CN116832615B - Continuous production process method for silicon isotopes - Google Patents
Continuous production process method for silicon isotopes Download PDFInfo
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- CN116832615B CN116832615B CN202311092097.9A CN202311092097A CN116832615B CN 116832615 B CN116832615 B CN 116832615B CN 202311092097 A CN202311092097 A CN 202311092097A CN 116832615 B CN116832615 B CN 116832615B
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- 238000000034 method Methods 0.000 title claims abstract description 51
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 36
- 239000010703 silicon Substances 0.000 title claims abstract description 36
- 238000010924 continuous production Methods 0.000 title claims abstract description 30
- 230000000536 complexating effect Effects 0.000 claims abstract description 102
- 235000011194 food seasoning agent Nutrition 0.000 claims abstract description 55
- 239000008139 complexing agent Substances 0.000 claims abstract description 45
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000011541 reaction mixture Substances 0.000 claims abstract description 35
- 239000000047 product Substances 0.000 claims abstract description 24
- 238000000926 separation method Methods 0.000 claims abstract description 21
- 239000006227 byproduct Substances 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 238000000354 decomposition reaction Methods 0.000 claims description 29
- 238000010668 complexation reaction Methods 0.000 claims description 27
- 239000012071 phase Substances 0.000 claims description 22
- 239000007788 liquid Substances 0.000 claims description 19
- 239000012535 impurity Substances 0.000 claims description 14
- RDOXTESZEPMUJZ-UHFFFAOYSA-N anisole Chemical group COC1=CC=CC=C1 RDOXTESZEPMUJZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000009833 condensation Methods 0.000 claims description 8
- 230000005494 condensation Effects 0.000 claims description 8
- 238000000605 extraction Methods 0.000 claims description 8
- 238000007599 discharging Methods 0.000 claims description 6
- 239000007791 liquid phase Substances 0.000 claims description 5
- UZKWTJUDCOPSNM-UHFFFAOYSA-N methoxybenzene Substances CCCCOC=C UZKWTJUDCOPSNM-UHFFFAOYSA-N 0.000 claims description 5
- WRECIMRULFAWHA-UHFFFAOYSA-N trimethyl borate Chemical compound COB(OC)OC WRECIMRULFAWHA-UHFFFAOYSA-N 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 238000011112 process operation Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 36
- 238000005086 pumping Methods 0.000 description 6
- 238000000746 purification Methods 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000005372 isotope separation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D59/00—Separation of different isotopes of the same chemical element
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D59/00—Separation of different isotopes of the same chemical element
- B01D59/02—Separation by phase transition
- B01D59/04—Separation by phase transition by distillation
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Silicon Compounds (AREA)
Abstract
The invention provides a silicon isotope continuous production process method, which applies a novel silicon isotope continuous production device and matched process parameters and comprises the following steps: sequentially injecting a complexing agent and silicon tetrafluoride into a seasoning tower for reaction, and injecting the reaction mixture into the complexing tower when the mole ratio of the complexing agent to the silicon tetrafluoride in the reaction mixture reaches 1.5-3; the reaction mixture circularly reacts along a complexing tower, an exchange tower and a decomposing tower to obtain a complexing product; when the abundance of Si28 in the complex reaches the target abundance, the frit column continues to inject the reaction mixture into the exchange column at the forefront, withdrawing the Si28 product from the bottom of the complex column and withdrawing the by-product from the bottom of the exchange column at the rearmost. The continuous production process of the silicon isotope can realize industrial production and obtain qualified commercial products, and can continuously produce the silicon isotope products, and has the advantages of low cost, high separation efficiency, simple process operation and simple control method.
Description
Technical Field
The invention belongs to the field of silicon isotope separation, and particularly relates to a continuous production process method of silicon isotopes.
Background
At present, methods for realizing silicon isotope separation mainly comprise a low-temperature rectification method, a gas centrifugation method, a laser method, a chemical exchange method and the like. Among them, the chemical exchange method has been the most promising method for realizing industrialized separation of silicon isotopes due to its advantages of high separation coefficient, large throughput, and the like.
The Chinese patent publication No. CN105524101A (publication No. 2016: 4: 27) discloses a preparation method of silicon tetrafluoride complex and equipment adopted by the method, methanol, ethanol or n-propanol is used as complexing agent to carry out complexation reaction with silicon tetrafluoride to obtain silicon tetrafluoride complex with high complexation degree, but the intermittent operation mode is adopted in the patent, because the number of equipment required for producing silicon isotopes by using a chemical exchange rectification method is very large, the process parameters are very precise, if an intermittent process is adopted, various parameters need to be readjusted after each batch of products are produced, the operation is extremely complex, and the method is limited by control level reasons, so that the abundance level of the current separation products is unstable.
Disclosure of Invention
In view of the above, the present invention aims to provide a continuous production process for silicon isotopes, which is to continuously extract products and match corresponding production process parameters, so as to greatly increase production efficiency.
In order to achieve the above purpose, the technical scheme of the invention is realized as follows:
the continuous production process of the silicon isotope comprises a seasoning tower, wherein a tower bottom feed inlet of the seasoning tower is communicated with a silicon tetrafluoride gas tank, a tower top feed inlet of the seasoning tower is communicated with a complexing agent tank, and a tower bottom discharge outlet of the seasoning tower is communicated with a tower top circulation port of the seasoning tower;
the tower kettle feed inlet of the complexing tower is communicated with the tower kettle discharge outlet of the seasoning tower;
the device comprises a plurality of exchange towers, wherein a plurality of top feed inlets of the exchange towers positioned at the forefront are communicated with a bottom discharge port of a complexation tower and a bottom discharge port of a seasoning tower in sequence;
the middle feed inlet of the decomposing tower is communicated with the discharge outlet at the bottom of the rearmost exchange tower;
the middle feed inlet of the impurity removing tower is communicated with the tower kettle discharge outlet of the decomposing tower, and the upper discharge outlet of the impurity removing tower is communicated with the tower top circulation port of the complexing tower;
the middle feed inlet of the gas-liquid separation tank is communicated with the top discharge outlet of the decomposing tower, the gas-phase discharge outlet of the gas-liquid separation tank is communicated with the circulating port at the bottom of the rearmost exchange tower, and the liquid-phase discharge outlet of the gas-liquid separation tank is communicated with the circulating port at the bottom of the decomposing tower;
the continuous production process method of the silicon isotope comprises the following steps:
s1, sequentially injecting a complexing agent and silicon tetrafluoride into a seasoning tower for reaction to obtain a reaction mixture, and injecting the reaction mixture into the complexing tower when the mole ratio of the complexing agent to the silicon tetrafluoride in the reaction mixture reaches 1.5-3;
s2, carrying out cyclic reaction on the reaction mixture along a complexing tower, an exchange tower and a decomposing tower to obtain a complexing product;
and S3, when the abundance of Si28 in the complexing product reaches the target abundance, continuously injecting a reaction mixture into the exchange tower positioned at the forefront by the seasoning tower, extracting Si28 product from the bottom of the complexing tower, and extracting byproducts from the bottom of the exchange tower positioned at the rearmost.
Specifically, the method comprises the following steps:
s1, a seasoning working section: in the working section, firstly, introducing a complexing agent into a seasoning tower, starting a self-circulation pump of the tower body of the seasoning tower, starting condensation of the tower body, then introducing silicon tetrafluoride at a certain flow rate, carrying out complexation reaction in the seasoning tower to generate a reaction mixture, detecting the complexation degree of the reaction mixture at fixed time, and closing the circulation pump of the tower body when the mole ratio of the complexing agent to the silicon tetrafluoride in the reaction mixture reaches 1.5-3.0;
s2, complexing working section: the reaction mixture is pumped into a complexing tower, a condensing jacket is arranged on the body of the complexing tower, the temperature in the complexing tower is ensured to be within a certain range by controlling the flow of condensed liquid, a complex is generated in the complexing tower, then the complex sequentially passes through a plurality of exchange towers and then enters a decomposing tower, a complexing agent is obtained at a tower kettle discharge port of the decomposing tower, and then flows into a impurity removing tower, the complexing agent subjected to impurity removal is extracted at an upper section discharge port of the impurity removing tower and flows into a circulating port at the top of the complexing tower; the method comprises the steps that silicon tetrafluoride gas is obtained from a discharge hole at the top of a decomposing tower, enters a circulating hole at the bottom of an exchange tower positioned at the rearmost part after passing through a gas buffer tank, sequentially passes through a plurality of exchange towers from back to front, returns to the circulating hole at the bottom of a complexing tower, and is subjected to complexing reaction with complexing agent obtained from stump on the complexing tower to obtain a complexing product;
and S3, continuously injecting a reaction mixture into the exchange tower positioned at the forefront by the seasoning tower when all parameters in the system reach stable and the abundance of Si28 in the complex product reaches the target abundance, extracting Si28 product from the bottom of the complex tower and extracting byproducts from the bottom of the exchange tower positioned at the rearmost.
Preferably, a decomposition preheater is arranged between the decomposition tower and the exchange tower positioned at the rearmost part, a bottom feed inlet of the decomposition preheater is communicated with a bottom discharge outlet of the exchange tower positioned at the rearmost part, and a top discharge outlet of the decomposition preheater is communicated with a middle feed inlet of the decomposition tower.
Preferably, a gas phase buffer tank is arranged between the gas-liquid separation tank and the exchange tower positioned at the rearmost, a middle feeding port of the gas phase buffer tank is communicated with a gas phase discharging port of the gas-liquid separation tank, a gas phase discharging port of the gas phase buffer tank is communicated with a circulating port positioned at the bottom of the rearmost exchange tower, and a liquid phase discharging port at the bottom of the gas phase buffer tank is communicated with a circulating port of a tower kettle of the decomposing tower.
Preferably, the sum of the heights of the packed sections of all the exchange columns is not less than 10 m.
Preferably, the bottom of the complexing tower is provided with a Si28 extraction outlet, and the bottom of the exchange tower positioned at the rearmost part is provided with a byproduct extraction outlet.
Preferably, the temperature of the tower body of the seasoning tower in the step S1 is 0-100 ℃, the pressure in the tower is 90-300kPa, and the temperature in the complexing tower in the step S2 is 0-100 ℃.
Preferably, the complexing agent is anisole or trimethyl borate.
Preferably, the target abundance is 99.5% or more.
Preferably, the decomposition preheater is operated at a temperature of 100-150 ℃ and the decomposer is operated at a temperature of 150-300 ℃.
Compared with the prior art, the silicon isotope continuous production process method provided by the invention has the following advantages:
the continuous production process of the silicon isotope can realize industrial production and obtain qualified commercial products, and can continuously produce the silicon isotope products, and has the advantages of low cost, high separation efficiency, simple process operation and simple control method.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention. In the drawings:
fig. 1 is a schematic structural diagram of a silicon isotope continuous production apparatus according to an embodiment of the present invention.
Reference numerals illustrate:
1. a seasoning tower; 2. a silicon tetrafluoride gas tank; 3. a complexing agent tank; 4. a complexing tower; 5. an exchange column; 6. a decomposing tower; 7. a impurity removing tower; 8. a gas-liquid separation tank; 9. a decomposition preheater; 10. a gas phase buffer tank; 11. a Si28 extraction port; 12. and a byproduct extraction port.
Detailed Description
It should be noted that, without conflict, the embodiments of the present invention and features of the embodiments may be combined with each other.
The invention will be described in detail below with reference to the drawings in connection with embodiments.
As shown in FIG. 1, the continuous production device for silicon isotopes used in the embodiment comprises a seasoning tower 1, a complexing tower 4, an exchange tower 5, a decomposing tower 6, an impurity removing tower 7 and a gas-liquid separating tank 8, wherein a tower bottom feed port of the seasoning tower 1 is communicated with a silicon tetrafluoride gas tank 2, a tower top feed port of the seasoning tower 1 is communicated with a complexing agent tank 3, a tower bottom discharge port of the seasoning tower 1 is communicated with a tower top circulation port of the seasoning tower 1, a tower bottom feed port of the complexing tower 4 is communicated with a tower bottom discharge port of the seasoning tower 1, si28 extraction ports 11 are arranged at the bottom of the complexing tower 4, three exchange towers 5 are sequentially communicated, the sum of the heights of filling sections of the three exchange towers is 10 meters, a tower top feed port of a first exchange tower is communicated with a tower bottom discharge port of the complexing tower 4 and a tower bottom circulation port of the seasoning tower 1, a tower top feed back port of the first exchange tower is communicated with a tower bottom circulation port of the complexing tower 4, the bottom discharge port of the exchange tower positioned at the front is sequentially communicated with the top feed port of the exchange tower positioned at the rear, the top return port of the exchange tower 5 positioned at the rear is sequentially communicated with the bottom circulation port of the exchange tower positioned at the front, the bottom of the third exchange tower is provided with a byproduct extraction port 12, the middle feed port of the decomposition tower 6 is communicated with the bottom discharge port of the third exchange tower, the middle feed port of the impurity removal tower 7 is communicated with the bottom discharge port of the decomposition tower 6, the upper discharge port of the impurity removal tower 7 is communicated with the top circulation port of the complexation tower 4, the middle feed port of the gas-liquid separation tank 8 is communicated with the top discharge port of the decomposition tower 6, the gas-phase discharge port of the gas-liquid separation tank 8 is communicated with the bottom circulation port of the third exchange tower, a decomposition preheater 9 is arranged between the decomposition tower 6 and the third exchange tower, the bottom feed inlet of the decomposition preheater 9 is communicated with the bottom feed outlet of the third exchange tower 5, the top feed outlet of the decomposition preheater 9 is communicated with the middle feed inlet of the decomposition tower 6, a gas phase buffer tank 10 is arranged between the gas-liquid separation tank 8 and the third exchange tower, the middle feed inlet of the gas phase buffer tank 10 is communicated with the gas phase feed outlet of the gas-liquid separation tank 8, the gas phase feed outlet of the gas phase buffer tank 10 is communicated with the bottom circulation port of the third exchange tower, and the liquid phase feed outlet at the bottom of the gas phase buffer tank 10 is communicated with the bottom circulation port of the decomposition tower 6.
Example 1
Starting a seasoning tower, introducing 100kg of anisole into the seasoning tower, starting a self-circulation pump of a tower body, starting condensation of the tower body, introducing 62kg of silicon tetrafluoride at a certain flow rate, carrying out complexation reaction in the seasoning tower to generate a reaction mixture, ensuring that the temperature of the tower body is maintained at 5+/-5 ℃, simultaneously ensuring that the pressure in the tower is maintained at 90+/-10 kPa, and pumping the reaction mixture into the complexation tower when the mole ratio of the complexing agent to the silicon tetrafluoride in the reaction mixture reaches 1.5. The complexing tower body is provided with a jacket. The temperature in the complexation tower is kept at 5+/-5 ℃ by controlling the flow of the medium. The complex generated in the complexing tower is pumped into an exchange tower through a material pump, exchange rectification is carried out in the exchange tower, then the complex in the last exchange tower is pumped into a decomposition preheater through the material pump for preheating and then enters a decomposer, wherein the concentrated silicon tetrafluoride generated in the decomposer enters the last exchange tower from the top end of the decomposer, and then sequentially passes through each exchange tower and then enters the complexing tower from the bottom of the complexing tower; the complexing agent generated in the decomposer enters a purifying tower for rectification and purification to obtain pure complexing agent, and then the complexing agent is pumped into the top of the complexing tower to carry out complexing reaction with silicon tetrafluoride gas entering from the bottom of the complexing tower. And (3) performing a circulation process, when the abundance of Si28 in the complex at the bottom of the complexing tower is more than or equal to 99.5%, closing a material conveying device from the material making tower to the complexing tower, opening a material conveying device from the material making tower to the exchange tower, and extracting a complex product with the abundance of Si28 being more than or equal to 99.5% from the bottom of the complexing tower and a byproduct from the bottom of the last exchange tower, thereby performing continuous production of silicon isotopes.
Example 2
Starting a seasoning tower, introducing 100kg of anisole into the seasoning tower, starting a self-circulation pump of a tower body, starting condensation of the tower body, introducing 32kg of silicon tetrafluoride at a certain flow rate, carrying out complexation reaction in the seasoning tower to generate a reaction mixture, ensuring that the temperature of the tower body is maintained at 45+/-5 ℃, simultaneously ensuring that the pressure in the tower is maintained at 150+/-10 kPa, and pumping the reaction mixture into the complexation tower when the mole ratio of complexing agent to silicon tetrafluoride in the reaction mixture reaches 2. The complexing tower body is provided with a jacket. The temperature in the complexation tower is kept at 45+/-5 ℃ by controlling the flow of the medium. The complex in the complexing tower is pumped into the exchange tower through a material pump, exchange rectification is carried out in the exchange tower, then the complex in the last exchange tower is pumped into a decomposition preheater through the material pump for preheating and then enters a decomposer, wherein the concentrated silicon tetrafluoride generated in the decomposer enters the last exchange tower from the top end of the decomposer, and then sequentially passes through each exchange tower and then enters the complexing tower from the bottom of the complexing tower; the complexing agent generated in the decomposer enters a purifying tower for rectification and purification to obtain pure complexing agent, and then the complexing agent is pumped into the top of the complexing tower to carry out complexing reaction with silicon tetrafluoride gas entering from the bottom of the complexing tower. And (3) performing a circulation process, when the abundance of Si28 in the complex at the bottom of the complexing tower is more than or equal to 99.5%, closing a material conveying device from the material making tower to the complexing tower, opening a material conveying device from the material making tower to the exchange tower, and extracting a complex product with the abundance of Si28 being more than or equal to 99.5% from the bottom of the complexing tower and a byproduct from the bottom of the last exchange tower, thereby performing continuous production of silicon isotopes.
Example 3
Starting a seasoning tower, introducing 100kg of anisole into the seasoning tower, starting a self-circulation pump of a tower body, starting condensation of the tower body, introducing 45kg of silicon tetrafluoride at a certain flow rate, carrying out complexation reaction in the seasoning tower to generate a reaction mixture, ensuring that the temperature of the tower body is maintained at 95+/-5 ℃, simultaneously ensuring that the pressure in the tower is maintained at 290+/-10 kPa, and pumping the complex into the complexation tower when the mole ratio of the complexing agent to the silicon tetrafluoride in the reaction mixture reaches 3. The complexing tower body is provided with a jacket. The temperature in the complexation tower is kept at 95+/-5 ℃ by controlling the flow of the medium. The complex in the complexing tower is pumped into the exchange tower through a material pump, exchange rectification is carried out in the exchange tower, then the complex in the last exchange tower is pumped into a decomposition preheater through the material pump for preheating and then enters a decomposer, wherein the concentrated silicon tetrafluoride generated in the decomposer enters the last exchange tower from the top end of the decomposer, and then sequentially passes through each exchange tower and then enters the complexing tower from the bottom of the complexing tower; the complexing agent generated in the decomposer enters a purifying tower for rectification and purification to obtain pure complexing agent, and then the complexing agent is pumped into the top of the complexing tower to carry out complexing reaction with silicon tetrafluoride gas entering from the bottom of the complexing tower. And (3) performing a circulation process, when the abundance of Si28 in the complex at the bottom of the complexing tower is more than or equal to 99.5%, closing a material conveying device from the material making tower to the complexing tower, opening a material conveying device from the material making tower to the exchange tower, and extracting a complex product with the abundance of Si28 being more than or equal to 99.5% from the bottom of the complexing tower and a byproduct from the bottom of the last exchange tower, thereby performing continuous production of silicon isotopes.
Example 4
Starting a seasoning tower, introducing 100kg of trimethyl borate into the seasoning tower, starting a self-circulation pump of a tower body, starting condensation of the tower body, introducing 66kg of silicon tetrafluoride at a certain flow rate, carrying out complexation reaction in the seasoning tower to generate a reaction mixture, ensuring that the temperature of the tower body is maintained at 5+/-5 ℃, simultaneously ensuring that the pressure in the tower is maintained at 90+/-10 kPa, and pumping the reaction mixture into the complexation tower when the mole ratio of complexing agent to the silicon tetrafluoride in the reaction mixture reaches 1.5. The complexing tower body is provided with a jacket. The temperature in the complexation tower is kept at 5+/-5 ℃ by controlling the flow of the medium. The complex generated in the complexing tower is pumped into an exchange tower through a material pump, exchange rectification is carried out in the exchange tower, then the complex in the last exchange tower is pumped into a decomposition preheater through the material pump for preheating and then enters a decomposer, wherein the concentrated silicon tetrafluoride generated in the decomposer enters the last exchange tower from the top end of the decomposer, and then sequentially passes through each exchange tower and then enters the complexing tower from the bottom of the complexing tower; the complexing agent generated in the decomposer enters a purifying tower for rectification and purification to obtain pure complexing agent, and then the complexing agent is pumped into the top of the complexing tower to carry out complexing reaction with silicon tetrafluoride gas entering from the bottom of the complexing tower. And (3) performing a circulation process, when the abundance of Si28 in the complex at the bottom of the complexing tower is more than or equal to 99.5%, closing a material conveying device from the material making tower to the complexing tower, opening a material conveying device from the material making tower to the exchange tower, and extracting a complex product with the abundance of Si28 being more than or equal to 99.5% from the bottom of the complexing tower and a byproduct from the bottom of the last exchange tower, thereby performing continuous production of silicon isotopes.
Example 5
Starting a seasoning tower, introducing 100kg of trimethyl borate into the seasoning tower, starting a self-circulation pump of a tower body, starting condensation of the tower body, introducing 50kg of silicon tetrafluoride at a certain flow rate, carrying out complexation reaction in the seasoning tower to generate a reaction mixture, ensuring that the temperature of the tower body is maintained at 45+/-5 ℃, simultaneously ensuring that the pressure in the tower is maintained at 150+/-10 kPa, and pumping the reaction mixture into the complexation tower when the mole ratio of complexing agent to the silicon tetrafluoride in the reaction mixture reaches 2. The complexing tower body is provided with a jacket. The temperature in the complexation tower is kept at 45+/-5 ℃ by controlling the flow of the medium. The complex in the complexing tower is pumped into the exchange tower through a material pump, exchange rectification is carried out in the exchange tower, then the complex in the last exchange tower is pumped into a decomposition preheater through the material pump for preheating and then enters a decomposer, wherein the concentrated silicon tetrafluoride generated in the decomposer enters the last exchange tower from the top end of the decomposer, and then sequentially passes through each exchange tower and then enters the complexing tower from the bottom of the complexing tower; the complexing agent generated in the decomposer enters a purifying tower for rectification and purification to obtain pure complexing agent, and then the complexing agent is pumped into the top of the complexing tower to carry out complexing reaction with silicon tetrafluoride gas entering from the bottom of the complexing tower. And (3) performing a circulation process, when the abundance of Si28 in the complex at the bottom of the complexing tower is more than or equal to 99.5%, closing a material conveying device from the material making tower to the complexing tower, opening a material conveying device from the material making tower to the exchange tower, and extracting a complex product with the abundance of Si28 being more than or equal to 99.5% from the bottom of the complexing tower and a byproduct from the bottom of the last exchange tower, thereby performing continuous production of silicon isotopes.
Example 6
Starting a seasoning tower, introducing 100kg of trimethyl borate into the seasoning tower, starting a self-circulation pump of a tower body, starting condensation of the tower body, introducing 33kg of silicon tetrafluoride at a certain flow rate, carrying out complexation reaction in the seasoning tower to generate a reaction mixture, ensuring that the temperature of the tower body is maintained at 95+/-5 ℃, simultaneously ensuring that the pressure in the tower is maintained at 290+/-10 kPa, and pumping the complex into the complexation tower when the mole ratio of complexing agent to the silicon tetrafluoride in the reaction mixture reaches 3. The complexing tower body is provided with a jacket. The temperature in the complexation tower is kept at 95+/-5 ℃ by controlling the flow of the medium. The complex in the complexing tower is pumped into the exchange tower through a material pump, exchange rectification is carried out in the exchange tower, then the complex in the last exchange tower is pumped into a decomposition preheater through the material pump for preheating and then enters a decomposer, wherein the concentrated silicon tetrafluoride generated in the decomposer enters the last exchange tower from the top end of the decomposer, and then sequentially passes through each exchange tower and then enters the complexing tower from the bottom of the complexing tower; the complexing agent generated in the decomposer enters a purifying tower for rectification and purification to obtain pure complexing agent, and then the complexing agent is pumped into the top of the complexing tower to carry out complexing reaction with silicon tetrafluoride gas entering from the bottom of the complexing tower. And (3) performing a circulation process, when the abundance of Si28 in the complex at the bottom of the complexing tower is more than or equal to 99.5%, closing a material conveying device from the material making tower to the complexing tower, opening a material conveying device from the material making tower to the exchange tower, and extracting a complex product with the abundance of Si28 being more than or equal to 99.5% from the bottom of the complexing tower and a byproduct from the bottom of the last exchange tower, thereby performing continuous production of silicon isotopes.
Claims (9)
1. The continuous production process method for the silicon isotopes is characterized in that the continuous production device for the silicon isotopes comprises a seasoning tower, wherein a tower bottom feed inlet of the seasoning tower is communicated with a silicon tetrafluoride gas tank, a tower top feed inlet of the seasoning tower is communicated with a complexing agent tank, and a tower bottom discharge outlet of the seasoning tower is communicated with a tower top circulation port of the seasoning tower;
the tower kettle feed inlet of the complexing tower is communicated with the tower kettle discharge outlet of the seasoning tower;
the device comprises a plurality of exchange towers, wherein a plurality of top feed inlets of the exchange towers positioned at the forefront are communicated with a bottom discharge port of a complexation tower and a bottom discharge port of a seasoning tower in sequence;
the middle feed inlet of the decomposing tower is communicated with the discharge outlet at the bottom of the rearmost exchange tower;
the middle feed inlet of the impurity removing tower is communicated with the tower kettle discharge outlet of the decomposing tower, and the upper discharge outlet of the impurity removing tower is communicated with the tower top circulation port of the complexing tower;
the middle feed inlet of the gas-liquid separation tank is communicated with the top discharge outlet of the decomposing tower, the gas-phase discharge outlet of the gas-liquid separation tank is communicated with the circulating port at the bottom of the rearmost exchange tower, and the liquid-phase discharge outlet of the gas-liquid separation tank is communicated with the circulating port at the bottom of the decomposing tower;
the continuous production process method of the silicon isotope comprises the following steps:
s1, a seasoning working section: in the working section, firstly, introducing a complexing agent into a seasoning tower, starting a self-circulation pump of the tower body of the seasoning tower, starting condensation of the tower body, then introducing silicon tetrafluoride at a certain flow rate, carrying out complexation reaction in the seasoning tower to generate a reaction mixture, detecting the complexation degree of the reaction mixture at fixed time, and closing the circulation pump of the tower body when the mole ratio of the complexing agent to the silicon tetrafluoride in the reaction mixture reaches 1.5-3.0;
s2, complexing working section: the reaction mixture is pumped into a complexing tower, a condensing jacket is arranged on the body of the complexing tower, the temperature in the complexing tower is ensured to be within a certain range by controlling the flow of condensed liquid, a complex is generated in the complexing tower, then the complex sequentially passes through a plurality of exchange towers and then enters a decomposing tower, a complexing agent is obtained at a tower kettle discharge port of the decomposing tower, and then flows into a impurity removing tower, the complexing agent subjected to impurity removal is extracted at an upper section discharge port of the impurity removing tower and flows into a circulating port at the top of the complexing tower; the method comprises the steps that silicon tetrafluoride gas is obtained from a discharge hole at the top of a decomposing tower, enters a circulating hole at the bottom of an exchange tower positioned at the rearmost part after passing through a gas buffer tank, sequentially passes through a plurality of exchange towers from back to front, returns to the circulating hole at the bottom of a complexing tower, and is subjected to complexing reaction with complexing agent obtained from stump on the complexing tower to obtain a complexing product;
and S3, continuously injecting a reaction mixture into the exchange tower positioned at the forefront by the seasoning tower when all parameters in the system reach stable and the abundance of Si28 in the complex product reaches the target abundance, extracting Si28 product from the bottom of the complex tower and extracting byproducts from the bottom of the exchange tower positioned at the rearmost.
2. The silicon isotope continuous production process according to claim 1, characterized in that: a decomposition preheater is arranged between the decomposition tower and the exchange tower positioned at the rearmost part, a bottom feed inlet of the decomposition preheater is communicated with a bottom discharge outlet of the exchange tower positioned at the rearmost part, and a top discharge outlet of the decomposition preheater is communicated with a middle feed inlet of the decomposition tower.
3. The silicon isotope continuous production process according to claim 1, characterized in that: the gas-liquid separation tank is provided with a gas phase buffer tank between the gas-liquid separation tank and the exchange tower positioned at the rearmost, a middle feeding hole of the gas phase buffer tank is communicated with a gas phase discharging hole of the gas-liquid separation tank, a gas phase discharging hole of the gas phase buffer tank is communicated with a circulating hole positioned at the bottom of the exchange tower positioned at the rearmost, and a liquid phase discharging hole at the bottom of the gas phase buffer tank is communicated with a circulating hole of a tower bottom of the decomposing tower.
4. The silicon isotope continuous production process according to claim 1, characterized in that: the sum of the heights of the filling sections of all the exchange towers is more than or equal to 10 meters.
5. The silicon isotope continuous production process according to claim 1, characterized in that: the bottom of the complexing tower is provided with a Si28 extraction port, and the bottom of the exchange tower positioned at the rearmost part is provided with a byproduct extraction port.
6. The silicon isotope continuous production process according to claim 1, characterized in that: the temperature of the tower body of the seasoning tower in the step S1 is 0-100 ℃, the pressure in the tower is 90-300kPa, and the temperature in the complexing tower in the step S2 is 0-100 ℃.
7. The silicon isotope continuous production process according to claim 1, characterized in that: the complexing agent is anisole or trimethyl borate.
8. The silicon isotope continuous production process according to claim 1, characterized in that: the target abundance is above 99.5%.
9. The silicon isotope continuous production process according to claim 1, characterized in that: the working temperature of the decomposition preheater is 100-150 ℃, and the working temperature of the decomposition device is 150-300 ℃.
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