CN210674475U - Purifying device for ethyl orthosilicate - Google Patents
Purifying device for ethyl orthosilicate Download PDFInfo
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- CN210674475U CN210674475U CN201921526079.6U CN201921526079U CN210674475U CN 210674475 U CN210674475 U CN 210674475U CN 201921526079 U CN201921526079 U CN 201921526079U CN 210674475 U CN210674475 U CN 210674475U
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Abstract
The utility model discloses a purification device of ethyl orthosilicate, including head tank and the adsorber that is used for adsorbing the metal ion in the raw materials, be equipped with the transfer pump between head tank and adsorber, the low reaches of adsorber group still links the rectifying column that is used for desorption metal ion, and the low reaches of rectifying column even has the finished product jar. The adsorbent adsorbs metal ions in the tetraethoxysilane without introducing new impurities. Meanwhile, compared with a sub-boiling distillation process, the process for removing metal ions by combining the adsorption process and the rectification process has lower requirement on temperature. The purifying device continuously purifies the n-ethyl silicate, thereby reducing the processing difficulty and improving the processing efficiency.
Description
Technical Field
The utility model relates to an ethyl orthosilicate processing technology field, in particular to ethyl orthosilicate's purification device.
Background
Tetraethoxysilane is an important process gas in semiconductor processing, tetraethoxysilane is deposited on the surface of a silicon wafer to form a silicon dioxide film under certain process conditions, the deposition rate of the silicon dioxide film can reach 50 a/min, and the thickness uniformity of the film is less than 3 percent. Tetraethoxysilane not only has excellent process characteristics, but also has higher safety in the deposition processing process, so that the tetraethoxysilane deposition process gradually becomes a mainstream process for depositing a silicon dioxide film.
Metal impurities can be introduced in the preparation process of the tetraethoxysilane, and the metal impurities can reduce the concentration of the tetraethoxysilane, so that trace metal impurities, ethanol, other organic impurities and moisture in a finished product need to be removed after reaction. In the prior art, metal impurities in raw materials are complexed by a complexing agent, and then tetraethoxysilane with higher concentration is obtained by a sub-distillation mode. However, the complexing agent is easy to introduce new metal ion impurities, and meanwhile, the sub-boiling distillation mode has the disadvantages of high processing difficulty, high energy consumption and low efficiency, so that the production cost of the product is increased, and the continuous production cannot be realized.
Therefore, how to effectively remove the metal impurities in the tetraethoxysilane is a technical problem which needs to be solved by the technical personnel in the field.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing a purification device of tetraethoxysilane, it has set up the adsorber, can eliminate the metal ion in the tetraethoxysilane effectively through absorbent mode.
In order to realize the above purpose, the utility model provides a purifying device of ethyl orthosilicate, include the head tank and be used for adsorbing the metallic ion's in the raw materials adsorber, the head tank with be equipped with the transfer pump between the adsorber, adsorber group low reaches still links the rectifying column that is used for desorption metallic ion, the low reaches of rectifying column even has the finished product jar.
Preferably, the raw material enters from the lower part of the adsorber, and the adsorber is provided with a filter layer positioned at the lower part and an adsorbent positioned above the filter layer.
Preferably, the filter layer includes the orifice plate that is located the lowermost part, the orifice plate top is equipped with the quartzy cotton filter layer, quartzy cotton filter layer top still is equipped with the quartz sand filter layer.
Preferably, the number of the adsorbers is greater than or equal to two, and the adsorbers are arranged in parallel.
Preferably, the device further comprises a nitrogen sealing system connected with the top of the raw material tank and used for sealing the raw material tank, wherein the nitrogen sealing system comprises an air source connected with the raw material tank through an air supply pipe, and a control valve is arranged in the air supply pipe.
Preferably, the rectifying tower comprises a first-stage rectifying tower and a second-stage rectifying tower which are arranged in series, a first-stage reboiler is arranged at the bottom of the first-stage rectifying tower, and a first-stage outlet pipeline of the first-stage rectifying tower is positioned at the bottom of the tower.
Preferably, the system further comprises a waste heat exchanger which is connected with a primary outlet pipeline and a primary inlet pipeline of the primary rectifying tower to recover the waste heat of the materials.
Preferably, a first-stage condenser is arranged at the top of the first-stage rectifying tower.
Preferably, a secondary reboiler is arranged at the bottom of the secondary rectifying tower.
Preferably, an outlet pipeline of the secondary rectifying tower is connected with the top of the tower, a finished product condenser is arranged on the top of the tower, and materials enter the finished product tank after being condensed.
The utility model provides a purifying device of ethyl orthosilicate, including head tank and the adsorber that is used for adsorbing the metal ion in the raw materials, be equipped with the transfer pump between head tank and adsorber, the low reaches of adsorber group still links the rectifying column that is used for desorption metal ion, and the low reaches of rectifying column even has the finished product jar.
The adsorbent adsorbs metal ions in the tetraethoxysilane without introducing new impurities. Meanwhile, compared with a sub-boiling distillation process, the process for removing metal ions by combining the adsorption process and the rectification process has lower requirement on temperature. The purifying device continuously purifies the n-ethyl silicate, thereby reducing the processing difficulty and improving the processing efficiency.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required to be used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
Fig. 1 is a schematic structural diagram of a purifying apparatus for ethyl orthosilicate provided by the present invention.
Wherein the reference numerals in fig. 1 are:
the system comprises a raw material tank 1, an infusion pump 2, an adsorber 3, a primary rectifying tower 4, a secondary rectifying tower 5, a waste heat exchanger 6, a finished product condenser 7, a finished product tank 8, a gas source 9, a pore plate 31, a quartz wool filter layer 32, a quartz sand filter layer 33, an adsorbent 34, a primary reboiler 41, a primary condenser 42, a secondary reboiler 51, a secondary condenser 52 and a flow meter 91.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention.
In order to make the technical field of the present invention better understand, the present invention will be described in detail with reference to the accompanying drawings and the detailed description.
Referring to fig. 1, fig. 1 is a schematic structural diagram of a purifying apparatus for tetraethoxysilane provided by the present invention.
The utility model provides a purifying device of tetraethoxysilane, as shown in figure 1, comprises a raw material tank 1, an absorber 3, a rectifying tower and a finished product tank 8 which are connected in sequence. The raw material tank 1 is filled with tetraethoxysilane to be purified, an infusion pump 2 is arranged between the raw material tank 1 and the adsorber 3, and the infusion pump 2 conveys tetraethoxysilane from the raw material tank 1 to the adsorber 3. The adsorber 3 is provided with an adsorbent 34 for adsorbing metal ions in the raw material, specifically, the adsorbent 34 removes the metal ions by using a complex adsorption technique, and the material of the adsorbent 34 can refer to the prior art and is not described herein again. Trace metal ions still remain in the adsorbed tetraethoxysilane, and the rectifying tower is used for removing the residual metal ions. The removed tetraethoxysilane flows into a finished product tank 8.
Optionally, the adsorber 3 includes a tank and a filter layer, adsorbent 34, located in the tank. The raw material enters from the lower part of the adsorber 3, the upper part flows out, the filter layer is positioned at the lower part of the tank body, and the adsorbent 34 is positioned above the filter layer. Impurities in the tetraethoxysilane are firstly filtered by the filter layer, and then the adsorbent 34 removes metal ions, so that the impurities in the tetraethoxysilane are prevented from influencing the performance of the adsorbent 34.
Optionally, the filter layer comprises an orifice plate 31, a quartz cotton filter layer 32 and a quartz sand filter layer 33 which are sequentially distributed from bottom to top. The diameters of the impurities filtered by the three are reduced in sequence, and the quartz sand can filter extremely fine impurities, so that the adsorbent 34 is ensured not to be interfered by the impurities.
In addition, the number of adsorbers 3 is generally two or more in order to increase the throughput of the purification apparatus. As shown in fig. 1, three adsorbers 3 are arranged in parallel, thereby improving the treatment efficiency of the purification apparatus. Meanwhile, once the adsorbent 34 is saturated, the metal ions cannot be removed any more, and at this time, the adsorbent 34 should be replaced by shutdown. The increase of the number of the adsorbers 3 can improve the saturation capacity of the purification device, thereby prolonging the production period of the purification device.
Optionally, because tetraethoxysilane easily volatilizes, holding vessel 1 even has nitrogen gas sealing system, realizes holding vessel 1's pressurization through nitrogen gas and seals, reduces the volume of volatilizing of raw materials. Specifically, as shown in fig. 1, the nitrogen sealing system includes an air source 9, an air supply pipe and a control valve, the air source 9 is connected to the top of the raw material tank 1 through the air supply pipe, the control valve is disposed in the air supply pipe, and the opening of the control valve is adjusted to control the pressure in the raw material tank 1. The air supply pipe is also connected with a flow meter 91, the flow meter 91 is connected with a control valve, and the opening degree of the control valve is adjusted according to the nitrogen flow, so that closed-loop control is realized, and the control result is more accurate. The control valve in this application and the governing valve of head tank 1, adsorber 3, rectifying column access & exit are by the control of safety instrument system, guarantee production process quantitative control, reduce risks such as excess temperature superpressure, have improved the security of production process.
In the embodiment, the purifying device for ethyl orthosilicate purifies ethyl orthosilicate through a process of rectifying after complexing adsorption, the process has low requirements on temperature and pressure, the purifying processing difficulty of ethyl orthosilicate is reduced, the efficiency is improved, meanwhile, decompression operation is not needed, and the energy consumption of the whole device is also reduced. In addition, in the application, a plurality of adsorbers 3 work in parallel, when the adsorbent 34 in one adsorber 3 is saturated, the regulating valve at the inlet and the outlet of the adsorber 3 can be closed to cut the adsorber 3 out of the device and replace the adsorbent 34, the whole device does not need to be stopped, and the production continuity is ensured.
Optionally, in order to improve the product purity, the rectifying tower comprises a first-stage rectifying tower 4 and a second-stage rectifying tower 5, wherein the bottom and outlet pipelines of the first-stage rectifying tower 4 are connected with the middle part of the second-stage rectifying tower 5, and the second-stage outlet pipeline of the second-stage rectifying tower 5 is positioned at the top of the tower. The first-stage rectifying tower 4 and the second-stage rectifying tower 5 are connected in series and are respectively used for removing light impurities and heavy impurities in materials, trace metal ions in the ethyl orthosilicate can be effectively removed through two-stage rectification, and the product quality is guaranteed.
The bottom of the first-stage rectifying tower 4 is provided with a first-stage reboiler 41, and the heat of the first-stage rectification of the tetraethoxysilane is provided by the first-stage reboiler 41. After the first-stage rectification, the tetraethoxysilane flows into the second-stage rectification tower 5 under the action of pressure, the temperature of the tetraethoxysilane is reduced at the moment, and the materials cannot be completely gasified, so that a second-stage reboiler 51 is arranged at the bottom of the second-stage rectification tower 5. The second-stage reboiler 51 heats the materials to completely evaporate the tetraethoxysilane, the outlet of the second-stage rectifying tower 5 is positioned at the top of the tower, and the evaporated tetraethoxysilane is condensed into a liquid state by the second-stage condenser 52 at the top of the tower and directly flows into the finished product tank 8. After rectification, the ethyl orthosilicate is directly canned, so that secondary pollution can be avoided, and the product quality is improved.
Optionally, the material in the rectification process of the first-stage rectification tower 4 can volatilize, and in order to avoid the overhigh pressure, the top of the first-stage rectification tower 4 is provided with a first-stage condenser 42. Gaseous state material flows back to in one-level rectifying column 4 after the condensation, and the top of the tower temperature can be adjusted in the material backward flow, improves the temperature gradient in the tower to improve the rectification effect.
The temperature of the material flowing out of the first-stage rectifying tower 4 is usually high, and heat is dissipated into the air in the flowing process of the material, so that energy waste is caused, and serious thermal pollution is brought to the environment. Therefore, a waste heat exchanger 6 is also arranged in the purifying device. Specifically, heat medium layer and refrigerant layer of waste heat exchanger 6 link to each other with the one-level export pipeline and the one-level import pipeline of one-level rectifying column 4 respectively, the import material and the export material of one-level rectifying column 4 carry out the heat transfer in waste heat exchanger 6, utilize the heat heating import material of export material, thereby reduce the energy consumption of reboiler, play the effect that energy-conserving this falls, tetraethoxysilane's purification device obtains it through material balance and can save 5% energy consumption at least during the operation. In addition, because the temperature of adsorber 3, one-level rectifying column 4 and second grade rectifying column 5 is higher, in order to reduce the heat and scatter and disappear, the periphery of three and the periphery of connecting line all are equipped with the heat preservation, and the heat preservation can reduce purification device's heat consumption, and then reduce the cost of enterprises.
Optionally, the finished product material is liquefied into liquid tetraethoxysilane after being cooled by the secondary condenser 52, but the temperature of the finished product material is still high, and the finished product material is directly filled into the finished product tank 8, so that the risk of over-temperature and over-pressure exists, and the finished product condenser 7 is further arranged between the secondary condenser 52 and the finished product tank 8. The material is cooled by the finished product condenser 7 and then enters the finished product tank 8, so that the risk of material storage can be reduced.
Optionally, an automatic sampling point is arranged in the purification device, and the components of the material are determined through automatic sampling and online analysis. Specifically, the automatic sampling point is located between the infusion pump 2 and the adsorber 3, and the structure of the automatic sampling system can refer to the prior art, and is not described herein again. Whole purification device passes through control system such as DCS and realizes automated control, not only can improve production efficiency, reduces the cost of labor, can also reduce the risk in the production process effectively, through instrument real time monitoring device's temperature and pressure, utilizes interlock system to ensure production safety.
In this embodiment, the purifying apparatus for ethyl orthosilicate further improves the quality of the material by using a second-stage rectification. Meanwhile, a waste heat exchanger 6 is further arranged in the purifying device and used for recovering waste heat of materials at the outlet of the primary rectifying tower 4, partial condensers in the purifying device exchange heat with cold water through the materials, the cold water is heated into hot water through heat in the materials, and the utilization efficiency of energy is further improved.
It is noted that, in this specification, relational terms such as first and second, and the like are used solely to distinguish one entity from another entity without necessarily requiring or implying any actual such relationship or order between such entities.
The purifying device of the tetraethoxysilane provided by the utility model is introduced in detail. The principles and embodiments of the present invention have been explained herein using specific examples, and the above descriptions of the embodiments are only used to help understand the method and its core ideas of the present invention. It should be noted that, for those skilled in the art, without departing from the principle of the present invention, the present invention can be further modified and modified, and such modifications and modifications also fall within the protection scope of the appended claims.
Claims (10)
1. The utility model provides a purification device of tetraethyl orthosilicate, which is characterized in that, including head tank (1) and adsorber (3) that are arranged in adsorbing the metal ion in the raw materials, head tank (1) with be equipped with transfer pump (2) between adsorber (3), adsorber (3) group low reaches still link has the rectifying column that is used for desorption metal ion, the low reaches of rectifying column link has finished product jar (8).
2. Purification device according to claim 1, characterized in that the feed enters from the lower part of the adsorber (3), the adsorber (3) having therein a lower filter layer and an adsorbent (34) above the filter layer.
3. The purification device according to claim 2, wherein the filter layer comprises a pore plate (31) at the lowest part, a quartz wool filter layer (32) is arranged above the pore plate (31), and a quartz sand filter layer (33) is also arranged above the quartz wool filter layer (32).
4. Purification device according to claim 1, wherein the number of adsorbers (3) is greater than or equal to two and arranged in parallel.
5. The purification apparatus according to claim 1, further comprising a nitrogen gas sealing system connected to the top of the feedstock tank (1) for sealing the feedstock tank (1), the nitrogen gas sealing system comprising a gas source (9) connected to the feedstock tank (1) through a gas supply pipe, the gas supply pipe having a control valve disposed therein.
6. The purification device according to any one of claims 1 to 5, wherein the rectification column comprises a primary rectification column (4) and a secondary rectification column (5) which are arranged in series, a primary reboiler (41) is arranged at the bottom of the primary rectification column (4), and a primary outlet pipeline of the primary rectification column (4) is positioned at the bottom of the column.
7. The purification device according to claim 6, further comprising a waste heat exchanger (6) connected to both the primary outlet line and the primary inlet line of the primary rectification column (4) for recovering waste heat of the material.
8. Purification device according to claim 7, wherein a primary condenser (42) is arranged at the top of the primary rectification column (4).
9. Purification apparatus according to claim 6, wherein the second rectification column (5) is provided at its bottom with a second reboiler (51).
10. The purification device according to claim 9, wherein the outlet line of the secondary rectification column (5) is connected to the top of the column, which is provided with a finished product condenser (7), and the material is condensed and then enters the finished product tank (8).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201921526079.6U CN210674475U (en) | 2019-09-12 | 2019-09-12 | Purifying device for ethyl orthosilicate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921526079.6U CN210674475U (en) | 2019-09-12 | 2019-09-12 | Purifying device for ethyl orthosilicate |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113121583A (en) * | 2021-04-21 | 2021-07-16 | 洛阳中硅高科技有限公司 | Preparation device and preparation method of electronic-grade ethyl orthosilicate |
| CN113292588A (en) * | 2021-05-26 | 2021-08-24 | 苏州金宏气体股份有限公司 | Purification method and purification system of electronic grade ethyl orthosilicate |
| CN114504872A (en) * | 2022-02-15 | 2022-05-17 | 北京袭明科技有限公司 | Method and device for producing high-purity electronic grade ethylene glycol |
-
2019
- 2019-09-12 CN CN201921526079.6U patent/CN210674475U/en active Active
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113121583A (en) * | 2021-04-21 | 2021-07-16 | 洛阳中硅高科技有限公司 | Preparation device and preparation method of electronic-grade ethyl orthosilicate |
| CN113121583B (en) * | 2021-04-21 | 2024-07-05 | 洛阳中硅高科技有限公司 | Preparation device and preparation method of electronic grade ethyl orthosilicate |
| CN113292588A (en) * | 2021-05-26 | 2021-08-24 | 苏州金宏气体股份有限公司 | Purification method and purification system of electronic grade ethyl orthosilicate |
| WO2022247166A1 (en) * | 2021-05-26 | 2022-12-01 | 苏州金宏气体股份有限公司 | Purification method and purification system for electronic grade tetraethyl orthosilicate |
| CN114504872A (en) * | 2022-02-15 | 2022-05-17 | 北京袭明科技有限公司 | Method and device for producing high-purity electronic grade ethylene glycol |
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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. |