CN109626380A - A kind of optical fiber grade silicon tetrachloride production reaction tower - Google Patents

A kind of optical fiber grade silicon tetrachloride production reaction tower Download PDF

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Publication number
CN109626380A
CN109626380A CN201811532449.7A CN201811532449A CN109626380A CN 109626380 A CN109626380 A CN 109626380A CN 201811532449 A CN201811532449 A CN 201811532449A CN 109626380 A CN109626380 A CN 109626380A
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CN
China
Prior art keywords
purification case
tower body
heater
optical fiber
feed pipe
Prior art date
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Pending
Application number
CN201811532449.7A
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Chinese (zh)
Inventor
陈道伟
郑云峰
黄远青
李开海
吴惠
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ZHEJIANG KAIHUA SYNTHETIC MATERIALS CO Ltd
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ZHEJIANG KAIHUA SYNTHETIC MATERIALS CO Ltd
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Priority to CN201811532449.7A priority Critical patent/CN109626380A/en
Publication of CN109626380A publication Critical patent/CN109626380A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/08Compounds containing halogen
    • C01B33/107Halogenated silanes
    • C01B33/1071Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/08Compounds containing halogen
    • C01B33/107Halogenated silanes
    • C01B33/10778Purification

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Silicon Compounds (AREA)

Abstract

The invention discloses a kind of optical fiber grade silicon tetrachlorides to produce reaction tower, including tower body, purify case, heating inner liner, heater, pre-heater, cooling cylinder and condenser, lower section inside the tower body is equipped with purification case, heating inner liner is installed inside the tank wall of the purification case, heating wire is installed in the heating inner liner, the heater installed on the heating wire and tower body outer right wall is electrically connected, top on the right side of the purification case is equipped with the first feed pipe, top on the left of the purification case is equipped with the second feed pipe, pre-heater is installed on second feed pipe, it purifies in the tower body of upper box part and cooling cylinder is installed.The present invention provides a kind of optical fiber grade silicon tetrachlorides to produce reaction tower, pass through the tower body of setting, purification case, heating inner liner, heater, pre-heater, cooling cylinder and condenser, it solves distillation and needs longer heating time, lead to that speed of production is slow, low efficiency, it is purified using the purifying technique of individual event, the problem of refining effect difference.

Description

A kind of optical fiber grade silicon tetrachloride production reaction tower
Technical field
The present invention relates to the development field of optical fiber grade silicon tetrachloride production technology, specially a kind of four chlorination of optical fiber grade Silicon produces reaction tower.
Background technique
Fiber optic communication is a kind of novel laser communication system to grow up nineteen seventies, is the world today The communication technology of upper most advanced, optimal future, fiber optic communication, which has, transmits big, good communication quality, long service life, confidentiality height The advantages that, with the development of society, fiber optic communication has become the prevailing transmission medium of present communications technology, the market of optical fiber is needed The amount of asking is continuously increased, and just gradually replaces cable communication.Therefore fiber optic materials have the development of national communication technology very heavy The meaning wanted.Silicon tetrachloride is primary raw material required for production optical fiber cable prefabricated rods, accounts for the 85%- of fiber composition content 95%, the purity of high purity silicon tetrachloride product directly affects the loss characteristic of optical fiber.Optical fiber grade silicon tetrachloride is generally by technical grade Silicon tetrachloride purification is made, up to tens kinds of various components that may be present in current industrial grade silicon tetrachloride, optical fiber grade four Requirement of the silicon chloride to impurity content is very high, more tightened up than semiconductor material to a certain extent, current country 80%-90% Silicon tetrachloride for optical fiber rely on import, there is a large amount of silicon tetrachloride byproduct to need to locate in the silicon industry in China at the same time Reason, therefore there is highly important application value to the research of optical fiber grade silicon tetrachloride purification technique.
But existing optical fiber grade silicon tetrachloride production reaction tower has the following deficiencies:
1. distillation needs longer heating time, lead to that speed of production is slow, low efficiency;
2. the purifying technique using individual event purifies, refining effect is poor.
Summary of the invention
(1) the technical issues of solving
In view of the deficiencies of the prior art, the present invention provides a kind of optical fiber grade silicon tetrachlorides to produce reaction tower, solves steaming It evaporates and needs longer heating time, lead to that speed of production is slow, low efficiency, purified using the purifying technique of individual event, refining effect is poor The problem of.
(2) technical solution
To achieve the above object, the invention provides the following technical scheme: a kind of optical fiber grade silicon tetrachloride produces reaction tower, packet Include tower body, purification case, heating inner liner, heater, pre-heater, cooling cylinder and condenser, the lower section installation inside the tower body There is purification case, heating inner liner is installed inside the tank wall of the purification case, heating wire, the electricity are installed in the heating inner liner The heater installed on heated filament and tower body outer right wall is electrically connected, and the top on the right side of the purification case is equipped with the first charging Pipe, the top purified on the left of case is equipped with the second feed pipe, is equipped with pre-heater on second feed pipe, described to mention Cooling cylinder is installed in the tower body of pure upper box part, condenser is installed in the cooling cylinder, is equipped with second on the condenser Discharge nozzle, the tank wall that second discharge nozzle passes through cooling cylinder extend to the outside of tower body.
Preferably, the lower part of the tower body is equipped with pedestal, and the lower part of the pedestal is equipped with bracket, the bracket about The symmetry axis of pedestal is symmetrical.
Preferably, the heating wire is distributed in the side wall and bottom of heating inner liner, and the heating wire is distributed at equal intervals In heating inner liner, two ends of the heating wire each extend to the outside of tower body and the binding post of heater is electrically connected.
Preferably, the middle position of the purification upper box part outer wall is equipped with servo motor, and the servo motor passes through Motor cabinet is fixedly connected with purification case, and the lower part of the servo motor is equipped with shaft, and the shaft extends to the interior of purification case Portion is fixedly connected with stirring rod.
Preferably, the stirring rod is distributed at equal intervals in shaft, and the middle position of the stirring rod passes through fixation Seat is fixedly connected with shaft, and the length of the stirring rod is less than the internal diameter of heating inner liner.
Preferably, the first feed pipe on the purification case extends to the outside of tower body, and is equipped on the first feed pipe First flow control valve, second feed pipe purified on case extends to the outside of tower body, and is equipped on the second feed pipe Second flow control valve.
Preferably, the middle position of the purification lower box part is equipped with the first discharge nozzle, pacifies on first discharge nozzle Equipped with the first solenoid valve, the top of the purification case is equipped with appendix, is equipped with second solenoid valve on the appendix.
Preferably, the upper end of the appendix extends to being internally mounted on the feed inlet of condenser of cooling cylinder, described The tank wall that the lower end of appendix passes through purification case extends to the inside of purification case.
(3) beneficial effect
The present invention provides a kind of optical fiber grade silicon tetrachloride produce reaction tower, have it is following the utility model has the advantages that
(1) of the invention, by the pre-heater of setting, when processing, second flow control valve is opened directly by raw material from the Two feed pipes are transported in purification case, and raw material while conveying in pre-heater operation the second feed pipe of heating is feeding The raw material of preparation is made to be heated to certain temperature in the process, convenient for the temperature that distillation needs can be heated rapidly to when later period distillation, The time for shortening distillation heating, the speed of distillation is accelerated, the speed of distillation is improved, to improve silicon tetrachloride production Efficiency, of simple structure and strong practicability solves distillation and needs longer heating time convenient for promoting the use of, and leads to production speed The problem of degree is slow, low efficiency.
(2) of the invention, pass through the first conveying pipeline of setting, first flow control valve, servo motor and stirring rod, charging knot Beam closes pre-heater and second flow control valve, opens first flow control valve from the first feed pipe and heats four into purification case Silicon chloride purifies hydrolysising solvent, while servo motor operation drives shaft rotation, and shaft drives stirring rod rotation stirring purification case In mixed solvent, be sufficiently mixed solvent, accelerate hydrolysis purified reaction, first its raw material is hydrolyzed before distilation and is mentioned It is pure, the degree of purification is promoted, the quality of silicon tetrachloride production is improved, two purification process are used in mixed way, and purification efficiency is high, product Quality is high, solves the purifying technique purification using individual event, the problem of refining effect difference.
Detailed description of the invention
Fig. 1 is schematic structural view of the invention;
Fig. 2 is external elevational schematic diagram of the present invention;
Fig. 3 is the structural schematic diagram that case is purified in Fig. 1 of the present invention;
Fig. 4 is the vertical view distribution schematic diagram of heating wire in Fig. 1 of the present invention.
In figure: 1, tower body;2, pedestal;3, bracket;4, case is purified;5, heating inner liner;6, heating wire;7, heater;8, One discharge nozzle;9, the first solenoid valve;10, the first feed pipe;11, first flow control valve;12, the second feed pipe;13, it preheats Device;14, second flow control valve;15, servo motor;16, shaft;17, stirring rod;18, cooling cylinder;19, appendix;20, Two solenoid valves;21, condenser;22, the second discharge nozzle;23, motor cabinet;24, fixing seat.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other Embodiment shall fall within the protection scope of the present invention.
It please refers to shown in Fig. 1-4, a kind of embodiment provided by the invention;A kind of optical fiber grade silicon tetrachloride production reaction tower, Including tower body 1, purification case 4, heating inner liner 5, heater 7, pre-heater 13, cooling cylinder 18 and condenser 21, inside tower body 1 Lower section is equipped with purification case 4, purifies and is equipped with heating inner liner 5 inside the tank wall of case 4, heating wire 6 is equipped in heating inner liner 5, The heater 7 installed on heating wire 6 and 1 outer right wall of tower body is electrically connected, the model JOC-JW-JOD of heater 7, electric heating Silk 6 is distributed in the side wall and bottom of heating inner liner 5, and heating wire 6 is distributed at equal intervals in heating inner liner 5, and the two of heating wire 6 A end each extends to the outside of tower body 1 and the binding post of heater 7 is electrically connected, and the top on purification case 4 right side is equipped with the One feed pipe 10, the first feed pipe 10 are connected on extraneous silicon tetrachloride purification hydrolysis solvent delivery device, 4 left side of purification case Top the second feed pipe 12 is installed, purify the outside that the first feed pipe 10 on case 4 extends to tower body 1, and the first charging First flow control valve 11 is installed, the model LDG-MK-C of first flow control valve 11 purifies second on case 4 on pipe 10 Feed pipe 12 extends to the outside of tower body 1, and second flow control valve 14 is equipped on the second feed pipe 12, second flow control The model LDG-MK-C of valve 14 is equipped with pre-heater 13, the model XY- of pre-heater 13 on second feed pipe 12 The middle position of YTJRQ, purification 4 external wall of upper portion of case are equipped with servo motor 15, and the model HF-SP of servo motor 15 is watched It takes motor 15 and is fixedly connected by motor cabinet 23 with purification case 4, the lower part of servo motor 15 is equipped with shaft 16, and shaft 16 extends It is fixedly connected to the inside of purification case 4 with stirring rod 17, stirring rod 17 is distributed at equal intervals in shaft 16, in stirring rod 17 Between be fixedly connected by fixing seat 24 with shaft 16 at position, the length of stirring rod 17 is less than the internal diameter of heating inner liner 5, purification case Cooling cylinder 18 is installed in the tower body 1 on 4 tops, condenser 21 is installed in cooling cylinder 18, purifies the middle position of 4 lower part of case First discharge nozzle 8 is installed, the first solenoid valve 9, the model ZCD of the first solenoid valve 9, purification are installed on the first discharge nozzle 8 The top of case 4 is equipped with appendix 19, is equipped with second solenoid valve 20 on appendix 19, the model ZCD of second solenoid valve 20, The upper end of appendix 19 extends to being internally mounted on the feed inlet of condenser 21 of cooling cylinder 18, the model L- of condenser 21 606, the tank wall that the lower end of appendix 19 passes through purification case 4 extends to the inside of purification case 4, is equipped with second on condenser 21 and goes out Expects pipe 22, the tank wall that the second discharge nozzle 22 passes through cooling cylinder 18 extend to the outside of tower body 1, and the lower part of tower body 1 is equipped with pedestal 2, the lower part of pedestal 2 is equipped with bracket 3, and bracket 3 is symmetrical about the symmetry axis of pedestal 2.
Working principle: when processing, raw material is directly transported to by opening second flow control valve 14 from the second feed pipe 12 to be mentioned In pure case 4, the raw material in the second feed pipe 12 is heated in the operation of pre-heater 13 while conveying, and charging terminates to close preheating Device 13 and second flow control valve 14 open first flow control valve 11 from the first feed pipe 10 and heat tetrachloro into purification case 4 SiClx purifies hydrolysising solvent, while the operation of servo motor 15 drives shaft 16 to rotate, and shaft 16 drives the rotation stirring of stirring rod 17 The mixed solvent in case 4 is purified, solvent is sufficiently mixed, accelerates hydrolysis purified reaction, silicon tetrachloride purification hydrolysis solvent delivery knot First flow control valve 11 is closed after beam, heater 7 runs the mixed solvent in the fever heating purification case 4 of heating wire 6, and to it Purification distillation is carried out, the gaseous silicon that the distillation of second solenoid valve 20 generates is opened at this time and is transported to cooling cylinder from appendix 19 In condenser 21 in 18, condenser 21 runs the silicon tetrachloride for being translated into liquid, and is transported to from the second discharge nozzle 22 The external world carries out down one of manufacturing procedure, after distillation, opens the first solenoid valve 9 and processing-waste is discharged from the first discharge nozzle 8 Purify case 4.
Can to sum up obtain, the present invention by setting tower body 1, purification case 4, heating inner liner 5, heater 7, pre-heater 13, Cooling cylinder 18 and condenser 21 solve distillation and need longer heating time, lead to that speed of production is slow, low efficiency, using list The purifying technique purification of item, the problem of refining effect difference.
It should be noted that, in this document, relational terms such as first and second and the like are used merely to a reality Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation In any actual relationship or order or sequence.Moreover, the terms "include", "comprise" or its any other variant are intended to Non-exclusive inclusion, so that the process, method, article or equipment including a series of elements is not only wanted including those Element, but also including other elements that are not explicitly listed, or further include for this process, method, article or equipment Intrinsic element.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding And modification, the scope of the present invention is defined by the appended.

Claims (8)

1. a kind of optical fiber grade silicon tetrachloride produces reaction tower, including tower body (1), purification case (4), heating inner liner (5), heater (7), pre-heater (13), cooling cylinder (18) and condenser (21), it is characterised in that: the internal lower section installation of the tower body (1) Have purification case (4), is equipped with heating inner liner (5) inside the tank wall of purification case (4), is equipped in the heating inner liner (5) The heater (7) installed in heating wire (6), the heating wire (6) and tower body (1) outer right wall is electrically connected, the purification case (4) top on the right side of is equipped with the first feed pipe (10), and the top on the left of purification case (4) is equipped with the second feed pipe (12), it is equipped with pre-heater (13) on second feed pipe (12), installation in the tower body (1) on described purification case (4) top Have cooling cylinder (18), be equipped with condenser (21) in the cooling cylinder (18), the second discharging is installed on the condenser (21) It manages (22), the tank wall that second discharge nozzle (22) passes through cooling cylinder (18) extends to the outside of tower body (1).
2. a kind of optical fiber grade silicon tetrachloride according to claim 1 produces reaction tower, it is characterised in that: the tower body (1) Lower part be equipped with pedestal (2), the lower part of the pedestal (2) is equipped with bracket (3), pair of the bracket (3) about pedestal (2) Claim axial symmetry distribution.
3. a kind of optical fiber grade silicon tetrachloride according to claim 1 produces reaction tower, it is characterised in that: the heating wire (6) it being distributed in the side wall and bottom of heating inner liner (5), the heating wire (6) is distributed at equal intervals in heating inner liner (5), The binding post of outside and heater (7) that two ends of the heating wire (6) each extend to tower body (1) is electrically connected.
4. a kind of optical fiber grade silicon tetrachloride according to claim 1 produces reaction tower, it is characterised in that: the purification case (4) middle position of external wall of upper portion is equipped with servo motor (15), and the servo motor (15) passes through motor cabinet (23) and mentions Pure case (4) is fixedly connected, and the lower part of the servo motor (15) is equipped with shaft (16), and the shaft (16) extends to purification case (4) inside is fixedly connected with stirring rod (17).
5. a kind of optical fiber grade silicon tetrachloride according to claim 4 produces reaction tower, it is characterised in that: the stirring rod (17) it is distributed at equal intervals on shaft (16), the middle position of the stirring rod (17) passes through fixing seat (24) and shaft (16) it is fixedly connected, the length of the stirring rod (17) is less than the internal diameter of heating inner liner (5).
6. a kind of optical fiber grade silicon tetrachloride according to claim 1 produces reaction tower, it is characterised in that: the purification case (4) the first feed pipe (10) on extends to the outside of tower body (1), and is equipped with first flow control on the first feed pipe (10) Valve (11), second feed pipe (12) purified on case (4) extend to the outside of tower body (1), and on the second feed pipe (12) Second flow control valve (14) are installed.
7. a kind of optical fiber grade silicon tetrachloride according to claim 1 produces reaction tower, it is characterised in that: the purification case (4) middle position of lower part is equipped with the first discharge nozzle (8), is equipped with the first solenoid valve on first discharge nozzle (8) (9), the top of purification case (4) is equipped with appendix (19), is equipped with second solenoid valve (20) on the appendix (19).
8. a kind of optical fiber grade silicon tetrachloride according to claim 7 produces reaction tower, it is characterised in that: the appendix (19) upper end extends to being internally mounted on the feed inlet of condenser (21) of cooling cylinder (18), under the appendix (19) The tank wall across purification case (4) is held to extend to the inside of purification case (4).
CN201811532449.7A 2018-12-14 2018-12-14 A kind of optical fiber grade silicon tetrachloride production reaction tower Pending CN109626380A (en)

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CN201811532449.7A CN109626380A (en) 2018-12-14 2018-12-14 A kind of optical fiber grade silicon tetrachloride production reaction tower

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2820698A (en) * 1954-06-25 1958-01-21 Du Pont Process for purifying silicon halide
CN102219222A (en) * 2011-04-22 2011-10-19 武汉新硅科技有限公司 Continuous rectification method for high-purity silicon tetrachloride for optical fiber
CN105502409A (en) * 2015-12-04 2016-04-20 天津大学 Method and device for purifying silicon tetrachloride of optical fiber grade through total reflux distillation
CN207996445U (en) * 2018-01-23 2018-10-23 宜兴市永加化工有限公司 A kind of Chemical Manufacture distilling apparatus

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2820698A (en) * 1954-06-25 1958-01-21 Du Pont Process for purifying silicon halide
CN102219222A (en) * 2011-04-22 2011-10-19 武汉新硅科技有限公司 Continuous rectification method for high-purity silicon tetrachloride for optical fiber
CN105502409A (en) * 2015-12-04 2016-04-20 天津大学 Method and device for purifying silicon tetrachloride of optical fiber grade through total reflux distillation
CN207996445U (en) * 2018-01-23 2018-10-23 宜兴市永加化工有限公司 A kind of Chemical Manufacture distilling apparatus

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
刘洪范: "《化学实验基础》", 31 December 1981, 山东科学技术出版社 *
宋如等: "《化工原理》", 30 September 2017, 电子科技大学出版社 *

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Application publication date: 20190416