CN109289707A - The feeding mechanism and its control system of a kind of germanium tetrachloride hydrolysis device and application - Google Patents

The feeding mechanism and its control system of a kind of germanium tetrachloride hydrolysis device and application Download PDF

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Publication number
CN109289707A
CN109289707A CN201811400268.9A CN201811400268A CN109289707A CN 109289707 A CN109289707 A CN 109289707A CN 201811400268 A CN201811400268 A CN 201811400268A CN 109289707 A CN109289707 A CN 109289707A
Authority
CN
China
Prior art keywords
flow
germanium tetrachloride
feeding mechanism
hydrolysis device
hydrolysis
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
CN201811400268.9A
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Chinese (zh)
Inventor
崔丁方
李恒方
廖吉伟
彭明清
陈知江
陈元欣
李雪寅
匡子登
何斌
蔡文红
陈志朋
罗谦
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Yunnan Chihong International Germanium Industry Co Ltd
Original Assignee
Yunnan Chihong International Germanium Industry Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Yunnan Chihong International Germanium Industry Co Ltd filed Critical Yunnan Chihong International Germanium Industry Co Ltd
Priority to CN201811400268.9A priority Critical patent/CN109289707A/en
Publication of CN109289707A publication Critical patent/CN109289707A/en
Priority to CN201910545074.6A priority patent/CN110090601A/en
Withdrawn legal-status Critical Current

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Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00Feed or outlet devices; Feed or outlet control devices
    • B01J4/008Feed or outlet control devices
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2204/00Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
    • B01J2204/002Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices the feeding side being of particular interest

Abstract

The embodiment of the invention discloses a kind of feeding mechanism of germanium tetrachloride hydrolysis device and its control system and applications, the hydrolysis device includes mixing chamber, hydrolysis room and the hydraulic pump for liquid to be transferred to hydrolysis room by mixing chamber, the feeding mechanism includes the feeder pipe being arranged at the top of mixing chamber and is arranged in feeder pipe for controlling the flow control structure of fluid flow, the flow control structure includes symmetrically arranged two fixture blocks, the flow of the gap adjustment liquid by adjusting two fixture blocks.Feeding mechanism provided in an embodiment of the present invention can liquid with precise control flow, to solve the problems, such as that germanium dioxide granularity is uneven in the prior art, density is small, apparent density differs greatly.The application also proposed a kind of for controlling the control system of charging rate, can automatically control the charging rate of germanium tetrachloride.

Description

The feeding mechanism and its control system of a kind of germanium tetrachloride hydrolysis device and application
Technical field
The present embodiments relate to chemical production technical fields, and in particular to a kind of charger of germanium tetrachloride hydrolysis device Structure and its control system and application.
Background technique
In GeO2Preparation process in, need GeCl4It is sent into hydrolysis device and reaction is hydrolyzed.Period, hydrolytic process Middle addition GeCl4Feeding mechanism cannot accurately control charging rate, influence hydrolysis reaction process.If GeCl4Be added it is too fast, Since hydrolytic process has little time fully reacting, foring includes GeCl4The hard GeO of drop2Shell bulky grain, makes GeCl4 Reduce with the contact area of water, has slowed down the progress of reaction.This shell is not easy by GeCl4Be impregnated with, with hydrolytic process into Row, shell is to GeCl4Drop internal extension, outer casing thickness further increase.The GeO generated in this way2Specific gravity is larger, almost GeCl4Twice of specific gravity.
To sum up, the prior art utilizes GeCl4Hydrolysis production GeO2During, add since feeding mechanism cannot be controlled accurately Expect speed, the germanium dioxide granularity of production is uneven, density is small, apparent density differs greatly, and affects product quality.
Summary of the invention
For this purpose, the embodiment of the present invention provide a kind of germanium tetrachloride hydrolysis device feeding mechanism and its control system with answer With cannot accurately control charging rate to solve feeding mechanism in the prior art, the germanium dioxide granularity of production is uneven, density The problem of small, apparent density differs greatly, influences product quality.
To achieve the goals above, embodiments of the present invention provide the following technical solutions:
In the first aspect of embodiments of the present invention, a kind of feeding mechanism of germanium tetrachloride hydrolysis device is provided, The hydrolysis device includes mixing chamber, hydrolyzes room and the hydraulic pump for liquid to be transferred to hydrolysis room by mixing chamber, described Feeding mechanism includes the feeder pipe being arranged at the top of mixing chamber and is arranged in feeder pipe for controlling the flow of fluid flow Control structure, the flow control structure include symmetrically arranged two fixture blocks, by the gap adjustment liquid for adjusting two fixture blocks Flow.
In one embodiment of the invention, the fixture block is semiellipsoid, the arcwall face and feeder pipe of semiellipsoid Tube wall be fixedly connected.
In one embodiment of the invention, the hydrolysis device is equipped with the control system for controlling two fixture block gaps System.
In one embodiment of the invention, the control system includes:
Flow sensor, for measuring the fluid flow between two fixture blocks,
PLC logic supervisory controller, by flow and the preset value of flow sensor measurement just compared with, and issue instruction, And
Flow control valve receives the instruction that PLC logic supervisory controller issues, when the flow of flow sensor measurement is greater than When preset value, flow control valve reduces the gap between two fixture blocks, when the flow of flow sensor measurement is less than preset value, Flow control valve expands the gap between two fixture blocks.
In one embodiment of the invention, the flow control valve is set in the outside of feeder pipe, and flow control valve It is corresponding with the position of two fixture blocks.
In the second aspect of embodiments of the present invention, a kind of GeO is provided2Preparation method, including by four chlorinations Germanium rectifying liquid, which is sent into hydrolyze in germanium tetrachloride hydrolysis device, is made GeO2Any one of, be equipped on the germanium tetrachloride hydrolysis device The feeding mechanism.
In one embodiment of the invention, the hydrolysis time of germanium tetrachloride rectifying liquid is 300min.
In one embodiment of the invention, when germanium tetrachloride rectifying liquid is sent into germanium tetrachloride hydrolysis device by feeding mechanism Fluid flow be 1L/h.
Embodiment according to the present invention has the advantages that the embodiment of the present invention provides a kind of germanium tetrachloride hydrolysis dress The feeding mechanism and its control system set and application, the feeding mechanism, should by the way that flow control structure is arranged in feeder pipe Flow control structure includes symmetrically arranged two fixture blocks, the flow of the gap adjustment liquid by adjusting two fixture blocks, so that The feeding mechanism of the application can liquid with precise control flow, thus solve in the prior art germanium dioxide granularity it is uneven, close Spend the problem of small, apparent density differs greatly.The application also proposed it is a kind of for controlling the control system of charging rate, can Automatically control the charging rate of germanium tetrachloride.In addition, the application also proposed a kind of GeO2Preparation method, by using this Shen Please method preparation GeO2Epigranular, density are big, apparent density difference is small, efficiently solve the deficiencies in the prior art.
Detailed description of the invention
It, below will be to embodiment party in order to illustrate more clearly of embodiments of the present invention or technical solution in the prior art Formula or attached drawing needed to be used in the description of the prior art are briefly described.It should be evident that the accompanying drawings in the following description is only It is merely exemplary, it for those of ordinary skill in the art, without creative efforts, can also basis The attached drawing of offer, which is extended, obtains other implementation attached drawings.
Structure depicted in this specification, ratio, size etc., only to cooperate the revealed content of specification, for Those skilled in the art understands and reads, and is not intended to limit the invention enforceable qualifications, therefore does not have technical Essential meaning, the modification of any structure, the change of proportionate relationship or the adjustment of size are not influencing the function of the invention that can be generated Under effect and the purpose that can reach, should all still it fall in the range of disclosed technology contents obtain and can cover.
Fig. 1 is a kind of structural representation of the feeding mechanism for germanium tetrachloride hydrolysis device that one embodiment of the invention provides Figure.
Description of symbols: 1- mixing chamber;2- hydrolyzes room;3- hydraulic pump;4- feeder pipe;5- fixture block.
Specific embodiment
Embodiments of the present invention are illustrated by particular specific embodiment below, those skilled in the art can be by this explanation Content disclosed by book is understood other advantages and efficacy of the present invention easily, it is clear that described embodiment is the present invention one Section Example, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not doing Every other embodiment obtained under the premise of creative work out, shall fall within the protection scope of the present invention.
Embodiment 1
As shown in Figure 1;The present embodiment provides a kind of feeding mechanism of germanium tetrachloride hydrolysis device, the hydrolysis device includes Mixing chamber 1, hydrolysis room 2 and the hydraulic pump 3 for liquid to be transferred to hydrolysis room 2 by mixing chamber 1, the feeding mechanism packet It includes the feeder pipe 4 that 1 top of mixing chamber is set and is arranged in feeder pipe 4 for controlling the flow control knot of fluid flow Structure, the flow control structure include symmetrically arranged two fixture blocks 5, and the gap size by adjusting two fixture blocks 5 adjusts liquid Uninterrupted.
Further, the fixture block 5 is semiellipsoid, the arcwall face of semiellipsoid and the fixed company of the tube wall of feeder pipe 4 It connects.
The feeding mechanism for the germanium tetrachloride hydrolysis device that the present embodiment proposes, the feeding mechanism in feeder pipe 4 by setting Flow control structure is set, which includes symmetrically arranged two fixture blocks 5, by the gap for adjusting two fixture blocks 5 The flow for adjusting liquid, enables the feeding mechanism liquid with precise control flow of the application, to solve in the prior art two The problem of germanium oxide granularity is uneven, density is small, apparent density differs greatly.
Embodiment 2
In the case where taking 1 technical solution of embodiment, the application is arranged for controlling two cards also on hydrolysis device The control system in 5 gap of block, the control system include:
Flow sensor, for measuring the fluid flow between two fixture blocks 5,
PLC logic supervisory controller, by flow and the preset value of flow sensor measurement just compared with, and issue instruction, And
Flow control valve receives the instruction that PLC logic supervisory controller issues, when the flow of flow sensor measurement is greater than When preset value, flow control valve reduces the gap between two fixture blocks 5, when the flow of flow sensor measurement is less than preset value When, flow control valve expands the gap between two fixture blocks 5.
Further, the flow control valve is set in the outside of feeder pipe 4, and flow control valve and two fixture blocks 5 Position is corresponding.
The control system that the present embodiment proposes includes flow sensor, PLC logic supervisory controller and flow control valve, energy The charging rate for enough automatically controlling germanium tetrachloride, effectively avoids the problem that fluid flow is excessive or too small in feeding mechanism.
Embodiment 3
In the case where taking 2 technical solution of embodiment 1 or embodiment, the present embodiment additionally provides a kind of GeO2Preparation Method, including germanium tetrachloride rectifying liquid is sent into hydrolyze in germanium tetrachloride hydrolysis device, GeO is made2, the germanium tetrachloride hydrolysis Embodiment 1 or feeding mechanism as described in example 2 are installed on device.
Further, the hydrolysis time of germanium tetrachloride rectifying liquid is 300min.
Further, germanium tetrachloride rectifying liquid by feeding mechanism be sent into germanium tetrachloride hydrolysis device when fluid flow be 1L/h。
The GeO that the present embodiment proposes2Preparation method, by using the application method prepare GeO2Epigranular, density Greatly, apparent density difference is small, efficiently solves the deficiencies in the prior art.
Although above having used general explanation and specific embodiment, the present invention is described in detail, at this On the basis of invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Therefore, These modifications or improvements without departing from theon the basis of the spirit of the present invention are fallen within the scope of the claimed invention.

Claims (8)

1. a kind of feeding mechanism of germanium tetrachloride hydrolysis device, the hydrolysis device includes mixing chamber, hydrolysis room and is used to incite somebody to action Liquid is transferred to the hydraulic pump of hydrolysis room by mixing chamber, it is characterised in that: the feeding mechanism includes being arranged at the top of mixing chamber Feeder pipe and be arranged in feeder pipe for controlling the flow control structure of fluid flow, which includes Symmetrically arranged two fixture blocks, the flow of the gap adjustment liquid by adjusting two fixture blocks.
2. the feeding mechanism of germanium tetrachloride hydrolysis device according to claim 1, it is characterised in that: the fixture block is half ellipse Sphere, the arcwall face of semiellipsoid are fixedly connected with the tube wall of feeder pipe.
3. the feeding mechanism of germanium tetrachloride hydrolysis device according to claim 1, it is characterised in that: set on the hydrolysis device There is the control system for controlling two fixture block gaps.
4. the feeding mechanism of germanium tetrachloride hydrolysis device according to claim 3, which is characterized in that the control system packet It includes:
Flow sensor, for measuring the fluid flow between two fixture blocks,
PLC logic supervisory controller, by flow and the preset value of flow sensor measurement just compared with, and issue instruction, and
Flow control valve receives the instruction that PLC logic supervisory controller issues, and presets when the flow of flow sensor measurement is greater than When value, flow control valve reduces the gap between two fixture blocks, when the flow of flow sensor measurement is less than preset value, flow Control valve expands the gap between two fixture blocks.
5. the feeding mechanism of germanium tetrachloride hydrolysis device according to claim 4, it is characterised in that: the flow control valve pocket It is located at the outside of feeder pipe, and flow control valve is corresponding with the position of two fixture blocks.
6. a kind of GeO2Preparation method, including by germanium tetrachloride rectifying liquid be sent into germanium tetrachloride hydrolysis device in hydrolysis be made GeO2, it is characterised in that: charger described in any one of claim 1-5 is installed on the germanium tetrachloride hydrolysis device Structure.
7. GeO according to claim 62Preparation method, it is characterised in that: the hydrolysis time of germanium tetrachloride rectifying liquid is 300min。
8. GeO according to claim 62Preparation method, it is characterised in that: germanium tetrachloride rectifying liquid is sent by feeding mechanism Fluid flow when germanium tetrachloride hydrolysis device is 1L/h.
CN201811400268.9A 2018-11-22 2018-11-22 The feeding mechanism and its control system of a kind of germanium tetrachloride hydrolysis device and application Withdrawn CN109289707A (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
CN201811400268.9A CN109289707A (en) 2018-11-22 2018-11-22 The feeding mechanism and its control system of a kind of germanium tetrachloride hydrolysis device and application
CN201910545074.6A CN110090601A (en) 2018-11-22 2019-06-21 The feeding mechanism and its control system of a kind of germanium tetrachloride hydrolysis device and application

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Application Number Priority Date Filing Date Title
CN201811400268.9A CN109289707A (en) 2018-11-22 2018-11-22 The feeding mechanism and its control system of a kind of germanium tetrachloride hydrolysis device and application

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CN201910545074.6A Pending CN110090601A (en) 2018-11-22 2019-06-21 The feeding mechanism and its control system of a kind of germanium tetrachloride hydrolysis device and application

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CN100513602C (en) * 2006-11-15 2009-07-15 云南临沧鑫圆锗业股份有限公司 Reclamation of germanium from germanium waste material by wet method
JP2009031866A (en) * 2007-07-24 2009-02-12 Yamatake Corp Flow control valve and flow control method
EP2706425B1 (en) * 2008-06-26 2020-09-23 Belparts Flow control system
CN202876800U (en) * 2012-08-03 2013-04-17 云南驰宏锌锗股份有限公司 Fully-closed germanium tetrachloride hydrolyzing device
CN102774877B (en) * 2012-08-03 2014-05-14 云南驰宏锌锗股份有限公司 Novel process for preparing germanium dioxide (GeO2)
CN202880921U (en) * 2012-08-03 2013-04-17 云南驰宏锌锗股份有限公司 Germanium tetrachloride hydrolysate separating device
CN103993179A (en) * 2014-05-27 2014-08-20 扬州宁达贵金属有限公司 Method for recovering germanium from germanium-silicon alloy
CN106475014A (en) * 2015-11-25 2017-03-08 衡阳恒荣高纯半导体材料有限公司 A kind of germanium tetrachloride hydrolysis device
CN106564933A (en) * 2016-11-22 2017-04-19 云南临沧鑫圆锗业股份有限公司 Preparation method of low-chloride high-purity germanium dioxide

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