CN219463370U - Production equipment of ethyl orthosilicate - Google Patents
Production equipment of ethyl orthosilicate Download PDFInfo
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- CN219463370U CN219463370U CN202320671924.9U CN202320671924U CN219463370U CN 219463370 U CN219463370 U CN 219463370U CN 202320671924 U CN202320671924 U CN 202320671924U CN 219463370 U CN219463370 U CN 219463370U
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The utility model discloses production equipment of tetraethoxysilane, which comprises the following components: the continuous electrodeionization device is used for separating metal ions in the mixed raw materials; the reactor is communicated with the continuous electrodeionization device and is used for enabling raw materials separated from metal ions by the continuous electrodeionization device to react to generate crude ethyl orthosilicate; the light component removing rectifying tower is communicated with the reactor and is used for removing light component impurities in the crude product of the ethyl orthosilicate; and the heavy-removal rectifying tower is communicated with the light-removal rectifying tower and is used for removing heavy component impurities in the crude product of the ethyl orthosilicate. The production equipment of the ethyl orthosilicate has the advantages of reducing the energy consumption of production, improving the yield of the ethyl orthosilicate, improving the impurity removal efficiency and reducing the production cost.
Description
Technical Field
The utility model relates to the technical field of semiconductors, in particular to production equipment of tetraethoxysilane.
Background
The synthesis of the tetraethoxysilane is mostly prepared by taking silicon tetrachloride which is a byproduct generated in the production process of polysilicon and trichlorosilane as a raw material to react with ethanol, and simultaneously generating hydrogen chloride. However, in the synthesis of the ethyl orthosilicate, if the content of metal ions in the silicon tetrachloride and the ethanol serving as raw materials is not controlled, the content of metal ions in the synthesized ethyl orthosilicate is very high, the difficulty is increased for the subsequent purification process, and the ethyl orthosilicate can be purified to meet the requirement of the integrated circuit chip manufacturing on the content of metal ion impurities only by very strong separation capability.
The existing scheme for improving the purity of the ethyl orthosilicate generally comprises the steps of synthesizing the ethyl orthosilicate, and then removing metal ions in the ethyl orthosilicate through a multi-stage rectifying tower or an adsorbent. However, the scheme has at least one of high energy consumption, low impurity removal efficiency, high cost, low yield and the like.
Disclosure of Invention
The utility model aims to provide production equipment of ethyl orthosilicate, which has the advantages of reducing the energy consumption of production, improving the yield of the ethyl orthosilicate, improving the impurity removal efficiency and reducing the production cost.
To achieve the above object, an embodiment of the present utility model provides an apparatus for producing ethyl orthosilicate, comprising:
the continuous electrodeionization device is used for separating metal ions in the mixed raw materials;
the reactor is communicated with the continuous electrodeionization device and is used for enabling raw materials separated from metal ions by the continuous electrodeionization device to react to generate crude ethyl orthosilicate;
the light component removing rectifying tower is communicated with the reactor and is used for removing light component impurities in the crude product of the ethyl orthosilicate;
and the heavy-removal rectifying tower is communicated with the light-removal rectifying tower and is used for removing heavy component impurities in the crude product of the ethyl orthosilicate.
In one or more embodiments of the utility model, the de-heavies rectification column has a heavy fraction outlet from which the heavy fraction impurities flow, and the de-light rectification column has a light fraction outlet from which the light fraction impurities flow; the continuous electrodeionization device comprises:
a light chamber having a light chamber inlet and a light chamber outlet for the mixed raw materials to enter and exit, the reactor being in communication with the light chamber outlet;
a dense chamber for receiving the metal ions separated in the dilute chamber, the dense chamber having a dense chamber outlet and a dense chamber inlet, and the dense chamber inlet being in communication with the heavy fraction outlet and/or the light fraction outlet for the heavy fraction impurity and/or the light fraction impurity to flow into the dense chamber as a fluid, the dense chamber outlet for the fluid to exit.
In one or more embodiments of the utility model, the continuous electrodeionization device includes a plurality of spaced apart dilute and concentrated compartments.
In one or more embodiments of the utility model, the apparatus for producing ethyl orthosilicate further comprises a mixer for mixing raw materials, the mixer being in communication with the continuous electrodeionization device.
In one or more embodiments of the utility model, the apparatus for producing ethyl orthosilicate further comprises a tail gas treatment device in communication with the reactor and/or the mixer.
In one or more embodiments of the utility model, a condenser is also provided between the reactor and the tail gas treatment device.
In one or more embodiments of the present utility model, the apparatus for producing ethyl orthosilicate further comprises:
the first raw material tank is used for containing silicon tetrachloride raw materials and is communicated with the mixer;
and the second raw material tank is used for containing ethanol raw materials and is communicated with the mixer.
In one or more embodiments of the present utility model, a first reboiler is arranged outside the bottom of the light component removal rectifying tower, a second reboiler is arranged outside the bottom of the heavy component removal rectifying tower, and a heater is arranged outside the reactor; the first reboiler, the second reboiler and the heater are respectively used for heating the light component removal rectifying tower, the heavy component removal rectifying tower and the reactor through heating mediums;
the heating medium flows through the first reboiler and/or the second reboiler and then enters the heater.
In one or more embodiments of the utility model, the heater is a jacketed heater.
In one or more embodiments of the utility model, the apparatus for producing ethyl orthosilicate further comprises a tailings treatment device in communication with the continuous electrodeionization device for collecting tailings discharged by the continuous electrodeionization device.
Compared with the prior art, the production equipment of the ethyl orthosilicate has the beneficial effects that:
(1) According to the utility model, the reaction raw materials are mixed and then are introduced into the continuous electrodeionization device, and metal ions in the raw materials are rapidly removed under the combined action of the ion-conductive materials in the continuous electrodeionization device and an electric field generated by the ion-conductive materials, so that the pollution of the reactor caused by the metal ions entering the reactor is avoided, and the product (ethyl orthosilicate) is always influenced by the metal ions.
(2) In the utility model, when the metal ions are removed, the metal ions are coated with a layer of raw material, so that the loss of some raw materials is caused, but the raw materials are mixed firstly, and the ethanol in the raw materials is excessive, so that most of the lost raw materials are ethanol, the loss of silicon tetrachloride is small, and the yield of subsequent products can be improved.
(3) In the utility model, the mixed raw materials are firstly subjected to metal ion removal by a continuous electrodeionization technology, so that the load of metal ion removal during product purification is reduced, and the product separation is easier (the process can be regarded as the process of purifying the product through a rectifying tower).
(4) In the utility model, the mixed raw materials are firstly subjected to metal ion removal through a continuous electrodeionization technology, and although a part of raw materials are lost, compared with a mode of firstly reacting to generate a product and then removing metal ions, the product is lost in the removal process, and the product is generated by reacting after the raw materials consume energy, so that the energy consumption required by removing the metal ions can be reduced.
Drawings
Fig. 1 is a schematic view of a production facility of ethyl orthosilicate according to an embodiment of the utility model.
The main reference numerals illustrate:
1. a continuous electrodeionization device; 11. a light room; 111. a dilute chamber inlet; 112. a dilute chamber outlet; 12. a concentration chamber; 121. a dense chamber outlet; 122. an inlet of the dense chamber; 2. a reactor; 21. a condenser; 22. a heater; 3. a light component removing rectifying tower; 31. a light component outlet; 32. a first reboiler; 4. a heavy-removal rectifying tower; 41. a heavy component outlet; 42. a second reboiler; 5. a mixer; 6. a tail gas treatment device; 7. a first feedstock tank; 8. a second feedstock tank; 9. and a tailing processing device.
Detailed Description
The following detailed description of embodiments of the utility model is, therefore, to be taken in conjunction with the accompanying drawings, and it is to be understood that the scope of the utility model is not limited to the specific embodiments.
Throughout the specification and claims, unless explicitly stated otherwise, the term "comprise" or variations thereof such as "comprises" or "comprising", etc. will be understood to include the stated element or component without excluding other elements or components.
As shown in fig. 1, the production apparatus of ethyl orthosilicate according to an embodiment of the utility model comprises a continuous electrodeionization device 1, a reactor 2, a light-component removal rectifying tower 3 and a heavy-component removal rectifying tower 4: the continuous electrodeionization device 1 is used for separating metal ions in the mixed raw materials; the reactor 2 is communicated with the continuous electrodeionization device 1 and is used for reacting raw materials separated by metal ions by the continuous electrodeionization device 1 to generate a crude product of tetraethoxysilane; the light component removing rectifying tower 3 is communicated with the reactor 2 and is used for removing light component impurities in the crude product of the tetraethoxysilane; the heavy-removal rectifying tower 4 is communicated with the light-removal rectifying tower 3 and is used for removing heavy component impurities in the crude product of the ethyl orthosilicate.
Wherein, the reactor 2 can be made of 316L stainless steel and the inner wall is lined with polytetrafluoroethylene material so as to avoid introducing new impurities and avoiding corrosion of equipment caused by hydrogen chloride generated by reaction. The light component removing rectifying tower 3 and heavy component removing rectifying tower 4 can be made of 316L material which is subjected to internal electrolytic polishing so as to avoid introducing new impurities.
The ethyl orthosilicate and the unreacted excessive ethanol generated by the reaction in the reactor 2 flow out from the bottom of the reactor 2 and enter the light component removing rectifying tower 3, so that the light component impurities are removed and flow out from the top of the light component removing rectifying tower 3. The mixture after the light component impurities are removed flows out of the bottom of the light component removal rectifying tower 3 and enters the heavy component removal rectifying tower 4 to remove heavy component impurities, the heavy component impurities flow out of the bottom of the heavy component removal rectifying tower 4, and the product electronic grade ethyl orthosilicate is extracted from the top of the heavy component removal rectifying tower 4. Specifically, the reactor 2 may be a reaction vessel.
In one embodiment, the heavy component removing rectifying tower 4 is provided with a heavy component outlet 41 for discharging heavy component impurities, and the light component removing rectifying tower 3 is provided with a light component outlet 31 for discharging light component impurities; the continuous electrodeionization device 1 includes a dilute chamber 11 and a dense chamber 12: the light chamber 11 has a light chamber inlet 111 and a light chamber outlet 112 for the mixed raw materials to enter and exit, and the reactor 2 is communicated with the light chamber outlet 112; the dense chamber 12 is for receiving the metal ions separated in the dilute chamber 11, the dense chamber 12 has a dense chamber outlet 121 and a dense chamber inlet 122, and the dense chamber inlet 122 is in communication with the heavy fraction outlet 41 and/or the light fraction outlet 31 for the heavy fraction impurities and/or the light fraction impurities to flow into the dense chamber 12 as a fluid, and the dense chamber outlet 121 is for the fluid to drain.
The light component impurities at the top of the light component removal rectifying tower 3 and/or the heavy component impurities at the bottom of the heavy component removal rectifying tower 4 are used as fluid in the dense chamber 12, and are received from metal ions separated from the dilute chamber 11, so that other materials with higher value are not used, the separated materials with high impurity content are reasonably utilized, the effect of recycling resources is achieved, and the material cost of impurity removal is reduced.
The continuous electrodeionization device 1 further includes a cathode and an anode to generate an electric field. The continuous electrodeionization apparatus 1 is a technology for removing metal ions by using a continuous electrodeionization technique (continuous electrodeionzation), which is a technique for separating ionic or ionizable substances (impurities) in a fluid by using a combination of ion-conductive materials such as ion exchange resins and ion exchange membranes and an electric field. Under the action of the electric field, anions and cations migrate through the ion exchange resin and the ion exchange membrane respectively, so that ions in the dilute chamber 11 are reduced, ions in the dense chamber 12 are increased, and fluid flowing out of the dilute chamber 11 is fluid from which metal ions are removed.
Further, the continuous electrodeionization device 1 includes a plurality of dilute chambers 11 and dense chambers 12 arranged at intervals, thereby improving the efficiency of impurity removal.
In one embodiment, the apparatus for producing ethyl orthosilicate further comprises a mixer 5 for mixing the raw materials, the mixer 5 being in communication with the continuous electrodeionization device 1.
In a specific embodiment, the apparatus for producing ethyl orthosilicate further comprises a tail gas treatment device 6, wherein the tail gas treatment device 6 is communicated with the reactor 2 and/or the mixer 5. The tetraethoxysilane is prepared by reacting a silicon tetrachloride raw material with an ethanol raw material, and hydrogen chloride gas is generated in the reaction process, so that the tail gas treatment device 6 plays a role in treating the hydrogen chloride gas. The tail gas treatment device 6 is connected with the mixer 5 because the silicon tetrachloride raw material and the ethanol raw material are fed into the mixer 5, and partial reaction occurs in the mixer 5 to generate a small amount of hydrogen chloride gas, so that the tail gas treatment device 6 is also required for treatment. Wherein the tail gas treatment device 6 may be in communication with the top of the reactor 2 and/or the top of the mixer 5.
In a specific embodiment, a condenser 21 is further provided between the reactor 2 and the tail gas treatment device 6. The vaporized ethanol is condensed by the condenser 21 and flows back to the reactor 2 by gravity to continue the reaction.
In one or more embodiments of the present utility model, the production apparatus of ethyl orthosilicate further includes a first raw material tank 7 and a second raw material tank 8; the first raw material tank 7 is used for containing silicon tetrachloride raw materials and is communicated with the mixer 5; the second raw material tank 8 is used for containing ethanol raw material and is communicated with the mixer 5.
In one or more embodiments of the present utility model, a first reboiler 32 is arranged outside the bottom of the light component removal rectifying tower 3, a second reboiler 42 is arranged outside the bottom of the heavy component removal rectifying tower 4, and a heater 22 is arranged outside the reactor 2; the first reboiler 32, the second reboiler 42 and the heater 22 heat the light component removal rectifying tower 3, the heavy component removal rectifying tower 4 and the reactor 2 respectively through heating mediums; wherein the heating medium flows through the first reboiler 32 and/or the second reboiler 42 before entering the heater 22.
It will be appreciated that the heater 22 may be a jacketed heater and is disposed over the outside of the reactor 2 to provide heating by the heating medium flowing within the jacketed heater. The reaction temperature of the silicon tetrachloride raw material and the ethanol raw material is lower than the temperature of the light component removal rectifying tower 3 and the heavy component removal rectifying tower 4 in the rectifying process, so that the temperature of the heating medium in the first reboiler 32 and the second reboiler 42 can be kept higher after the heating medium flows out and can be reused, and the heating medium can be sent into the heater 22 to be used as the heating medium for continuous use, thereby playing a role in saving energy.
In this embodiment, the devices or structures may be connected by a pipe, and a metering pump may be mounted on the pipe, so as to play a role in driving the liquid in the pipe to flow.
In one embodiment, the production equipment of the tetraethoxysilane further comprises a tailing treatment device 9, wherein the tailing treatment device 9 is communicated with the continuous electrodeionization device 1 and is used for collecting tailings discharged by the continuous electrodeionization device 1. Specifically, the tailings disposal device 9 may be in communication with the concentrate chamber outlet 121 via a conduit. The tailings may be considered as the fluid exiting the rich chamber outlet 121.
The process for preparing the ethyl orthosilicate by the production equipment of the ethyl orthosilicate can comprise the following steps:
and uniformly mixing the silicon tetrachloride raw material and the ethanol raw material in a reactor 2 to obtain a mixed raw material.
And (3) feeding the mixed raw materials into a continuous electrodeionization device 1, separating metal ions in the mixed raw materials, feeding the separated metal ions into a reactor 2, and reacting to obtain a crude product of the tetraethoxysilane.
And (3) sequentially feeding the crude product of the ethyl orthosilicate into a light-removal rectifying tower 3 and a heavy-removal rectifying tower 4, and removing light component impurities and heavy component impurities in the crude product of the ethyl orthosilicate to obtain the purified ethyl orthosilicate.
In summary, the production equipment of the ethyl orthosilicate has the following beneficial effects:
(1) According to the utility model, the reaction raw materials are mixed and then are introduced into the continuous electrodeionization device, and metal ions in the raw materials are rapidly removed under the combined action of the ion-conductive materials in the continuous electrodeionization device and an electric field generated by the ion-conductive materials, so that the pollution of the reactor caused by the metal ions entering the reactor is avoided, and the product (ethyl orthosilicate) is always influenced by the metal ions.
(2) In the utility model, when the metal ions are removed, the metal ions are coated with a layer of raw material, so that the loss of some raw materials is caused, but the raw materials are mixed firstly, and the ethanol in the raw materials is excessive, so that most of the lost raw materials are ethanol, the loss of silicon tetrachloride is small, and the yield of subsequent products can be improved.
(3) In the utility model, the mixed raw materials are firstly subjected to metal ion removal by a continuous electrodeionization technology, so that the load of metal ion removal during product purification is reduced, and the product separation is easier (the process can be regarded as the process of purifying the product through a rectifying tower).
(4) In the utility model, the mixed raw materials are firstly subjected to metal ion removal through a continuous electrodeionization technology, and although a part of raw materials are lost, compared with a mode of firstly reacting to generate a product and then removing metal ions, the product is lost in the removal process, and the product is generated by reacting after the raw materials consume energy, so that the energy consumption required by removing the metal ions can be reduced.
(5) In the utility model, the light component impurities at the top of the light removal rectifying tower and the heavy component impurities at the bottom of the heavy removal rectifying tower are used as fluid in the concentration chamber, the fluid is received from the metal ions separated in the light chamber, other materials with higher value are not used, and the separated materials with high impurity content are reasonably utilized.
(6) According to different energy levels of the heating medium, the heating medium is reasonably used. After the heating mediums of the two rectifying towers are respectively discharged from the two rectifying towers, the temperature is higher, the heating mediums can be reused, and the heater fed into the reactor is used as the heating mediums for continuous use, so that the utilization rate of energy sources is improved, and the energy consumption is reduced.
The foregoing descriptions of specific exemplary embodiments of the present utility model are presented for purposes of illustration and description. It is not intended to limit the utility model to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain the specific principles of the utility model and its practical application to thereby enable one skilled in the art to make and utilize the utility model in various exemplary embodiments and with various modifications as are suited to the particular use contemplated. It is intended that the scope of the utility model be defined by the claims and their equivalents.
Claims (10)
1. A production facility of ethyl orthosilicate, characterized by comprising:
the continuous electrodeionization device is used for separating metal ions in the mixed raw materials;
the reactor is communicated with the continuous electrodeionization device and is used for enabling raw materials separated from metal ions by the continuous electrodeionization device to react to generate crude ethyl orthosilicate;
the light component removing rectifying tower is communicated with the reactor and is used for removing light component impurities in the crude product of the ethyl orthosilicate;
and the heavy-removal rectifying tower is communicated with the light-removal rectifying tower and is used for removing heavy component impurities in the crude product of the ethyl orthosilicate.
2. The apparatus for producing ethyl orthosilicate as set forth in claim 1, wherein said heavy fraction removal rectifying column has a heavy fraction outlet from which said heavy fraction impurities flow out, and said light fraction removal rectifying column has a light fraction outlet from which said light fraction impurities flow out; the continuous electrodeionization device comprises:
a light chamber having a light chamber inlet and a light chamber outlet for the mixed raw materials to enter and exit, the reactor being in communication with the light chamber outlet;
a dense chamber for receiving the metal ions separated in the dilute chamber, the dense chamber having a dense chamber outlet and a dense chamber inlet, and the dense chamber inlet being in communication with the heavy fraction outlet and/or the light fraction outlet for the heavy fraction impurity and/or the light fraction impurity to flow into the dense chamber as a fluid, the dense chamber outlet for the fluid to exit.
3. The apparatus for producing ethyl orthosilicate as set forth in claim 2, wherein the continuous electrodeionization device comprises a plurality of spaced apart dilute and concentrated compartments.
4. The apparatus for producing ethyl orthosilicate as set forth in claim 1, further comprising a mixer for mixing raw materials, the mixer being in communication with the continuous electrodeionization device.
5. The apparatus for producing ethyl orthosilicate as set forth in claim 4, further comprising a tail gas treatment device in communication with the reactor and/or the mixer.
6. The apparatus for producing ethyl orthosilicate as claimed in claim 4, wherein a condenser is further provided between the reactor and the tail gas treatment device.
7. The apparatus for producing ethyl orthosilicate as set forth in claim 4, further comprising:
the first raw material tank is used for containing silicon tetrachloride raw materials and is communicated with the mixer;
and the second raw material tank is used for containing ethanol raw materials and is communicated with the mixer.
8. The production equipment of the ethyl orthosilicate as set forth in claim 1, wherein a first reboiler is arranged outside the bottom of the light component removal rectifying tower, a second reboiler is arranged outside the bottom of the heavy component removal rectifying tower, and a heater is arranged outside the reactor; the first reboiler, the second reboiler and the heater are respectively used for heating the light component removal rectifying tower, the heavy component removal rectifying tower and the reactor through heating mediums;
the heating medium flows through the first reboiler and/or the second reboiler and then enters the heater.
9. The apparatus for producing ethyl orthosilicate as set forth in claim 8, wherein the heater is a jacket heater.
10. The apparatus for producing ethyl orthosilicate as set forth in claim 1, further comprising a tailings disposal device in communication with the continuous electrodeionization device for collecting tailings from the continuous electrodeionization device.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202320671924.9U CN219463370U (en) | 2023-03-30 | 2023-03-30 | Production equipment of ethyl orthosilicate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202320671924.9U CN219463370U (en) | 2023-03-30 | 2023-03-30 | Production equipment of ethyl orthosilicate |
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| Publication Number | Publication Date |
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| CN219463370U true CN219463370U (en) | 2023-08-04 |
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| CN202320671924.9U Active CN219463370U (en) | 2023-03-30 | 2023-03-30 | Production equipment of ethyl orthosilicate |
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