent storage tank
Mixture squeezes into dehydrating tower dehydration again, until qualified；
(2) react before need to entire complex reaction Tower System carry out vacuumize process, when pressure gauge reading stablize close to-
After the numerical value of 0.1Mpa, stop vacuumizing, and keep vacuum；
(3) purity is higher than to 99.99% SiF4Gas is passed through in complex reaction tower, until pressure gauge reading reaches 0.2Mpa；Simultaneously
Coolant is passed through to complex reaction tower collet；
(4) anhydrous complexing agent delivery pump is opened, anhydrous complexing agent, complexing are added to complex reaction column overhead with the flow velocity of 50L/h
Agent and SiF4Gas carries out complex reaction in complex reaction tower, and keeping the temperature of tower bottom complex compound is 0 DEG C, tower bottom pressure gauge pressure
Power is in 0.25MPa or so, as gradually SiF is added into complex reaction tower in the progress of reaction4Gas；
(5) the ocratation complex compound that reaction generates enters the storage of complex compound storage tank, detects its complexing degree, reaching 100% or so is
Qualification, water content are lower than 50ppm, return complex reaction top of tower again if too low and carry out complex reaction；
Equipment used by the ocratation complex compound preparation method, including complexing agent storage tank (1), complexing agent delivery pump (2),
Dehydrating tower (3), anhydrous complexing agent storage tank (4), anhydrous complexing agent delivery pump (5), SiF4Steel cylinder (6), complex reaction tower (7), network
Close object storage tank (8) and vacuum pump (9)；The lower transport port of the complexing agent storage tank (1) is through complexing agent delivery pump (2) and dehydration
Tower (3) lower transport port communicates；The top of the top transmission port of the dehydrating tower (3) and anhydrous complexing agent storage tank (4) passes
Defeated port communicates；The lower transport port of the anhydrous complexing agent storage tank (4) is anti-through anhydrous complexing agent delivery pump (5) and complexing
The top transmission port of tower (7) is answered to communicate；The SiF4The top transmission port of steel cylinder (6) and the bottom of complex reaction tower (7)
Transmission port communicates；The top transmission end of complex reaction tower (7) the bottom complex compound collection port and complex compound storage tank (8)
Mouth communicates；The working port of the vacuum pump (9) is communicated with the top transmission port of complex reaction tower (7)；It is anti-in the complexing
Tower (7) is answered to be externally provided with collet (10)；Complex reaction tower (7) tower top and tower bottom be respectively equipped with range be -0.1MPa~
The pressure gauge of 1.0MPa；The thermometer that range is -50~200 DEG C is equipped in the complex reaction (7) tower bottom.
3. a kind of preparation method of ocratation complex compound, which is characterized in that make complexing agent with normal propyl alcohol, with SiF4Gas is anti-
It answers, includes the following steps:
(1) normal propyl alcohol is squeezed into dehydrating tower from complexing agent storage tank by starting complexing agent delivery pump, and anhydrous complexing agent is entered after dehydration and is stored up
Tank storage, detects anhydrous complexing agent water content, is qualification lower than 50ppm, will be in anhydrous complexing agent storage tank if being higher than the value
Complexing agent squeezes into dehydrating tower dehydration again, until qualified；
(2) react before need to entire complex reaction Tower System carry out vacuumize process, when pressure gauge reading stablize close to-
After the numerical value of 0.1Mpa, stop vacuumizing, and keep vacuum；
(3) purity is higher than to 99.99% SiF4Gas is passed through in complex reaction tower, until pressure gauge reading reaches 0.2Mpa；Simultaneously
Coolant is passed through to complex reaction tower collet；
(4) anhydrous complexing agent delivery pump is opened, anhydrous complexing agent, complexing are added to complex reaction column overhead with the flow velocity of 50L/h
Agent and SiF4Gas carries out complex reaction in complex reaction tower, and keeping the temperature of tower bottom complex compound is 2 DEG C, tower bottom pressure gauge pressure
Power is in 0.3MPa or so, as gradually SiF is added into complex reaction tower in the progress of reaction4Gas；
(5) the ocratation complex compound that reaction generates enters the storage of complex compound storage tank, detects its complexing degree, reaching 100% or so is
Qualification, water content are lower than 50ppm, return complex reaction top of tower again if too low and carry out complex reaction；
Equipment used by the ocratation complex compound preparation method, including complexing agent storage tank (1), complexing agent delivery pump (2),
Dehydrating tower (3), anhydrous complexing agent storage tank (4), anhydrous complexing agent delivery pump (5), SiF4Steel cylinder (6), complex reaction tower (7), network
Close object storage tank (8) and vacuum pump (9)；The lower transport port of the complexing agent storage tank (1) is through complexing agent delivery pump (2) and dehydration
Tower (3) lower transport port communicates；The top of the top transmission port of the dehydrating tower (3) and anhydrous complexing agent storage tank (4) passes
Defeated port communicates；The lower transport port of the anhydrous complexing agent storage tank (4) is anti-through anhydrous complexing agent delivery pump (5) and complexing
The top transmission port of tower (7) is answered to communicate；The SiF4The top transmission port of steel cylinder (6) and the bottom of complex reaction tower (7)
Transmission port communicates；The top transmission end of complex reaction tower (7) the bottom complex compound collection port and complex compound storage tank (8)
Mouth communicates；The working port of the vacuum pump (9) is communicated with the top transmission port of complex reaction tower (7)；It is anti-in the complexing
Tower (7) is answered to be externally provided with collet (10)；Complex reaction tower (7) tower top and tower bottom be respectively equipped with range be -0.1MPa~
The pressure gauge of 1.0MPa；The thermometer that range is -50~200 DEG C is equipped in the complex reaction (7) tower bottom.
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 CN105524101A (en) | 2016-04-27 |
| CN105524101B true CN105524101B (en) | 2019-01-04 |
Family
ID=55766663
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510945826.XA Expired - Fee Related CN105524101B (en) | 2015-12-17 | 2015-12-17 | Ocratation complex compound preparation method and its used equipment |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105524101B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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 |
|---|
| Separation of Silicon Isotopes by Chemical Exchange between Silicon Tetrafluoride and Its Complex Compounds with Aliphatic Alcohols;A. V. Khoroshilov等，;《Theoretical Foundations of Chemical Engineering》;20101231;第569-573页，尤其是第569页右栏 * |
| THE INTERACTION OF SILICON TETRAFLUORIDE WITH METHANOL;J. P. GUERTIN等，;《Canadian Journal of Chemistry》;19631231;第1477-第1484页，尤其是第1477页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105524101A (en) | 2016-04-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106145037B (en) | The method that the device and High Purity Hydrogen processed of hydrogen are recycled from silicon epitaxial furnace emptying end gas | |
| Bork et al. | Simple descriptors for proton-conducting perovskites from density functional theory | |
| CN106238725A (en) | A kind of thermal conductance copper powder of high wicking rate low-apparent-density and preparation method thereof | |
| CN102503424B (en) | Method for increasing sintering efficiency of FeSe superconducting material | |
| CN105524101B (en) | Ocratation complex compound preparation method and its used equipment | |
| CN105366639A (en) | Portable hydrogen production equipment by automatic control of aluminum-water reaction | |
| CN106854715B (en) | A kind of lanthanum-magnesium containing yttrium-nickel system AB3Type hydrogen storage alloy and its preparation process | |
| CN102795608B (en) | Method for purification and recovery of argon, nitrogen and hydrogen by rare earth alloy-sponge titanium mixture | |
| CN104140085B (en) | The apparatus and method of water and carbon dioxide in a kind of deep removal nitrous oxide | |
| CN1990380B (en) | Technique for purifying and recovering argon gas by rare earth lanthanide series radical alloy degasser in single-crystal silicon preparation | |
| CN106966364A (en) | A kind of synthesis technique of deuterate aluminium lithium | |
| CN202494273U (en) | Helium purification device in condensation method | |
| CN103979488B (en) | Adopt the technique of MAGNESIUM METAL continuous seepage hydrogen and magnesium hydroxide | |
| CN102765723B (en) | Method for synthesizing KSi hydrogen storage alloy | |
| CN105664718B (en) | The production enrichment of multitower separation28Si、29Si and30Si methods and its used device | |
| CN206051561U (en) | A kind of ultrapure carbon dioxide production system | |
| CN204702506U (en) | The device of recover hydrogen from silicon epitaxial furnace emptying end gas | |
| CN102942539B (en) | Epoxy propane recovery and purification process | |
| CN105776136A (en) | Device and method used for recycling hydrogen from chlor-alkali industry vented tail gas and preparing high purity hydrogen | |
| CN202778416U (en) | Device for compositing dicumyl peroxide | |
| CN102928452B (en) | A kind of assay method of imidazole type ion liquid negative ion hydrogen bond Forming ability | |
| CN104909337A (en) | Lithium metaborate hydrogen storage composite material adulterated with lithium hydride and preparation method thereof | |
| CN104843653B (en) | Method and the equipment therefor of ultra-clean and high-purity sulphuric acid is prepared in film absorption | |
| CN207108476U (en) | The hydrogen formation apparatus of output voltage stabilizing can be automatically adjusted | |
| CN206106775U (en) | Coolant liquid separator under vacuum processing environment |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20190104 Termination date: 20191217 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |