CN105439090A - Apparatus for preparing anhydrous metal chloride - Google Patents
Apparatus for preparing anhydrous metal chloride Download PDFInfo
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- CN105439090A CN105439090A CN201510923341.0A CN201510923341A CN105439090A CN 105439090 A CN105439090 A CN 105439090A CN 201510923341 A CN201510923341 A CN 201510923341A CN 105439090 A CN105439090 A CN 105439090A
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- reaction
- tube
- reaction tubes
- soft rubber
- rubber ball
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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 an apparatus for preparing anhydrous metal chloride. The apparatus comprises a reaction tube, a drying device, a heating sleeve, a temperature control unit, a cooling jacket and a cooling device, wherein a movable material loading tube is placed in a reaction zone of the reaction tube, a reaction vessel is fixed on the material loading tube, a metal block is placed in the reaction vessel, a temperature measurement tube is fixed on the inner wall of the material loading tube, a thermocouple is arranged in the temperature measurement tube and connected with the temperature control unit, and a crystallization zone of the reaction tube is provided with a crystal collecting tube. Chlorine is dried by the drying device and then reacted with metal, and reacted gas enters a tail gas gathering device. The apparatus provided by the invention has the advantages of reasonable process, stationary reaction, easiness in controlling introduction of impurities, low making cost, no pollution, no toxicity and harm, high yield, high product purity, etc.
Description
Technical field
The invention belongs to chemical equipment technical field, be specifically related to one and prepare the muriatic device of anhydrous metal.
Background technology
The muriatic synthetic method of anhydrous metal mainly contains peroxide breaks down chlorination process, hydrate direct heating evaporation, dehydration of organic solvent method etc. both at home and abroad at present.These methods that limit by each side condition and product quality have various shortcoming: as dehydration of organic solvent method organic solvent cannot be reused, and organic solvent easily remains on a small quantity and causes product to turn black after fractionation by distillation operation, has peculiar smell; Peroxide breaks down chlorination rule can not effectively removal oxygen element; And there is equipment complexity, the shortcoming such as productive rate is lower, seriously polluted, products obtained therefrom purity is not high, contaminant overstandard, crystallization jaundice.
Summary of the invention
Existingly preparing the muriatic above-mentioned shortcoming of anhydrous metal to overcome, the invention provides one and preparing the muriatic device of anhydrous metal.
It is as follows that the present invention solves the problems of the technologies described above adopted technical scheme:
One prepares the muriatic device of anhydrous metal, comprise reaction tubes, loading pipe, crystallization collection tube, heating jacket, cooling jacket, right soft rubber ball, left soft rubber ball, pneumatic tube, escape pipe, reaction utensil, temperature tube, thermopair, temperature control unit, device for absorbing tail gas, the right part of described reaction tubes is reaction zone, the left part of described reaction tubes is crystallizing field, the outside correspondence of described reaction tubes is provided with heating jacket and cooling jacket, and reaction tubes two ends are respectively equipped with right soft rubber ball and left soft rubber ball; Pneumatic tube and loading pipe is provided with in described right soft rubber ball, described loading pipe is placed in the reaction zone of reaction tubes through right soft rubber ball, reaction utensil is provided with above loading pipe, metal block is placed with in reaction utensil, described loading inside pipe wall is fixedly installed temperature tube, be provided with thermopair in described temperature tube, described thermopair is connected with temperature control unit; Be provided with escape pipe and crystallization collection tube in described left soft rubber ball, described crystallization collection tube is positioned at the crystallizing field of reaction tubes through left soft rubber ball, and described escape pipe is connected with device for absorbing tail gas.
Further, described pneumatic tube is connected with chlorine by Two stage dryer device, described Two stage dryer device by built with liquid desiccant drying chamber, airway, be composed in series built with the moisture eliminator of desiccants, make chlorine enter reaction tubes before be sufficiently removed moisture content.
Further, described reaction utensil is semisphere concave inward structure.
Further, the reaction zone of described heating jacket uniform fold reaction tubes, to ensure that reaction tubes is heated evenly.
Further, the crystallizing field of described cooling jacket uniform fold reaction tubes, to ensure reaction tubes Homogeneous cooling.
Further, described reaction tubes is pyroceram.Like this, reaction tubes is not fragile, and reaction is easy to observe.
Further, described crystallization collection tube is concave inward structure, facilitates the collection of crystallization.
One according to the present invention prepares the muriatic device of anhydrous metal, compared with the existing device for the preparation of anhydrous chloride, has following beneficial effect:
(1) chlorine completely removes moisture content in chlorine through two-stage drying before entering reaction tubes.
(2) loading inside pipe wall is fixedly installed temperature tube, thermopair is placed in temperature tube, this mode of connection closely can be measured fast to temperature of charge, measured temperature is closer to the true temperature numerical value of reactant, what also can control reaction more accurately carries out the generation that temperature prevents foreign material simultaneously, improves the required muriatic purity of anhydrous metal.
(3) crystallizing field of reaction tubes is furnished with refrigerating unit, can accelerate the muriatic process of cooling of anhydrous metal, improves and prepares the muriatic efficiency of anhydrous metal.
(4) have crystallization collection tube in reaction tubes, crystallized product is collected convenient.
(5) device for absorbing tail gas is furnished with on the left of reaction tubes, for absorbing the toxic gases such as chlorine.Safe preparation process environmental protection.
The invention provides one and prepare the muriatic device of anhydrous metal, the direct chlorination process of metal is adopted to prepare anhydrous metal muriate, have that rational technology, reacting balance, the introducing of impurity easy to control, cost of manufacture are low, pollution-free, toxicological harmless, productive rate and product purity advantages of higher, anhydrous metal chloride crystallization purity prepared by the present invention can reach more than 99.99%, and productive rate can reach more than 95%.
Accompanying drawing explanation
Fig. 1 is reaction unit structural representation of the present invention.
Fig. 2 is the structural representation of Two stage dryer device.
In accompanying drawing: 1, reaction tubes; 2, metal block; 3, reaction utensil; 4 loading pipes; 5, temperature tube; 6, thermopair; 7, right soft rubber ball; 8, pneumatic tube; 9, heating jacket; 10, temperature control unit; 11, crystallization collection tube; 12, left soft rubber ball; 13, escape pipe; 14, cooling jacket; 15, cooling apparatus; 16, inlet pipe; 17, drying chamber; 18, liquid desiccant; 19, airway; 20, moisture eliminator; 21, desiccants.
Embodiment
In order to make technical problem solved by the invention, technical scheme and beneficial effect clearly understand, below in conjunction with drawings and Examples, the present invention is described in further detail.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Please refer to Fig. 1, one prepares the muriatic device of anhydrous metal, comprises reaction tubes 1, loading pipe 4, crystallization collection tube 11, heating jacket 9, cooling jacket 14, right soft rubber ball 7, left soft rubber ball 12, pneumatic tube 8, escape pipe 13, reaction utensil 3, temperature tube 5, thermopair 6, temperature control unit 10, device for absorbing tail gas.
The right part of reaction tubes 1 is reaction zone, and outside uniform fold has heating jacket 9, and described heating jacket 9 is connected with heating unit.The left part of reaction tubes 1 is crystallizing field, and outside uniform fold has cooling jacket 14, and described cooling jacket 14 is connected with cooling apparatus 15.Reaction tubes 1 two ends are respectively equipped with right soft rubber ball 7 and left soft rubber ball 12, are sealed at reaction tubes about 1 two ends.It should be noted that, when practical application, also can adopt other sealing means.
Be provided with pneumatic tube 8 and loading pipe 4 in right soft rubber ball 7, described loading pipe 4 is placed in the reaction zone of reaction tubes 1 through right soft rubber ball 7, and loading pipe 4 is provided with reaction utensil 3 above, is placed with metal block 2 in reaction utensil 3.The metal-powder that described metal block 2 can adopt granularity thinner, to improve speed of response, makes reaction more abundant.Loading pipe 4 external diameter is less than reaction tubes 1 internal diameter, to be placed in reaction tubes 1 and to ensure the complete same chlorine reaction of metal block 2 in reaction utensil 3 to make loading pipe 4.
Loading pipe 4 inwall is fixedly installed temperature tube 5, is provided with thermopair 6 in described temperature tube 5, and described thermopair 6 is connected with temperature control unit 10.This mode of connection closely can be measured fast to temperature of charge, measured temperature is closer to the true temperature numerical value of reactant, what also can control reaction more accurately carries out the generation that temperature prevents foreign material simultaneously, improves the required muriatic purity of anhydrous metal.
As shown in Figure 2, pneumatic tube 8 is connected with chlorine by Two stage dryer device, described Two stage dryer device is composed in series by drying chamber 17, airway 19, moisture eliminator 20, described pneumatic tube 8 is connected with drying chamber 17, described drying chamber 17 is connected with described moisture eliminator 20 through airway 19, described moisture eliminator 20 is connected with chlorine pot or chlorine still, liquid desiccant 18 is equipped with in drying chamber 17 inside, desiccants 21 is equipped with in moisture eliminator 20 inside, and chlorine completely removes moisture content in chlorine through two-stage drying device before entering reaction tubes 1.
As shown in Figure 1, be provided with escape pipe 13 and crystallization collection tube 11 in left soft rubber ball 12, described crystallization collection tube 11 is positioned at the crystallizing field of reaction tubes 1 through left soft rubber ball 12, described escape pipe 13 is connected with device for absorbing tail gas.Crystallization collection tube 11 external diameter is slightly less than reaction tubes 1 internal diameter, but gap is therebetween very little, is substantially collected by crystallization collection tube 11 to make crystallisate.Escape pipe 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 environmental protection.
It is as follows that the present invention prepares the muriatic technique of anhydrous metal:
The first step: take out right soft rubber ball 7, by needing the metal block 2 carrying out reacting to be placed on reaction utensil 3, compressing right soft rubber ball 7 and making it seal closely.
Second step: pass into chlorine and make it enter drying chamber 17 by inlet pipe 16, by liquid desiccant 18, absorbs the moisture content in chlorine, then enters moisture eliminator 20 by airway 19, is further absorbed the moisture content in chlorine by desiccants 21.
3rd step: open temperature control unit 10 again after the chlorine in question response pipe 1 is saturated, heated up by heating jacket 9 pairs of reaction tubess 1, after reaching temperature of reaction, metal block 2 and chlorine reaction start to distil, then holding stage is entered, stop heating up after metal block 2 with chlorine complete reaction, close heat riser.
Final step: open cooling apparatus 15 and carry out crystallization, to be crystallized completely after, take out left side soft rubber ball and collecting and sampling carried out in the crystallization on crystallization collection tube 11.Result of laboratory test shows that the anhydrous metal chloride crystallization purity of gained can reach more than 99.99%, and productive rate can reach more than 95%.
Describedly be only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalently replace and improvement etc., all should be included within protection scope of the present invention.In the present invention, unaccounted device and equipment all can adopt prior art to be realized.
Claims (7)
1. prepare the muriatic device of anhydrous metal for one kind, comprise reaction tubes, loading pipe, crystallization collection tube, heating jacket, cooling jacket, right soft rubber ball, left soft rubber ball, pneumatic tube, escape pipe, reaction utensil, temperature tube, thermopair, temperature control unit, device for absorbing tail gas, the left part of described reaction tubes is reaction zone, the right part of described reaction tubes is crystallizing field, the outside of described reaction tubes is provided with heating jacket and cooling jacket, and reaction tubes two ends are respectively equipped with right soft rubber ball and left soft rubber ball; Pneumatic tube and loading pipe is provided with in described right soft rubber ball, described loading pipe is placed in the reaction zone of reaction tubes through right soft rubber ball, reaction utensil is provided with above loading pipe, metal block is placed with in reaction utensil, described loading inside pipe wall is fixedly installed temperature tube, be provided with thermopair in described temperature tube, described thermopair is connected with temperature control unit; Be provided with escape pipe and crystallization collection tube in described left soft rubber ball, described crystallization collection tube is positioned at the crystallizing field of reaction tubes through left soft rubber ball, and described escape pipe is connected with device for absorbing tail gas.
2. one according to claim 1 prepares the muriatic device of anhydrous metal, it is characterized in that, described pneumatic tube is connected with chlorine by Two stage dryer device, described Two stage dryer device by built with liquid desiccant drying chamber, airway, be composed in series built with the moisture eliminator of desiccants, make chlorine enter reaction tubes before be sufficiently removed moisture content.
3. one according to claim 1 prepares the muriatic device of anhydrous metal, it is characterized in that, described reaction utensil is semisphere concave inward structure.
4. one according to claim 1 prepares the muriatic device of anhydrous metal, it is characterized in that, the reaction zone of described heating jacket uniform fold reaction tubes, to ensure that reaction tubes is heated evenly.
5. one according to claim 1 prepares the muriatic device of anhydrous metal, it is characterized in that, the crystallizing field of described cooling jacket uniform fold reaction tubes, to ensure reaction tubes Homogeneous cooling.
6. one according to claim 1 prepares the muriatic device of anhydrous metal, it is characterized in that, described reaction tubes is pyroceram.
7. one according to claim 1 prepares the muriatic device of anhydrous metal, it is characterized in that, described crystallization collection tube is concave inward structure, facilitates the collection of 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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| CN201510923341.0A CN105439090B (en) | 2015-12-14 | 2015-12-14 | A kind of device for preparing anhydrous metal chloride |
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| CN105439090A true CN105439090A (en) | 2016-03-30 |
| CN105439090B CN105439090B (en) | 2018-02-06 |
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Cited By (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 |
Citations (9)
| 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 |
| JP2010001207A (en) * | 2008-05-19 | 2010-01-07 | Toho Titanium Co Ltd | Device and method for manufacturing metal chloride |
| 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 |
| JP2014181153A (en) * | 2013-03-19 | 2014-09-29 | Toho Titanium Co Ltd | Method for producing titanium tetrachloride |
| 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 |
-
2015
- 2015-12-14 CN CN201510923341.0A patent/CN105439090B/en active Active
Patent Citations (9)
| 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 |
| JP2010001207A (en) * | 2008-05-19 | 2010-01-07 | Toho Titanium Co Ltd | Device and method for manufacturing metal chloride |
| 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 |
| JP2014181153A (en) * | 2013-03-19 | 2014-09-29 | Toho Titanium Co Ltd | Method for producing titanium tetrachloride |
| 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 |
Cited By (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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| CN105439090B (en) | 2018-02-06 |
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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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