CN203959836U - The system of purifying silicon tetrachloride - Google Patents
The system of purifying silicon tetrachloride Download PDFInfo
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- CN203959836U CN203959836U CN201420353786.0U CN201420353786U CN203959836U CN 203959836 U CN203959836 U CN 203959836U CN 201420353786 U CN201420353786 U CN 201420353786U CN 203959836 U CN203959836 U CN 203959836U
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Abstract
The system that the utility model discloses a kind of purifying silicon tetrachloride, comprising: rectifying tower body, limits absorption distillation section, lights removal section and heavies removal section from top to bottom successively in described rectifying tower body; Silicon tetrachloride entrance, described silicon tetrachloride entrance is arranged between described absorption distillation section and described lights removal section; Silicon tetrachloride outlet, described silicon tetrachloride outlet is arranged between described lights removal section and described heavies removal section; Vapour outlet, described vapour outlet is arranged on described absorption distillation section top; And heavy constituent outlet, described heavy constituent outlet is arranged on described heavies removal section bottom.This system can prepare the silicon tetrachloride of optical fiber rank, and can realize large scale continuous prod.
Description
Technical field
The utility model belongs to field of polysilicon production, and particularly, the utility model relates to a kind of system of purifying silicon tetrachloride.
Background technology
In recent years, along with the development of China's informatization, market constantly increases the demand of fiber products, aggregate demand breaks through 100,000,000 core kilometers, there is the phenomenon that optical fiber is under-supply in market, and the important technology factor that restriction optical fiber output increases is exactly that China is too high to the degree of dependence of one of import preform and important source material thereof ultrapure silicon tetrachloride (ultralow-hydrogen low content silicon tetrachloride) for optical fiber.So, be the development of supporting that national information is built, the technology that optical fiber ultrapure silicon tetrachloride is prepared in research and development becomes the task of top priority.
The method of preparing optical fiber ultrapure silicon tetrachloride mainly comprises rectification method, absorption process, partial hydrolysis method, complexometry, light chlorination process etc.Wherein rectifying tower and absorption process belong to Physical, only can prepare the silicon tetrachloride of certain purity, in the time preparing optical fiber ultrapure silicon tetrachloride, have problems; Partial hydrolysis method, complexometry and light chlorination process belong to chemical method, remove the impurity in silicon tetrachloride by reaction, can be for the preparation of optical fiber ultrapure silicon tetrachloride, but because partial hydrolysis method and complexometry have operational difficulty and shortcoming that cannot scale operation, its application is restricted.
At present domestic preparation on a large scale aspect optical fiber ultrapure silicon tetrachloride also in blank.Beijing total institute of coloured research discloses a kind of rectifying formula photochlorination apparatus (number of patent application: 200910260296.X), and this device is only applicable to laboratory study, cannot realize continuous production and effectively industry amplification.Wuhan New Silicon Technology Co., Ltd. discloses the continuous distillation method of a kind of optical fiber high purity silicon tetrachloride, though solved the problem of continuous and scale operation, the purity of silicon tetrachloride cannot reach ultrapure requirement.
Therefore, the technology of existing purifying silicon tetrachloride need further research.
Utility model content
The utility model is intended to solve at least to a certain extent one of technical problem in correlation technique.For this reason, an object of the present utility model is to propose a kind of system of purifying silicon tetrachloride, and this system can prepare the silicon tetrachloride of optical fiber rank, and can realize large scale continuous prod.
Aspect one of the present utility model, the utility model proposes a kind of system of purifying silicon tetrachloride, comprising:
Rectifying tower body, limits absorption distillation section, lights removal section and heavies removal section from top to bottom successively in described rectifying tower body;
Silicon tetrachloride entrance, described silicon tetrachloride entrance is arranged between described absorption distillation section and described lights removal section;
Silicon tetrachloride outlet, described silicon tetrachloride outlet is arranged between described lights removal section and described heavies removal section;
Vapour outlet, described vapour outlet is arranged on described absorption distillation section top; And
Heavy constituent outlet, described heavy constituent outlet is arranged on described heavies removal section bottom.
According to the system of the purifying silicon tetrachloride of the utility model embodiment by adsorb and rectifying in single tower simultaneously, efficiently solve system operation difficulty and problem that cannot large scale continuous prod, and operational efficiency and the operation continuity of system are significantly improved, simultaneously, absorption is combined with rectifying, in absorption, carry out heat and mass, ensured the purity of silicon tetrachloride product, thereby can prepare the silicon tetrachloride of optical fiber rank.
In addition, can also there is following additional technical characterictic according to the system of the purifying silicon tetrachloride of the utility model above-described embodiment:
In embodiment more of the present utility model, the system of described purifying silicon tetrachloride further comprises: silicon tetrachloride vaporization device, and described silicon tetrachloride vaporization device has liquid silicon tetrachloride entrance, the heavy constituent of not vaporizing outlet and the outlet of gas silicon tetrachloride; And silicon tetrachloride superheater, described silicon tetrachloride superheater has gas silicon tetrachloride entrance and the outlet of overheated silicon tetrachloride, and institute's gas silicon tetrachloride entrance is connected with described gas silicon tetrachloride outlet, described overheated silicon tetrachloride outlet is connected with described silicon tetrachloride entrance.Thus, can effectively prepare the silicon tetrachloride of optical fiber rank.
In embodiment more of the present utility model, the system of described purifying silicon tetrachloride further comprises: the first refrigerating unit, described the first refrigerating unit has steam-in and condensate outlet, and described steam-in is connected with described vapour outlet, described condensate outlet is connected with described absorption distillation section; And second refrigerating unit, described the second refrigerating unit has light constituent entrance and through overcooled light constituent outlet, and described light constituent entrance is connected with described condensate outlet.Thus, light constituent in can efficient recovery system.
In embodiment more of the present utility model, the system of described purifying silicon tetrachloride further comprises: the 3rd refrigerating unit, described the 3rd refrigerating unit has the silicon tetrachloride outlet of rectifying silicon tetrachloride entrance and purifying, and described rectifying silicon tetrachloride entrance is connected with described silicon tetrachloride outlet; And the 4th refrigerating unit, described the 4th refrigerating unit exports and is connected with described do not vaporize heavy constituent outlet and described heavy constituent.Thus, heavy constituent in can efficient recovery system.
In embodiment more of the present utility model, the internals of described absorption distillation section are the structured packing with surface recombination sorbent material, and number of theoretical plate is 10～20.Thus, can significantly improve absorption distillation efficiency.
In embodiment more of the present utility model, the internals of described lights removal section are wire cloth structured packing and plate ripple arranged packing, and number of theoretical plate is 20～40.Thus, can significantly improve lights removal efficiency.
In embodiment more of the present utility model, the internals of described heavies removal section are wire cloth structured packing and plate ripple arranged packing, and number of theoretical plate is 5～15.Thus, can significantly improve heavies removal efficiency.
Brief description of the drawings
Fig. 1 is according to the system architecture schematic diagram of the purifying silicon tetrachloride of an embodiment of the utility model;
Fig. 2 is according to the system architecture schematic diagram of the purifying silicon tetrachloride of another embodiment of the utility model.
Embodiment
Describe embodiment of the present utility model below in detail, the example of described embodiment is shown in the drawings, and wherein same or similar label represents same or similar element or has the element of identical or similar functions from start to finish.Be exemplary below by the embodiment being described with reference to the drawings, be intended to for explaining the utility model, and can not be interpreted as restriction of the present utility model.
In description of the present utility model, it will be appreciated that, term " " center ", " longitudinally ", " laterally ", " length ", " width ", " thickness ", " on ", D score, " front ", " afterwards ", " left side ", " right side ", " vertically ", " level ", " top ", " end " " interior ", " outward ", " clockwise ", " counterclockwise ", " axially ", " radially ", orientation or the position relationship of instructions such as " circumferentially " are based on orientation shown in the drawings or position relationship, only the utility model and simplified characterization for convenience of description, instead of device or the element of instruction or hint indication must have specific orientation, with specific orientation structure and operation, therefore can not be interpreted as restriction of the present utility model.
In addition, term " first ", " second " be only for describing object, and can not be interpreted as instruction or hint relative importance or the implicit quantity that indicates indicated technical characterictic.Thus, at least one this feature can be expressed or impliedly be comprised to the feature that is limited with " first ", " second ".In description of the present utility model, the implication of " multiple " is at least two, for example two, and three etc., unless otherwise expressly limited specifically.
In the utility model, unless otherwise clearly defined and limited, the terms such as term " installation ", " being connected ", " connection ", " fixing " should be interpreted broadly, and for example, can be to be fixedly connected with, and can be also to removably connect, or integral; Can be mechanical connection, can be also electrical connection; Can be to be directly connected, also can indirectly be connected by intermediary, can be the connection of two element internals or the interaction relationship of two elements, unless separately there is clear and definite restriction.For the ordinary skill in the art, can understand as the case may be the concrete meaning of above-mentioned term in the utility model.
In the utility model, unless otherwise clearly defined and limited, First Characteristic Second Characteristic " on " or D score can be that the first and second features directly contact, or the first and second features are by intermediary indirect contact.And, First Characteristic Second Characteristic " on ", " top " and " above " but First Characteristic directly over Second Characteristic or oblique upper, or only represent that First Characteristic level height is higher than Second Characteristic.First Characteristic Second Characteristic " under ", " below " and " below " can be First Characteristic under Second Characteristic or tiltedly, or only represent that First Characteristic level height is less than Second Characteristic.
Aspect one of the present utility model, the utility model proposes a kind of system of purifying silicon tetrachloride.The system of the purifying silicon tetrachloride below with reference to Fig. 1-2 to the utility model embodiment is described in detail.According to embodiment of the present utility model, this system comprises:
Rectifying tower body 100: according to embodiment of the present utility model, limit successively absorption distillation section 11, lights removal section 12 and heavies removal section 13 in rectifying tower body 100 from top to bottom.According to embodiment of the present utility model, between absorption distillation section 11 and lights removal section 12, be provided with silicon tetrachloride entrance 14, for silicon tetrachloride being supplied to rectifying tower body 100.According to embodiment of the present utility model, between lights removal section 12 and heavies removal section 13, be provided with silicon tetrachloride outlet 15, for the silicon tetrachloride through rectification process is discharged to rectifying tower body 100.According to embodiment of the present utility model, absorption distillation section 11 tops are provided with vapour outlet 16, for the steam producing is discharged to rectifying tower body 100.According to embodiment of the present utility model, heavies removal section 13 bottoms are provided with heavy constituent outlet 17, discharge rectifying body 100 for the heavy constituent that rectification process is obtained.
According to embodiment of the present utility model, absorption distillation section 11 is carried out the condition of absorption distillation and is not particularly limited, and according to specific embodiment of the utility model, the tower top temperature of absorption distillation section can be 65～95 degrees Celsius, and pressure can be 0.05～0.2MPa.Particularly, the internals of absorption distillation section can be the structured packing with surface recombination sorbent material, and theoretical plate number is 10～20.
According to embodiment of the present utility model, lights removal section 12 is carried out the condition of rectification process and is not particularly limited, according to specific embodiment of the utility model, the head temperature of lights removal section can be 65～95 degrees Celsius, and pressure can be 0.05～0.2MPa.Particularly, the internals of lights removal section can be wire cloth structured packing and plate ripple arranged packing, and number of theoretical plate is 20～40.
According to embodiment of the present utility model, heavies removal section 13 is carried out the condition of rectification process and is not particularly limited, according to specific embodiment of the utility model, the head temperature of heavies removal section can be 75～95 degrees Celsius, and pressure can be 0.05～0.2MPa.Particularly, the internals of heavies removal section 13 can be wire cloth structured packing and plate ripple arranged packing, and number of theoretical plate is 5～15.
According to the system of the purifying silicon tetrachloride of the utility model embodiment by adsorb and rectifying in single tower simultaneously, efficiently solve system operation difficulty and problem that cannot large scale continuous prod, and operational efficiency and the operation continuity of system are significantly improved, simultaneously, absorption is combined with rectifying, in absorption, carry out heat and mass, ensured the purity of silicon tetrachloride product, thereby can prepare the silicon tetrachloride of optical fiber rank.
With reference to figure 2, further comprise according to the system of the purifying silicon tetrachloride of the utility model embodiment:
Silicon tetrachloride vaporization device 200: according to embodiment of the present utility model, silicon tetrachloride vaporization device 200 has liquid silicon tetrachloride entrance 21, the heavy constituent of not vaporizing outlet 22 and gas silicon tetrachloride outlet 23, and be suitable for liquid silicon tetrachloride to carry out vaporization process, thereby can obtain gas silicon tetrachloride.According to embodiment of the present utility model, the condition of in silicon tetrachloride vaporization device, liquid silicon tetrachloride being vaporized is also not particularly limited, according to specific embodiment of the utility model, it can be that 85～105 degrees Celsius and pressure are to carry out under 0.1～0.25MPa pressure condition in temperature that liquid silicon tetrachloride is vaporized.Particularly, liquid silicon tetrachloride is vaporized, owing to containing part heavy constituent in liquid silicon tetrachloride, by temperature control, can make wherein entrained part heavy constituent impurity not vaporize, thereby can obtain gas silicon tetrachloride thus, thus, can significantly improve the purity of silicon tetrachloride.
Silicon tetrachloride superheater 300: silicon tetrachloride superheater 300 has gas silicon tetrachloride entrance 31 and overheated silicon tetrachloride outlet 32, and gas silicon tetrachloride entrance 31 is connected with gas silicon tetrachloride outlet 23, and be suitable for gas silicon tetrachloride to carry out Overheating Treatment, thereby can obtain overheated silicon tetrachloride.According to embodiment of the present utility model, overheated silicon tetrachloride outlet 32 is connected with silicon tetrachloride entrance 14, and is suitable for silicon tetrachloride to be supplied in rectifying tower body 100.According to embodiment of the present utility model, in silicon tetrachloride superheater 300, gas silicon tetrachloride is carried out the condition of Overheating Treatment and is not particularly limited, according to specific embodiment of the utility model, it is to carry out under 0.1～0.25MPa pressure condition with pressure that Overheating Treatment can be 95～115 degrees Celsius in temperature.Particularly, contriver finds, gas silicon tetrachloride is carried out to Overheating Treatment and can effectively avoid silicon tetrachloride vapor to liquefy in course of conveying and increase transporting resistance.
The first refrigerating unit 400: according to embodiment of the present utility model, the first refrigerating unit 400 has steam-in 41 and condensate outlet 42, and steam-in 41 is connected with vapour outlet 16, the vapour mixture being suitable for producing in rectifying tower body carries out the first cooling process, thereby can obtain phegma and light constituent, condensate outlet 42 is connected with absorption distillation section 11, is suitable for returning using a part for phlegma as phegma to absorption distillation section and proceeds rectification process.According to embodiment of the present utility model, in phegma, contain silicon tetrachloride.According to embodiment of the present utility model, phegma can be 10～15 with the mass flow rate of the liquid silicon tetrachloride that is supplied to silicon tetrachloride vaporization device.According to embodiment of the present utility model, the condition of the first cooling process is also not particularly limited, and according to specific embodiment of the utility model, it is to carry out under 0.05～0.2MPa pressure condition with pressure that the first cooling process can be 55～85 degrees Celsius in temperature.
The second refrigerating unit 500: according to embodiment of the present utility model, the second refrigerating unit 500 has light constituent entrance 51 and exports 52 through overcooled light constituent, and light constituent entrance 51 is connected with condensate outlet 42, and the another part that is suitable for the phlegma to obtaining from the first refrigerating unit 400 carries out the second cooling process as light constituent.According to embodiment of the present utility model, the condition of the second cooling process is also not particularly limited, and according to specific embodiment of the utility model, it is to carry out under 0.05～0.2MPa pressure condition with pressure that the second cooling process can be 25～65 degrees Celsius in temperature.According to embodiment of the present utility model, light constituent can contain trichlorosilane and a small amount of silicon tetrachloride.
The 3rd refrigerating unit 600: according to embodiment of the present utility model, the 3rd refrigerating unit 600 has the silicon tetrachloride outlet 62 of rectifying silicon tetrachloride entrance 61 and purifying, and rectifying silicon tetrachloride entrance 61 is connected with silicon tetrachloride outlet 15, and be suitable for the silicon tetrachloride through rectification process to carry out the 3rd cooling process, thereby can obtain the silicon tetrachloride of purifying.According to embodiment of the present utility model, the condition of the 3rd cooling process is also not particularly limited, and according to specific embodiment of the utility model, it is to carry out under 0.05～0.2MPa pressure condition with pressure that the 3rd cooling process can be 75～95 degrees Celsius in temperature.According to embodiment of the present utility model, the purity of the silicon tetrachloride of the purifying obtaining can be 99.9999～99.999999%.
The 4th refrigerating unit 700: according to embodiment of the present utility model, the 4th refrigerating unit 700 is connected with heavy constituent outlet 17 with the heavy constituent outlet 22 of not vaporizing, and is suitable for heavy constituent to carry out the 4th cooling process.According to embodiment of the present utility model, the condition of the 4th cooling process is also not particularly limited, and according to specific embodiment of the utility model, it is to carry out under 0.05～0.2MPa pressure condition with pressure that the 4th cooling process can be 35～85 degrees Celsius in temperature.According to embodiment of the present utility model, heavy constituent can contain methyl chlorosilane and a small amount of silicon tetrachloride.
As mentioned above, can have and be selected from following advantage one of at least according to the system of the purifying silicon tetrachloride of the utility model embodiment:
, by being combined with rectifying, absorption conducts heat in absorption according to the system of the purifying silicon tetrachloride of the utility model embodiment, thus the purity of guarantee silicon tetrachloride product;
According to the system of the purifying silicon tetrachloride of the utility model embodiment, adsorption treatment and rectification process are realized at Dan Tazhong, operation is simple, energy-saving and cost-reducing.
Below with reference to specific embodiment, the utility model is described, it should be noted that, these embodiment are only descriptive, and limit never in any form the utility model.
Embodiment
First through silicon tetrachloride vaporization device 200 carry out vaporization process from the liquid silicon tetrachloride A that operation is come above, thereby obtain respectively gas silicon tetrachloride and the heavy constituent of not vaporizing, wherein gas silicon tetrachloride is supplied to silicon tetrachloride superheater 300, obtain overheated silicon tetrachloride, then the overheated silicon tetrachloride obtaining is supplied to rectifying tower body by the silicon tetrachloride entrance between absorption distillation section and lights removal section, after the vapor mixing of Ta Nei and the rising of lights removal section, carry out absorption distillation section absorption impurity, carry out rectification process simultaneously, the vapour mixture that contains light constituent is discharged from the vapour outlet at absorption distillation section top, then carry out the first cooling process through the first refrigerating unit 400, obtain phlegma, be supplied to the second refrigerating unit 500 using a part for phlegma as light constituent and carry out the second cooling process, obtain through overcooled light constituent B, steam and overheated silicon tetrachloride that another part of phlegma is back to absorption distillation section and rising as phegma carry out heat and mass, the silicon tetrachloride that processing obtains through absorption distillation continues to enter lights removal section and carries out rectification process, the light constituent obtaining passes through absorption distillation section successively, the first refrigerating unit and the second refrigerating unit, and discharge from the silicon tetrachloride outlet between light constituent rectifying section and heavy constituent rectifying section through the silicon tetrachloride of rectification process, obtain the silicon tetrachloride C (purity is 99.9999～99.999999%) of purifying through the 3rd refrigerating unit 600, and continuing to enter heavies removal section, the heavy constituent obtaining carries out rectification process, in like manner, light constituent passes through lights removal section successively, absorption distillation section, the first refrigerating unit and the second refrigerating unit, and heavy constituent is discharged from the bottom of heavies removal section, after the not vaporization heavy constituent that obtains is mixed, deliver to the 4th refrigerating unit 700 and carry out the 4th cooling process with separating in silicon tetrachloride vaporization device, obtain through overcooled heavy constituent D.
In the description of this specification sheets, the description of reference term " embodiment ", " some embodiment ", " example ", " concrete example " or " some examples " etc. means to be contained at least one embodiment of the present utility model or example in conjunction with specific features, structure, material or the feature of this embodiment or example description.In this manual, to the schematic statement of above-mentioned term not must for be identical embodiment or example.And, specific features, structure, material or the feature of description can one or more embodiment in office or example in suitable mode combination.In addition,, not conflicting in the situation that, those skilled in the art can carry out combination and combination by the feature of the different embodiment that describe in this specification sheets or example and different embodiment or example.
Although illustrated and described embodiment of the present utility model above, be understandable that, above-described embodiment is exemplary, can not be interpreted as restriction of the present utility model, those of ordinary skill in the art can change above-described embodiment in scope of the present utility model, amendment, replacement and modification.
Claims (7)
1. a system for purifying silicon tetrachloride, is characterized in that, comprising:
Rectifying tower body, limits absorption distillation section, lights removal section and heavies removal section from top to bottom successively in described rectifying tower body;
Silicon tetrachloride entrance, described silicon tetrachloride entrance is arranged between described absorption distillation section and described lights removal section;
Silicon tetrachloride outlet, described silicon tetrachloride outlet is arranged between described lights removal section and described heavies removal section;
Vapour outlet, described vapour outlet is arranged on described absorption distillation section top; And
Heavy constituent outlet, described heavy constituent outlet is arranged on described heavies removal section bottom.
2. the system of purifying silicon tetrachloride according to claim 1, is characterized in that, further comprises:
Silicon tetrachloride vaporization device, described silicon tetrachloride vaporization device has liquid silicon tetrachloride entrance, the heavy constituent of not vaporizing outlet and the outlet of gas silicon tetrachloride; And
Silicon tetrachloride superheater, described silicon tetrachloride superheater has gas silicon tetrachloride entrance and the outlet of overheated silicon tetrachloride, and described gas silicon tetrachloride entrance is connected with described gas silicon tetrachloride outlet, described overheated silicon tetrachloride outlet is connected with described silicon tetrachloride entrance.
3. the system of purifying silicon tetrachloride according to claim 2, is characterized in that, further comprises:
The first refrigerating unit, described the first refrigerating unit has steam-in and condensate outlet, and described steam-in is connected with described vapour outlet, and described condensate outlet is connected with described absorption distillation section; And
The second refrigerating unit, described the second refrigerating unit has light constituent entrance and exports through overcooled light constituent, and described light constituent entrance is connected with described condensate outlet.
4. the system of purifying silicon tetrachloride according to claim 1, is characterized in that, further comprises:
The 3rd refrigerating unit, described the 3rd refrigerating unit has the silicon tetrachloride outlet of rectifying silicon tetrachloride entrance and purifying, and described rectifying silicon tetrachloride entrance is connected with described silicon tetrachloride outlet; And
The 4th refrigerating unit, described the 4th refrigerating unit is connected with described heavy constituent outlet with the described heavy constituent outlet of not vaporizing.
5. the system of purifying silicon tetrachloride according to claim 1, is characterized in that, the internals of described absorption distillation section are the structured packing with surface recombination sorbent material, and number of theoretical plate is 10～20.
6. the system of purifying silicon tetrachloride according to claim 1, is characterized in that, the internals of described lights removal section are wire cloth structured packing and plate ripple arranged packing, and number of theoretical plate is 20～40.
7. the system of purifying silicon tetrachloride according to claim 1, is characterized in that, the internals of described heavies removal section are wire cloth structured packing and plate ripple arranged packing, and number of theoretical plate is 5～15.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201420353786.0U CN203959836U (en) | 2014-06-26 | 2014-06-26 | The system of purifying silicon tetrachloride |
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| CN201420353786.0U CN203959836U (en) | 2014-06-26 | 2014-06-26 | The system of purifying silicon tetrachloride |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104058409A (en) * | 2014-06-26 | 2014-09-24 | 中国恩菲工程技术有限公司 | Silicon tetrachloride purification system |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104058409A (en) * | 2014-06-26 | 2014-09-24 | 中国恩菲工程技术有限公司 | Silicon tetrachloride purification system |
| CN104058409B (en) * | 2014-06-26 | 2016-01-27 | 中国恩菲工程技术有限公司 | The system of purifying silicon tetrachloride |
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