CN202876800U - Fully-closed germanium tetrachloride hydrolyzing device - Google Patents

Fully-closed germanium tetrachloride hydrolyzing device Download PDF

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Publication number
CN202876800U
CN202876800U CN 201220384044 CN201220384044U CN202876800U CN 202876800 U CN202876800 U CN 202876800U CN 201220384044 CN201220384044 CN 201220384044 CN 201220384044 U CN201220384044 U CN 201220384044U CN 202876800 U CN202876800 U CN 202876800U
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hydrolysis
germanium tetrachloride
enclosed
totally
utility
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CN 201220384044
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Chinese (zh)
Inventor
孙成余
王少龙
李贤辉
彭明清
何斌
杨金彩
蔡文红
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Yunnan Chihong International Germanium Industry Co ltd
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Yunnan Chihong Zinc and Germanium Co Ltd
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Abstract

The utility model provides a fully-closed germanium tetrachloride hydrolyzing device. According to the scheme of the embodiment of the utility model, the hydrolyzing device comprises a kettle body, an upper cover, a first feeding opening, a second feeding opening, an air exhausting opening and a material discharging opening, wherein a hydrolyzing reaction space is limited in the kettle body; the upper cover is arranged at the top of the kettle body; the first feeding opening is formed in the upper cover and is used for supplying germanium tetrachloride refined liquid to the hydrolyzing reaction space; the second feeding opening is formed in the upper cover and is used for supplying ultrapure water to the hydrolyzing reaction space; the air exhausting opening is formed in the upper cover and is used for discharging hydrogen chloride gas generated from hydrolyzing reaction from the hydrolyzing reaction space; and the material discharging opening is formed in the bottom of the kettle body and is used for discharging hydrolyzed products. With the adoption of the fully-closed germanium tetrachloride hydrolyzing device, the germanium tetrachloride hydrolyzing reaction can be carried out under a closed condition.

Description

Germanium tetrachloride totally-enclosed hydrolysis device
Technical field
The utility model relates to field of metallurgy, and more specifically, the utility model relates to germanium tetrachloride totally-enclosed hydrolysis device.
Background technology
In the germanium extractive technique, take germanium concentrate as raw material, obtain high-purity GeO through chlorinated distillation, multiple steaming, rectifying, hydrolysis, filtration, oven dry, calcining 2Product.Wherein with the reaction that is hydrolyzed of germanium tetrachloride rectifying liquid and ultra-pure water, obtain the mixture of germanium dioxide and hydrogen chloride, for obtaining purity, GeO that particle diameter is qualified 2Product, necessary strict controlled hydrolysis reaction temperature, unlikely too high or too low for temperature so that GeO 2Grain diameter is inhomogeneous, and must realize separating the mixture of germanium dioxide and hydrogen chloride through filtration means.
Yet the means of at present germanium tetrachloride hydrolysis preparation germanium dioxide still remain to be improved.
The utility model content
The utility model one of is intended to solve the problems of the technologies described above at least to a certain extent or provides at least a kind of useful commerce to select.For this reason, a purpose of the present utility model is to propose a kind of device that can be effective to carry out the germanium tetrachloride hydrolysis.
Aspect one of the present utility model, the utility model proposes a kind of germanium tetrachloride totally-enclosed hydrolysis device.According to embodiment of the present utility model, this hydrolysis device comprises: kettle is limited with the hydrolysis space in the described kettle; Loam cake, described loam cake is arranged on the top of described kettle; The first charging aperture, described the first charging aperture are arranged on and cover on described, are used for supplying with to described hydrolysis space germanium tetrachloride rectifying liquid; The second charging aperture, described the second charging aperture are arranged on and cover on described, are used for supplying with ultra-pure water to described hydrolysis space; Exhaust outlet, described exhaust outlet are arranged on and cover on described, are used for the hydrogen chloride gas of hydrolysis reaction volatilization is discharged from described hydrolysis space; And discharge gate, described discharge gate is arranged on the bottom of described kettle, is used for the discharge water hydrolysis products.Utilize this germanium tetrachloride totally-enclosed hydrolysis device, can carry out in confined conditions the germanium tetrachloride hydrolysis.
According to embodiment of the present utility model, above-mentioned germanium tetrachloride totally-enclosed hydrolysis device can also have following additional technical feature:
Germanium tetrachloride totally-enclosed hydrolysis device of the present utility model may further include agitating device, and described agitating device is arranged in the described hydrolysis space, is used for stirring the reactant in described hydrolysis space.Thus, further raising utilizes germanium tetrachloride totally-enclosed hydrolysis device to carry out the efficient of germanium tetrachloride hydrolysis.
Germanium tetrachloride totally-enclosed hydrolysis device of the present utility model may further include motor, and described motor is arranged on and covers on described, and links to each other with described agitating device, is used for controlling described agitating device.Thus, further raising utilizes germanium tetrachloride totally-enclosed hydrolysis device to carry out the efficient of germanium tetrachloride hydrolysis.
Germanium tetrachloride totally-enclosed hydrolysis device of the present utility model may further include the reaction observation panel, and described reaction observation panel is arranged on and covers on described.Thus, further raising utilizes germanium tetrachloride totally-enclosed hydrolysis device to carry out the efficient of germanium tetrachloride hydrolysis.
Germanium tetrachloride totally-enclosed hydrolysis device of the present utility model may further include attemperating unit, and described attemperating unit is arranged on the outside of described kettle.Thus, further raising utilizes germanium tetrachloride totally-enclosed hydrolysis device to carry out the efficient of germanium tetrachloride hydrolysis.
In the germanium tetrachloride totally-enclosed hydrolysis device of the present utility model, described attemperating unit is circulating frozen brine-cooled device.Thus, further raising utilizes germanium tetrachloride totally-enclosed hydrolysis device to carry out the efficient of germanium tetrachloride hydrolysis.
Germanium tetrachloride totally-enclosed hydrolysis device of the present utility model may further include four supports, and described support links to each other with described kettle, is used for supporting kettle.
In the germanium tetrachloride totally-enclosed hydrolysis device of the present utility model, described exhaust outlet links to each other with the alkali liquor absorption device.Thus, reclaim the hydrogen chloride gas of hydrolysis reaction volatilization.
Germanium tetrachloride totally-enclosed hydrolysis device of the present utility model may further include temperature measuring equipment, and described temperature measuring equipment is arranged on and covers on described.Thus, further raising utilizes germanium tetrachloride totally-enclosed hydrolysis device to carry out the efficient of germanium tetrachloride hydrolysis.
Overcome traditional open hydrolysis device output hydrogen chloride gas according to the totally-enclosed hydrolysis device of the utility model embodiment environment has been caused the environmental protection pressure of corrosion, and adopted chilled brine that hydrolysis temperature in the still is controlled, significantly improved GeO 2The hydrolysis output capacity.
Additional aspect of the present utility model and advantage in the following description part provide, and part will become obviously from the following description, or recognize by practice of the present utility model.
Description of drawings
Above-mentioned and/or additional aspect of the present utility model and advantage are from obviously and easily understanding becoming the description of embodiment in conjunction with following accompanying drawing, wherein:
Fig. 1 is the structural representation according to the germanium tetrachloride totally-enclosed hydrolysis device of an embodiment of the utility model.
The specific embodiment
The below describes embodiment of the present utility model in detail, and the example of described embodiment is shown in the drawings, and wherein identical or similar label represents identical or similar element or the element with identical or similar functions from start to finish.Be exemplary below by the embodiment that is 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 "; " vertically "; " laterally "; " length "; " width "; " thickness ", " on ", D score, " front ", " afterwards ", " left side ", " right side ", " vertically ", " level ", " top ", " end ", " interior ", " outward ", " clockwise ", orientation or the position relationship of indications such as " counterclockwise " are based on orientation shown in the drawings or position relationship, only be for convenience of description the utility model and simplified characterization, rather than device or the element of indication 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 the utility model, unless clear and definite regulation and restriction are arranged in addition, broad understanding should be done in the terms such as term " installation ", " linking to each other ", " connection ", " fixing ", for example, can be to be fixedly connected with, and also can be to removably connect, or connect integratedly; Can be mechanical connection, also can be to be electrically connected; Can be directly to link to each other, also can indirectly link to each other by intermediary, can be the connection of two element internals.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 clear and definite regulation and restriction are arranged in addition, First Characteristic Second Characteristic it " on " or D score can comprise that the first and second features directly contact, can comprise that also the first and second features are not directly contacts but by the other feature contact between them.And, First Characteristic Second Characteristic " on ", " top " and " above " comprise First Characteristic directly over Second Characteristic and oblique upper, or only represent that the First Characteristic level height is higher than Second Characteristic.First Characteristic Second Characteristic " under ", " below " and " below " comprise First Characteristic under the Second Characteristic and tiltedly, or only represent that the First Characteristic level height is less than Second Characteristic.
The utility model is based on inventor's following discovery and finishes:
At present, hydrolysis usually carries out in semi-open still, and not only hydrogen chloride gas is reasonably processed, and environment is brought certain corrosion, and does not have effective temperature control measure, GeO 2Output capacity is not high, sometimes also can affect greatly quality; All under open operating environment, hydrolysis produces a large amount of hydrogen chloride gas to this hydrolysis---filter process, and environment is brought very large pressure, has affected on the one hand GeO 2Product quality is polluted easily, and the hydrogen chloride gas of hydrolysis reaction volatilization has corrosivity, when affecting environment worker's occupational health is worked the mischief, and has been not suitable with the needs of modern production.
For this reason, in first aspect of the present utility model, the utility model proposes a kind of can be effectively to the germanium tetrachloride reaction that is hydrolyzed, obtain to contain the germanium tetrachloride totally-enclosed hydrolysis device of the hydrolysate of germanium dioxide.According to embodiment of the present utility model, with reference to figure 5, this germanium tetrachloride totally-enclosed hydrolysis device comprises: kettle 52, the first charging aperture 55, the second charging aperture 510, exhaust outlet 59 and discharge gate 155.According to embodiment of the present utility model, be limited with the hydrolysis space in the kettle 52 of this germanium tetrachloride totally-enclosed hydrolysis device, the top that loam cake 54 is arranged on described kettle 52 is used for the hydrolysis space that this kettle 52 of sealing limits, the first charging aperture 55 is arranged on the loam cake 54, be used for to hydrolysis space supply germanium tetrachloride rectifying liquid, the second charging aperture 510 is arranged on the loam cake 54, be used for supplying with ultra-pure water to the hydrolysis space, exhaust outlet 59 is arranged on the loam cake 54, be used for the hydrogen chloride gas of hydrolysis reaction volatilization is discharged from the hydrolysis space, discharge gate 155 is arranged on the bottom of kettle 52, is used for the discharge water hydrolysis products.Utilize this germanium tetrachloride totally-enclosed hydrolysis device, can carry out in confined conditions the germanium tetrachloride hydrolysis.
According to embodiment of the present utility model, germanium tetrachloride totally-enclosed hydrolysis device of the present utility model may further include agitating device 511, and agitating device 511 can be arranged in the hydrolysis space, is used for stirring the reactant in hydrolysis space.Thus, can by the contact area of Effective Raise reactant, utilize germanium tetrachloride totally-enclosed hydrolysis device to carry out the efficient of germanium tetrachloride hydrolysis thereby further improve.Germanium tetrachloride totally-enclosed hydrolysis device of the present utility model can further include motor 57, and motor 57 is arranged on the described loam cake 54, and links to each other with agitating device 511, is used for control agitating device 511.Thus, can hang down easily the driving agitating device, utilize germanium tetrachloride totally-enclosed hydrolysis device to carry out the efficient of germanium tetrachloride hydrolysis thereby further improve.In addition, germanium tetrachloride totally-enclosed hydrolysis device of the present utility model may further include reaction observation panel 56, and reaction observation panel 56 is arranged on the loam cake 54.Thus, can conveniently observe the process of hydrolysis, utilize germanium tetrachloride totally-enclosed hydrolysis device to carry out the efficient of germanium tetrachloride hydrolysis thereby further improve.Germanium tetrachloride totally-enclosed hydrolysis device of the present utility model may further include attemperating unit 12, and attemperating unit 12 is arranged on the outside of kettle 52.Thus, can easily the temperature in the hydrolysis space be controlled at optimal reaction temperature, for example subzero 5 ~ 15 degrees centigrade, can further improve thus and utilize germanium tetrachloride totally-enclosed hydrolysis device to carry out the efficient of germanium tetrachloride hydrolysis.According to embodiment of the present utility model, in the germanium tetrachloride totally-enclosed hydrolysis device of the present utility model, attemperating unit 12 is circulating frozen brine-cooled device.For example, can be by chilled brine import 53 and chilled brine outlet 513 be set, realize that chilled brine is cooling device circulating in the chuck for example, thus, can effectively control the temperature in the reaction compartment, utilize germanium tetrachloride totally-enclosed hydrolysis device to carry out the efficient of germanium tetrachloride hydrolysis thereby further improve.Germanium tetrachloride totally-enclosed hydrolysis device of the present utility model may further include temperature measuring equipment 58, temperature element for example, and according to embodiment of the present utility model, temperature measuring equipment 58 is arranged on the loam cake 54.Thus, the reaction temperature in can Real Time Monitoring hydrolysis space utilizes germanium tetrachloride totally-enclosed hydrolysis device to carry out the efficient of germanium tetrachloride hydrolysis thereby further improve.
In addition, germanium tetrachloride totally-enclosed hydrolysis device of the present utility model may further include four supports 51, and described support links to each other with described kettle, is used for supporting kettle.According to embodiment of the present utility model, the support of making kettle is set to, so that autoclave body bottom is arranged under the support ground level, thereby is convenient to direct discharging.
According to embodiment of the present utility model, in the germanium tetrachloride totally-enclosed hydrolysis device of the present utility model, described exhaust outlet links to each other with the alkali liquor absorption device.Thus, can be undertaken subsequent treatment after emptying by row of conduits to alkali liquor absorption device the hydrogen chloride gas of hydrolysis reaction volatilization, utilize germanium tetrachloride totally-enclosed hydrolysis device to carry out the germanium tetrachloride hydrolysis thereby further improve, reclaim the efficient of hydrogen chloride gas, and reduced pollution.
In the germanium tetrachloride totally-enclosed hydrolysis device of the present utility model, discharge gate links to each other with the centrifuge washing filter.Thus, can further improve and utilize germanium tetrachloride totally-enclosed hydrolysis device to carry out the efficient that germanium dioxide is reclaimed in germanium tetrachloride hydrolysis.
Thus, with reference to figure 1, the utility model proposes a kind of method that can utilize system described above to obtain germanium dioxide from germanium tetrachloride.According to embodiment of the present utility model, the method can comprise the following steps:
Germanium tetrachloride is hydrolyzed in the totally-enclosed hydrolysis kettle, in order to obtain the germanium tetrachloride hydrolysate, described germanium tetrachloride hydrolysate is germanium dioxide and hydrogen chloride.
According to embodiment of the present utility model, adopt the totally-enclosed hydrolysis device to the reaction that is hydrolyzed of germanium tetrachloride rectifying liquid, hydrogen chloride gas with the hydrolysis reaction volatilization is completely enclosed within the still on the one hand, and is emptying after row of conduits to alkali liquor absorption device is processed, and alleviated environmental protection pressure.According to embodiment of the present utility model, because the germanium tetrachloride hydrolysis generates GeO 2Reaction be reversible reaction, by in the hydrolysis device chuck, passing into continuously chilled brine, according to specific embodiment of the utility model, can control that hydrolysis temperature had both guaranteed at subzero 5 ~ 15 ℃ that hydrolysis was towards being conducive to GeO in the reactor 2The direction that generates is carried out, and has guaranteed again GeO 2Grain diameter is even, meets target level of product quality, has significantly improved GeO 2Output capacity.
Thus, the utility model proposes a kind of germanium tetrachloride totally-enclosed hydrolysis device, implementation step is as follows: 1. germanium tetrachloride rectifying liquid is sent in the totally-enclosed hydrolysis device, hydrolysis ratio input ultra-pure water according to germanium tetrachloride: ultra-pure water=1:6 ~ 7 reacts, opening chilled brine control reaction temperature is subzero 5 ~ 15 ℃, reaction time 30 ~ 60min; The hydrogen chloride gas of reaction institute output all drains into the alkali liquor absorption device and processes rear emptying.
In the description of this specification, 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 the example in conjunction with specific features, structure, material or the characteristics of this embodiment or example description.In this manual, the schematic statement of above-mentioned term not necessarily referred to identical embodiment or example.And the specific features of description, structure, material or characteristics can be with suitable mode combinations in any one or more embodiment or example.
Although the above has illustrated and has described embodiment of the present utility model, 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 in scope of the present utility model, can change above-described embodiment in the situation that does not break away from principle of the present utility model and aim, modification, replacement and modification.

Claims (9)

1. a germanium tetrachloride totally-enclosed hydrolysis device is characterized in that, comprising:
Kettle is limited with the hydrolysis space in the described kettle;
Loam cake, described loam cake is arranged on the top of described kettle;
The first charging aperture, described the first charging aperture are arranged on and cover on described, are used for supplying with to described hydrolysis space germanium tetrachloride rectifying liquid;
The second charging aperture, described the second charging aperture are arranged on and cover on described, are used for supplying with ultra-pure water to described hydrolysis space;
Exhaust outlet, described exhaust outlet are arranged on and cover on described, are used for the hydrogen chloride gas that hydrolysis generates is discharged from described hydrolysis space; And
Discharge gate, described discharge gate is arranged on the bottom of described kettle, is used for the discharge water hydrolysis products.
2. germanium tetrachloride totally-enclosed hydrolysis device according to claim 1 is characterized in that, further comprises agitating device, and described agitating device is arranged in the described hydrolysis space, is used for stirring the reactant in described hydrolysis space.
3. germanium tetrachloride totally-enclosed hydrolysis device according to claim 1 is characterized in that, further comprises motor, and described motor is arranged on and covers on described, and links to each other with described agitating device, is used for controlling described agitating device.
4. germanium tetrachloride totally-enclosed hydrolysis device according to claim 1 is characterized in that, further comprises the reaction observation panel, and described reaction observation panel is arranged on and covers on described.
5. germanium tetrachloride totally-enclosed hydrolysis device according to claim 1 is characterized in that, further comprise attemperating unit, described attemperating unit is arranged on the outside of described kettle.
6. germanium tetrachloride totally-enclosed hydrolysis device according to claim 5 is characterized in that, described attemperating unit is circulating frozen brine-cooled device.
7. germanium tetrachloride totally-enclosed hydrolysis device according to claim 1 is characterized in that, further comprises four supports, and described support links to each other with described kettle, is used for supporting kettle.
8. germanium tetrachloride totally-enclosed hydrolysis device according to claim 1 is characterized in that, described exhaust outlet links to each other with the alkali liquor absorption device.
9. germanium tetrachloride totally-enclosed hydrolysis device according to claim 1 is characterized in that, further comprises temperature measuring equipment, and described temperature measuring equipment is arranged on and covers on described.
CN 201220384044 2012-08-03 2012-08-03 Fully-closed germanium tetrachloride hydrolyzing device Expired - Lifetime CN202876800U (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102784611A (en) * 2012-08-03 2012-11-21 云南驰宏锌锗股份有限公司 Germanium tetrachloride fully-closed hydrolysis device
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
CN110090601A (en) * 2018-11-22 2019-08-06 云南驰宏国际锗业有限公司 The feeding mechanism and its control system of a kind of germanium tetrachloride hydrolysis device and application

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102784611A (en) * 2012-08-03 2012-11-21 云南驰宏锌锗股份有限公司 Germanium tetrachloride fully-closed hydrolysis device
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
CN110090601A (en) * 2018-11-22 2019-08-06 云南驰宏国际锗业有限公司 The feeding mechanism and its control system of a kind of germanium tetrachloride hydrolysis device and application

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C14 Grant of patent or utility model
GR01 Patent grant
TR01 Transfer of patent right
TR01 Transfer of patent right

Effective date of registration: 20190624

Address after: 655000 Floor 1-9 and Floor 1-2 of Cuifeng West Road and Xuefu Road, Qujing City, Yunnan Province

Patentee after: YUNNAN CHIHONG INTERNATIONAL GERMANIUM INDUSTRY Co.,Ltd.

Address before: 655011 Qujing Economic and Technological Development Zone, Qujing City, Yunnan Province

Patentee before: YUNNAN CHIHONG ZINC & GERMANIUM Co.,Ltd.

CX01 Expiry of patent term
CX01 Expiry of patent term

Granted publication date: 20130417