CN105439090B - A kind of device for preparing anhydrous metal chloride - Google Patents
A kind of device for preparing anhydrous metal chloride Download PDFInfo
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- CN105439090B CN105439090B CN201510923341.0A CN201510923341A CN105439090B CN 105439090 B CN105439090 B CN 105439090B CN 201510923341 A CN201510923341 A CN 201510923341A CN 105439090 B CN105439090 B CN 105439090B
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- rubber stopper
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B9/00—General methods of preparing halides
- C01B9/02—Chlorides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Inorganic Chemistry (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Drying Of Gases (AREA)
Abstract
The invention discloses a kind of device for preparing anhydrous metal chloride, including reaction tube, drying equipment, heating mantle, temperature control device, coolant jacket and cooling device, the loading pipe of activity is placed in the reaction zone of reaction tube, loading pipe is fixed on reaction utensil, metal derby is placed in reaction utensil, loading inside pipe wall is fixedly installed temperature tube, and thermocouple is placed in temperature tube, and thermocouple is connected with temperature control device；The crystal region of reaction tube is provided with crystallization collecting pipe.Chlorine is dried by drying equipment, is then reacted with metal, and reacted gas enters tail gas collecting device.The present apparatus has the advantages that rational technology, reacting balance, the introducing of impurity easy to control, low manufacture cost, pollution-free, nonhazardous, yield and product purity are high.
Description
Technical field
The invention belongs to chemical equipment technical field, and in particular to a kind of device for preparing anhydrous metal chloride.
Background technology
The synthetic method of anhydrous metal chloride mainly has peroxide breaks down chloridising, hydrate directly to add both at home and abroad at present
Heat dehydration method, dehydration of organic solvent method etc..Being limited these methods by each side condition and product quality has various shortcomings：If any
Solvent evaporation organic solvent can not be reused, and organic solvent easily remains and causes to produce on a small quantity after separated process
Product black, and have peculiar smell；Peroxide breaks down chlorination rule can not effectively removal oxygen element；And equipment complexity, yield be present
It is relatively low, seriously polluted, products obtained therefrom purity is not high, contaminant overstandard, crystallization jaundice the shortcomings of.
The content of the invention
In order to overcome the existing disadvantages mentioned above for preparing anhydrous metal chloride, the invention provides one kind to prepare anhydrous gold
Belong to the device of chloride.
Technical scheme is as follows used by the present invention solves above-mentioned technical problem：
A kind of device for preparing anhydrous metal chloride, including reaction tube, loading pipe, crystallization collecting pipe, heating mantle, cooling
Set, right rubber stopper, left rubber stopper, appendix, escape pipe, reaction utensil, temperature tube, thermocouple, temperature control device, tail gas absorption dress
Put, the right part of the reaction tube is reaction zone, and the left part of the reaction tube is crystal region, the outside of the reaction tube
Heating mantle and coolant jacket are correspondingly provided with, reaction tube both ends are respectively equipped with right rubber stopper and left rubber stopper；Set in the right rubber stopper
There are appendix and loading pipe, the loading pipe is placed in the reaction zone of reaction tube through right rubber stopper, is provided with above loading pipe anti-
Ware is answered, metal derby is placed with reaction utensil, the loading inside pipe wall is fixedly installed temperature tube, thermoelectricity is provided with the temperature tube
Even, the thermocouple is connected with temperature control device；Escape pipe and crystallization collecting pipe are provided with the left rubber stopper, the crystallization is collected
Pipe is located at through left rubber stopper in the crystal region of reaction tube, and the escape pipe is connected with device for absorbing tail gas.
Further, the appendix is connected by Two stage dryer device with chlorine, and the Two stage dryer device is by built-in
The drying chamber, airway tube, the drier built with desiccants for having liquid desiccant are composed in series, and chlorine is entered reaction tube
Moisture content is sufficiently removed before.
Further, the reaction utensil is hemispherical concave inward structure.
Further, the reaction zone of the heating mantle uniform fold reaction tube, to ensure that reaction tube is heated evenly.
Further, the crystal region of the coolant jacket uniform fold reaction tube, to ensure that reaction tube uniformly cools down.
Further, the reaction tube is pyroceram.So, reaction tube is hardly damaged, and reaction is easy to observe.
Further, the crystallization collecting pipe is concave inward structure, the collection of convenient crystallization.
According to a kind of device for preparing anhydrous metal chloride of the present invention, it is used to prepare anhydrous chloride with existing
Device is compared, and is had the advantages that：
（1）Chlorine moisture content in it completely removes chlorine before entering reaction tube by two-stage drying.
（2）Loading inside pipe wall is fixedly installed temperature tube, and thermocouple is placed in temperature tube, and this connected mode can be to anti-
Thing temperature is answered to carry out closely quickly measurement, measured temperature, while also can be more closer to the true temperature numerical value of reactant
Accurately the trip temperature that enters of control reaction prevents the generation of debris, the purity of anhydrous metal chloride needed for raising.
（3）The crystal region of reaction tube is furnished with cooling device, can accelerate the cooling procedure of anhydrous metal chloride, improves system
The efficiency of standby anhydrous metal chloride.
（4）There is crystallization collecting pipe in reaction tube, crystallized product is collected convenient.
（5）It is furnished with device for absorbing tail gas on the left of reaction tube, for absorbing the toxic gases such as chlorine.Safe preparation process ring
Protect.
The invention provides a kind of device for preparing anhydrous metal chloride, and anhydrous gold is prepared using metal direct chlorination method
Belong to chloride, there is rational technology, reacting balance, the introducing of impurity easy to control, low manufacture cost, pollution-free, nonhazardous, yield
With product purity it is high the advantages that, the anhydrous metal chloride crystallization purity for preparing of the present invention can reach more than 99.99%, yield
More than 95% can be reached.
Brief description of the drawings
Fig. 1 is the reaction unit structural representation of the present invention.
Fig. 2 is the structural representation of Two stage dryer device.
In accompanying drawing：1st, reaction tube；2nd, metal derby；3rd, reaction utensil；4 loading pipes；5th, temperature tube；6th, thermocouple；7th, right rubber
Plug；8th, appendix；9th, heating mantle；10th, temperature control device；11st, collecting pipe is crystallized；12nd, left rubber stopper；13rd, escape pipe；14th, cool down
Set；15th, cooling device；16th, air inlet pipe；17th, drying chamber；18th, liquid desiccant；19th, airway tube；20th, drier；21st, solid-state
Drier.
Embodiment
In order that technical problem solved by the invention, technical scheme and beneficial effect are more clearly understood, below in conjunction with
Drawings and Examples, the present invention is described in further detail.It should be appreciated that specific embodiment described herein is only
To explain the present invention, it is not intended to limit the present invention.
It refer to Fig. 1, a kind of device for preparing anhydrous metal chloride, including reaction tube 1, loading pipe 4, crystallization collecting pipe
11st, heating mantle 9, coolant jacket 14, right rubber stopper 7, left rubber stopper 12, appendix 8, escape pipe 13, reaction utensil 3, temperature tube 5, heat
Galvanic couple 6, temperature control device 10, device for absorbing tail gas.
The right part of reaction tube 1 is reaction zone, and outside uniform fold has heating mantle 9, the heating mantle 9 and heater
It is connected.The left part of reaction tube 1 is crystal region, and outside uniform fold has coolant jacket 14, the coolant jacket 14 and cooling device
15 are connected.The both ends of reaction tube 1 are respectively equipped with right rubber stopper 7 and left rubber stopper 12, and the left and right ends of reaction tube 1 are sealed.Need
It is bright, in practical application, can also use other sealing means.
Appendix 8 and loading pipe 4 are provided with right rubber stopper 7, the loading pipe 4 is placed in reaction tube 1 through right rubber stopper 7
In reaction zone, loading pipe 4 is provided with reaction utensil 3 above, and metal derby 2 is placed with reaction utensil 3.The metal derby 2 can use grain
The thinner metal dust of degree, to improve reaction speed, makes reaction more abundant.The external diameter of loading pipe 4 is less than the internal diameter of reaction tube 1, so that
Loading pipe 4 is placed in reaction tube 1 and ensures the completely same chlorine reaction of the metal derby 2 in reaction utensil 3.
The inwall of loading pipe 4 is fixedly installed temperature tube 5, and thermocouple 6, the thermocouple 6 and temperature are provided with the temperature tube 5
Control device 10 connects.This connected mode can carry out closely quickly measuring to temperature of charge, and measured temperature is closer
The true temperature numerical value of reactant, while also can more accurately control the trip temperature that enters of reaction to prevent the generation of debris, improve
The purity of required anhydrous metal chloride.
As shown in Fig. 2 appendix 8 is connected by Two stage dryer device with chlorine, the Two stage dryer device is by drying chamber
17th, airway tube 19, drier 20 are composed in series, and the appendix 8 is connected with drying chamber 17, and the drying chamber 17 passes through airway tube
19 are connected with the drier 20, and the drier 20 is connected with chlorine pot or chlorine still, and the inside of drying chamber 17 is equipped with liquid
State drier 18, the inside of drier 20 are equipped with desiccants 21, and chlorine is complete by two-stage drying device before reaction tube 1 is entered
Eliminate moisture content in chlorine entirely.
As shown in figure 1, being provided with escape pipe 13 and crystallization collecting pipe 11 in left rubber stopper 12, the crystallization collecting pipe 11 passes through
Left rubber stopper 12 is located in the crystal region of reaction tube 1, and the escape pipe 13 is connected with device for absorbing tail gas.Crystallize outside collecting pipe 11
Footpath is slightly less than the internal diameter of reaction tube 1, but gap very little therebetween, so that crystal is crystallized collecting pipe 11 and collected substantially.Go out
Tracheae 13 is connected on device for absorbing tail gas, and device for absorbing tail gas is used for absorbing the toxic gases such as chlorine.Safe preparation process ring
Protect.
The technique that the present invention prepares anhydrous metal chloride is as follows：
The first step：Take out right rubber stopper 7, it would be desirable to which the metal derby 2 reacted is placed on reaction utensil 3, compresses right rubber
Leather plug 7 makes its sealing close.
Second step：It is passed through chlorine and is passed to air inlet pipe 16 into drying chamber 17, passes through liquid desiccant 18, absorb chlorine
In moisture content, then by airway tube 19 enter drier 20, the moisture content in chlorine is further absorbed by desiccants 21.
3rd step：Chlorine saturation in question response pipe 1 opens temperature control device 10 again later, by heating mantle 9 to reaction tube 1
Heated up, after reaction temperature is reached, metal derby 2 starts to distil with chlorine reaction, subsequently into holding stage, treats metal derby
2, with stopping heating up after chlorine completely reaction, close heat riser.
Final step：Open cooling device 15 crystallized, it is to be crystallized completely after, take out left side rubber stopper will crystallize receive
Crystallization on collector 11 is collected sampling.Result of laboratory test shows that the anhydrous metal chloride crystallization purity of gained can reach
More than 99.99%, yield can reach more than 95%.
It is described be only presently preferred embodiments of the present invention, be not intended to limit the invention, it is all the present invention spirit and
All any modification, equivalent and improvement made within principle etc., should be included in the scope of the protection.The present invention
In unaccounted device and equipment can be realized using prior art.
Claims (7)
1. a kind of device for preparing anhydrous metal chloride, including reaction tube, loading pipe, crystallization collecting pipe, heating mantle, cooling
Set, right rubber stopper, left rubber stopper, appendix, escape pipe, reaction utensil, temperature tube, thermocouple, temperature control device, tail gas absorption dress
Put, the left part of the reaction tube is crystal region, and the right part of the reaction tube is reaction zone, the outside of the reaction tube
Provided with heating mantle and coolant jacket, reaction tube both ends are respectively equipped with right rubber stopper and left rubber stopper；It is provided with the right rubber stopper defeated
Tracheae and loading pipe, the loading pipe are placed in the reaction zone of reaction tube through right rubber stopper, and reaction utensil is provided with above loading pipe,
Metal derby is placed with reaction utensil, the loading inside pipe wall is fixedly installed temperature tube, thermocouple, institute are provided with the temperature tube
Thermocouple is stated to be connected with temperature control device；Escape pipe and crystallization collecting pipe are provided with the left rubber stopper, the crystallization collecting pipe is worn
Cross left rubber stopper to be located in the crystal region of reaction tube, the escape pipe is connected with device for absorbing tail gas.
2. a kind of device for preparing anhydrous metal chloride according to claim 1, it is characterised in that the appendix leads to
Cross Two stage dryer device with chlorine to be connected, the Two stage dryer device is by built with the drying chamber of liquid desiccant, airway tube, interior
Drier equipped with desiccants is composed in series, and chlorine is sufficiently removed moisture content before entering reaction tube.
3. a kind of device for preparing anhydrous metal chloride according to claim 1, it is characterised in that the reaction utensil is
Hemispherical concave inward structure.
4. a kind of device for preparing anhydrous metal chloride according to claim 1, it is characterised in that the heating mantle is equal
The reaction zone of even covering reaction tube, to ensure that reaction tube is heated evenly.
5. a kind of device for preparing anhydrous metal chloride according to claim 1, it is characterised in that the coolant jacket is equal
The crystal region of even covering reaction tube, to ensure that reaction tube uniformly cools down.
6. a kind of device for preparing anhydrous metal chloride according to claim 1, it is characterised in that the reaction tube is
Pyroceram.
7. a kind of device for preparing anhydrous metal chloride according to claim 1, it is characterised in that the crystallization is collected
Manage as concave inward structure, the collection of convenient crystallization.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510923341.0A CN105439090B (en) | 2015-12-14 | 2015-12-14 | A kind of device for preparing anhydrous metal chloride |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510923341.0A CN105439090B (en) | 2015-12-14 | 2015-12-14 | A kind of device for preparing anhydrous metal chloride |
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| CN105439090A CN105439090A (en) | 2016-03-30 |
| CN105439090B true CN105439090B (en) | 2018-02-06 |
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| CN201510923341.0A Active CN105439090B (en) | 2015-12-14 | 2015-12-14 | A kind of device for preparing anhydrous metal chloride |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107983291A (en) * | 2017-10-28 | 2018-05-04 | 株洲冶炼集团股份有限公司 | A kind of devices and methods therefor for preparing anhydrous gallium chloride |
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| CN101792174A (en) * | 2010-03-12 | 2010-08-04 | 韶关市锦源实业有限公司 | Anhydrous indium chloride synthesizing method |
| CN102352439A (en) * | 2011-07-18 | 2012-02-15 | 株洲冶炼集团股份有限公司 | Method of producing zinc chloride and aluminum chloride by using waste zinc-aluminum alloy |
| CN202254801U (en) * | 2011-07-13 | 2012-05-30 | 沈少波 | Tubular reaction furnace and chlorination reaction device with same |
| CN103626215A (en) * | 2013-09-17 | 2014-03-12 | 攀钢集团攀枝花钢铁研究院有限公司 | Method and device for preparing aluminum trichloride |
| CN205187847U (en) * | 2015-12-14 | 2016-04-27 | 株洲冶炼集团股份有限公司 | Prepare anhydrous metal chloride's device |
| CN205288376U (en) * | 2015-10-19 | 2016-06-08 | 清远先导材料有限公司 | Apparatus for producing of gallium trichloride |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010001207A (en) * | 2008-05-19 | 2010-01-07 | Toho Titanium Co Ltd | Device and method for manufacturing metal chloride |
| JP5897488B2 (en) * | 2013-03-19 | 2016-03-30 | 東邦チタニウム株式会社 | Method for producing titanium tetrachloride |
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2015
- 2015-12-14 CN CN201510923341.0A patent/CN105439090B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101254943A (en) * | 2008-04-07 | 2008-09-03 | 昆明理工大学 | Preparation method of high-purity indium triiodide |
| CN101792174A (en) * | 2010-03-12 | 2010-08-04 | 韶关市锦源实业有限公司 | Anhydrous indium chloride synthesizing method |
| CN202254801U (en) * | 2011-07-13 | 2012-05-30 | 沈少波 | Tubular reaction furnace and chlorination reaction device with same |
| CN102352439A (en) * | 2011-07-18 | 2012-02-15 | 株洲冶炼集团股份有限公司 | Method of producing zinc chloride and aluminum chloride by using waste zinc-aluminum alloy |
| CN103626215A (en) * | 2013-09-17 | 2014-03-12 | 攀钢集团攀枝花钢铁研究院有限公司 | Method and device for preparing aluminum trichloride |
| CN205288376U (en) * | 2015-10-19 | 2016-06-08 | 清远先导材料有限公司 | Apparatus for producing of gallium trichloride |
| CN205187847U (en) * | 2015-12-14 | 2016-04-27 | 株洲冶炼集团股份有限公司 | Prepare anhydrous metal chloride's device |
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Inventor after: Fu Dongcai Inventor after: Lin Wenjun Inventor after: Tang Yiqiu Inventor after: Dai Huimin Inventor after: Wang Wenjun Inventor after: Liu Yining Inventor after: Tang Aiyong Inventor before: Tang Yiqiu Inventor before: Liu Yining Inventor before: Wang Wenjun Inventor before: Dai Huimin Inventor before: Tang Aiyong |
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