CN210751343U - High-purity ethyl orthosilicate purification device - Google Patents
High-purity ethyl orthosilicate purification device Download PDFInfo
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- CN210751343U CN210751343U CN201921713082.9U CN201921713082U CN210751343U CN 210751343 U CN210751343 U CN 210751343U CN 201921713082 U CN201921713082 U CN 201921713082U CN 210751343 U CN210751343 U CN 210751343U
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Abstract
The utility model discloses a high-purity ethyl orthosilicate purifying device, which comprises an evaporation tower, a reboiler and a condenser; the evaporation tower is provided with a feed inlet, a feed port, a feed back port, a discharge port and a condensation reflux port; the reboiler is provided with a feeding inlet, a return outlet, a steam inlet and a steam outlet; the condenser is provided with a gas material inlet, a finished product outlet, a circulating water inlet and a circulating water outlet; the feeding port is connected to the feeding inlet through a pipeline, the feed back port is connected to the feed back outlet through a pipeline, the discharge port is connected to the gas material inlet through a pipeline, and the finished product outlet is provided with a first finished product pipeline and a second finished product pipeline. The utility model discloses can realize that simple process changes, the evaporation tower that only needs to increase similar rectifying column device can realize the further promotion of purity, not only can save the cost, reduces the energy consumption, can play the effect of rectifying column rectification moreover, also is very convenient in follow-up production operation.
Description
Technical Field
The utility model belongs to the technical field of the material purification, concretely relates to high-purity tetraethoxysilane purification device.
Background
In the semiconductor process, high-purity ethyl silicate is used as an oxide layer material, and the function of the high-purity ethyl silicate is to generate a silicon dioxide film on the surface of a silicon wafer through high-temperature deposition in low-pressure chemical vapor deposition (LPCVD). With the improvement of nanotechnology, in order to improve the electrical performance and yield of semiconductor devices and avoid the defect of long-time high-temperature oxidation of an oxide layer with a certain thickness, the requirement on the purity of ethyl orthosilicate is higher and higher, and certain research and technical exploration are needed to reach the purity of 4N and above 4N5 at present, especially to reach the purity of metal ions above 9N level.
At present, the purification of the tetraethoxysilane basically needs to be realized by rectification purification to achieve higher purity, and the purification device has the characteristic of energy conservation. The other is sub-boiling rectification, but the energy consumption is large. Both of the two methods can purify the tetraethoxysilane to about 4N, but the further improvement of the purity can face huge challenges, and whether to continue increasing the number of the towers or changing the process method can be considered in multiple aspects. In particular, the contact of the metal filler cannot avoid the pollution of metal ions, so that the later removal of the metal ions also has great disadvantages.
The disadvantages of the prior art are as follows: 1. the process flow is complex, the distillation equipment is required to be added or a novel process flow is required to be changed for further improving the material purity, the investment and the energy consumption are increased, the subsequent production operation is troublesome, and 5 or more distillation columns are required for distillation and purification in order to achieve the purity of 4N 5; 2. the removal of metal ions has the possibility of pollution, the metal ions are difficult to reach 9N level, and a metal packed tower is a pollution source.
Disclosure of Invention
The invention aims at providing a high-purity tetraethoxysilane purification device, which can realize the simplification of the process, can realize the further promotion of the purity only by adding an evaporation tower similar to a rectifying tower device, not only can save the cost and reduce the energy consumption, but also can play the rectifying effect of the rectifying tower, and is very convenient in the subsequent production operation.
In order to achieve the purpose of the invention, the technical scheme adopted by the utility model is as follows: a high-purity ethyl orthosilicate purification device comprises an evaporation tower, a reboiler and a condenser;
a feed inlet and a feed port are arranged at the middle lower part of the evaporation tower, the feed inlet and the feed port are positioned on two side surfaces of the evaporation tower, a feed back port is arranged above the feed port on the evaporation tower, a filler is arranged on a path from the feed back port to the top of the evaporation tower in the evaporation tower, a discharge port is arranged at the top of the evaporation tower, and a condensation reflux port is arranged on the side surface of the top of the evaporation tower;
the reboiler is provided with a feeding inlet, a return outlet, a steam inlet and a steam outlet, the feeding inlet is positioned on the side surface of the bottom of the reboiler, the return outlet is positioned at the top of the reboiler, the steam inlet and the steam outlet are positioned on the side surface of the reboiler, and the steam inlet is positioned above the steam outlet;
the condenser is provided with a gas material inlet, a finished product outlet, a circulating water inlet and a circulating water outlet, the gas material inlet and the circulating water outlet are positioned at the top of the condenser, and the finished product outlet and the circulating water inlet are positioned at the bottom of the condenser;
the feeding port is connected to a feeding inlet through a pipeline, the return port is connected to a return outlet through a pipeline, the discharge port is connected to a gas material inlet through a pipeline, a first finished product pipeline and a second finished product pipeline are arranged on the finished product outlet, the first finished product pipeline is used for connecting the finished product outlet and the condensation return port, and the second finished product pipeline is used for discharging finished products.
In the technical scheme, the working pressure in the evaporation tower is 49-51 KPa, and the temperature is 149-151 ℃. Preferably, the operating pressure in the evaporation column is 50KPa and the temperature is 150 ℃.
In the technical scheme, the inner surface of the evaporation tower is sprayed with a polytetrafluoroethylene coating.
In the technical scheme, the filler is polytetrafluoroethylene filler, and the height of the filler is 1350-1450 mm. Preferably, the height of the packing is 1400 mm.
In the above technical scheme, the top of the evaporation tower is also provided with a vent.
In the above technical scheme, the evacuation port is provided with a first double-sleeve pipe with a length greater than 2m, the first double-sleeve pipe comprises a first sleeve pipe and a first inner pipe arranged in the first sleeve pipe, the size of the first sleeve pipe is DN50, and the size of the first inner pipe is DN 25.
In the technical scheme, the bottom of the evaporation tower and the bottom of the reboiler are both provided with sewage outlets.
In the technical scheme, a second double sleeve pipe with the length larger than 8m is installed on the sewage draining outlet, the second double sleeve pipe comprises a second sleeve pipe and a second inner pipe arranged in the second sleeve pipe, the size of the second sleeve pipe is DN50, and the size of the second inner pipe is DN 25.
In the technical scheme, the heating source of the reboiler selects steam with the pressure of 0.19-0.21 MPa. Preferably, the heating source of the reboiler is steam with pressure of 0.2 MPa.
In the technical scheme, the temperature of circulating water used by the condenser is 29-31 ℃. Preferably, the condenser uses circulating water at a temperature of 30 ℃.
In the above, DN is the nominal diameter of the pipe, also called mean outer diameter. Wherein DN50 represents a 2-inch tube with an inner diameter of 50mm, an outer diameter of 56mm and a wall thickness of 3 mm; DN25 represents a 1 inch tube with an inner diameter of 25mm, an outer diameter of 32mm and a wall thickness of 3.5 mm.
Because of the application of the technical scheme, compared with the prior art, the utility model has the following advantages:
1. the utility model realizes the purification of the ethyl orthosilicate by using the evaporation tower, the reboiler and the condenser, is easy to realize the improvement of a purity grade of the product, and has simple operation and no complex process;
2. the device has simple equipment, less investment and low cost, and compared with a 30m rectifying tower, the device of the utility model has the height of only 2.5 m;
3. the utility model has simple negative pressure rectification function through simple flash evaporation;
4. the utility model discloses a packing is polytetrafluoroethylene filler in the distillation column, and the pollution sources is few in the tower, can effectively get rid of metal ion content, makes the product metal ion grade can be more than 9N level.
Drawings
Fig. 1 is a diagram of a structure of an apparatus according to a first embodiment of the present invention.
Wherein: 1. an evaporation tower; 2. a reboiler; 3. a condenser; 4. a feed inlet; 5. a feed port; 6. a feed back port; 7. a discharge port; 8. a condensing reflux port; 9. a feed inlet; 10. a feed back outlet; 11. a steam inlet; 12. a steam outlet; 13. a gas feed inlet; 14. a finished product outlet; 15. a circulating water inlet; 16. a circulating water outlet; 17. emptying the air; 18. a first double cannula; 19. a sewage draining outlet; 20. a second double cannula.
Detailed Description
The invention will be further described with reference to the following drawings and examples:
the first embodiment is as follows:
referring to fig. 1, a high-purity ethyl orthosilicate purification device comprises an evaporation tower 1, a reboiler 2 and a condenser 3;
a feed inlet 4 and a feed port 5 are arranged at the middle lower part of the evaporation tower, the feed inlet and the feed port are positioned on two side surfaces of the evaporation tower, a feed back port 6 is arranged above the feed port on the evaporation tower, a filler is arranged on a path from the feed back port to the top of the evaporation tower, a discharge port 7 is arranged at the top of the evaporation tower, and a condensation reflux port 8 is arranged on the side surface of the top of the evaporation tower;
the reboiler is provided with a feeding inlet 9, a return outlet 10, a steam inlet 11 and a steam outlet 12, the feeding inlet is positioned on the side surface of the bottom of the reboiler, the return outlet is positioned at the top of the reboiler, the steam inlet and the steam outlet are positioned on the side surface of the reboiler, and the steam inlet is positioned above the steam outlet;
the condenser is provided with a gas material inlet 13, a finished product outlet 14, a circulating water inlet 15 and a circulating water outlet 16, the gas material inlet and the circulating water outlet are positioned at the top of the condenser, and the finished product outlet and the circulating water inlet are positioned at the bottom of the condenser;
the feeding port is connected to a feeding inlet through a pipeline, the return port is connected to a return outlet through a pipeline, the discharge port is connected to a gas material inlet through a pipeline, a first finished product pipeline and a second finished product pipeline are arranged on the finished product outlet, the first finished product pipeline is used for connecting the finished product outlet and the condensation return port, and the second finished product pipeline is used for discharging finished products.
In this embodiment, the working pressure in the evaporation tower is 50KPa, and the temperature is 150 ℃, that is, the negative pressure vaporization and rectification state is achieved.
In this embodiment, the inner surface of the evaporation tower is sprayed with a teflon coating.
In the embodiment, the height of the evaporation tower is 3500mm, the diameter of the evaporation tower is 200mm, the tower bottom is 500mm, the filler is polytetrafluoroethylene filler, and the height of the filler is 1400mm, so that pollution caused by the adoption of metal filler is avoided.
In this embodiment, the top of the evaporation tower is further provided with an evacuation port 17.
In this embodiment, the evacuation port is provided with a first double sleeve 18 having a length greater than 2m, the first double sleeve includes a first sleeve and a first inner tube disposed in the first sleeve, the size of the first sleeve is DN50, and the size of the first inner tube is DN 25.
In this embodiment, the bottom of the evaporation tower and the bottom of the reboiler are both provided with a drain outlet 19.
In this embodiment, a second double sleeve 20 with a length greater than 8m is installed on the sewage draining exit, the second double sleeve includes a second sleeve and a second inner pipe arranged in the second sleeve, the size of the second sleeve is DN50, and the size of the second inner pipe is DN 25.
The utility model discloses because the temperature is high in the tower, evacuation mouth and drain all adopt double-pipe structure to use the cooling circulation water ejection of compact of cooling. The circulating water of the first double-sleeve pipe enters from top to bottom, and the circulating water of the second double-sleeve pipe enters from bottom to top. Considering the negative pressure in the evaporation tower, a corresponding vacuum pump is arranged at the rear end of the evacuation port to extract low-boiling-point substances, and a corresponding liquid pump is arranged at the rear end of the sewage discharge port to convert waste liquid.
In this embodiment, the heating source of the reboiler is steam with a pressure of 0.2 MPa.
In this embodiment, the temperature of the circulating water used by the condenser is 30 ℃.
The utility model discloses a device is when using, and the tetraethoxysilane product gets into from the feed inlet of evaporating tower, send into the reboiler through the pay-off mouth and vaporize and return the evaporating tower through the feed back mouth after heating, rise to the top of the tower through the tower internal packing, metal ion impurity is eluted by the filler and is got off and discharge from the drain at the bottom of the tower, and the product after the purification flows in from the gas material entry of condenser rear end, and after the condenser condensation, liquid partly flows back to the top of the tower through the condensation backward flow mouth and forms the backward flow, and partly converts into the finished product and carries out the ejection of compact; continuously performing heat exchange between the condensed liquid and the gas vaporized by the reboiler in the tower, collecting impurities such as ethanol and diethyl ether at the top of the tower, and discharging through a vent at the top of the tower; high-boiling residues such as polymers (dimers, trimers) of ethyl orthosilicate are accumulated at the bottom of the tower and then discharged through a drain outlet.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to the above-described embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A high-purity ethyl orthosilicate purification device is characterized in that: comprises an evaporation tower, a reboiler and a condenser;
a feed inlet and a feed port are arranged at the middle lower part of the evaporation tower, the feed inlet and the feed port are positioned on two side surfaces of the evaporation tower, a feed back port is arranged above the feed port on the evaporation tower, a filler is arranged on a path from the feed back port to the top of the evaporation tower in the evaporation tower, a discharge port is arranged at the top of the evaporation tower, and a condensation reflux port is arranged on the side surface of the top of the evaporation tower;
the reboiler is provided with a feeding inlet, a return outlet, a steam inlet and a steam outlet, the feeding inlet is positioned on the side surface of the bottom of the reboiler, the return outlet is positioned at the top of the reboiler, the steam inlet and the steam outlet are positioned on the side surface of the reboiler, and the steam inlet is positioned above the steam outlet;
the condenser is provided with a gas material inlet, a finished product outlet, a circulating water inlet and a circulating water outlet, the gas material inlet and the circulating water outlet are positioned at the top of the condenser, and the finished product outlet and the circulating water inlet are positioned at the bottom of the condenser;
the feeding port is connected to a feeding inlet through a pipeline, the return port is connected to a return outlet through a pipeline, the discharge port is connected to a gas material inlet through a pipeline, a first finished product pipeline and a second finished product pipeline are arranged on the finished product outlet, the first finished product pipeline is used for connecting the finished product outlet and the condensation return port, and the second finished product pipeline is used for discharging finished products.
2. The purification device of high-purity tetraethoxysilane according to claim 1, which is characterized in that: the working pressure in the evaporation tower is 49-51 KPa, and the temperature is 149-151 ℃.
3. The purification device of high-purity tetraethoxysilane according to claim 1, which is characterized in that: the inner surface of the evaporation tower is sprayed with a polytetrafluoroethylene coating.
4. The purification device of high-purity tetraethoxysilane according to claim 1, which is characterized in that: the filler is polytetrafluoroethylene filler, and the height of the filler is 1350-1450 mm.
5. The purification device of high-purity tetraethoxysilane according to claim 1, which is characterized in that: and the top of the evaporation tower is also provided with a vent.
6. The purification device of high-purity tetraethoxysilane according to claim 5, wherein: the emptying port is provided with a first double sleeve with the length larger than 2m, the first double sleeve comprises a first sleeve and a first inner tube arranged in the first sleeve, the size of the first sleeve is DN50, and the size of the first inner tube is DN 25.
7. The purification device of high-purity tetraethoxysilane according to claim 1, which is characterized in that: and drain outlets are formed in the bottom of the evaporation tower and the bottom of the reboiler.
8. The purification apparatus of high-purity tetraethoxysilane according to claim 7, characterized in that: install the second double cannula that length is greater than 8m on the drain, the second double cannula includes second sleeve pipe and sets up the second inner tube in the second sleeve pipe, the size of second sleeve pipe is DN50, the size of second inner tube is DN 25.
9. The purification device of high-purity tetraethoxysilane according to claim 1, which is characterized in that: the heating source of the reboiler is steam with the pressure of 0.19-0.21 MPa.
10. The purification device of high-purity tetraethoxysilane according to claim 1, which is characterized in that: the temperature of circulating water used by the condenser is 29-31 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921713082.9U CN210751343U (en) | 2019-10-14 | 2019-10-14 | High-purity ethyl orthosilicate purification device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921713082.9U CN210751343U (en) | 2019-10-14 | 2019-10-14 | High-purity ethyl orthosilicate purification device |
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| CN210751343U true CN210751343U (en) | 2020-06-16 |
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| CN201921713082.9U Active CN210751343U (en) | 2019-10-14 | 2019-10-14 | High-purity ethyl orthosilicate purification device |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115193085A (en) * | 2022-06-24 | 2022-10-18 | 苏州金宏气体股份有限公司 | System and method for controlling tower top pressure and temperature of rectifying tower for producing tetraethoxysilane |
-
2019
- 2019-10-14 CN CN201921713082.9U patent/CN210751343U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115193085A (en) * | 2022-06-24 | 2022-10-18 | 苏州金宏气体股份有限公司 | System and method for controlling tower top pressure and temperature of rectifying tower for producing tetraethoxysilane |
| CN115193085B (en) * | 2022-06-24 | 2024-04-12 | 金宏气体股份有限公司 | Overhead pressure and temperature control system and method for rectifying tower for producing ethyl orthosilicate |
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| CP03 | Change of name, title or address |
Address after: 215152 Anmin Road, Panyang Industrial Park, Huangdai Town, Xiangcheng District, Suzhou City, Jiangsu Province Patentee after: Jinhong Gas Co.,Ltd. Address before: 215152 No. 6 Anmin Road, Panyang Industrial Park, Huangdi Town, Xiangcheng District, Suzhou City, Jiangsu Province Patentee before: SUZHOU JINHONG GAS Co.,Ltd. |
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