CN100586860C - Preparation for anhydrous magnesium chloride powder - Google Patents
Preparation for anhydrous magnesium chloride powder Download PDFInfo
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- CN100586860C CN100586860C CN200710078065A CN200710078065A CN100586860C CN 100586860 C CN100586860 C CN 100586860C CN 200710078065 A CN200710078065 A CN 200710078065A CN 200710078065 A CN200710078065 A CN 200710078065A CN 100586860 C CN100586860 C CN 100586860C
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- magnesium chloride
- crucible
- nozzle
- collecting bin
- conveying pipeline
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Abstract
The invention provides a method for the production and a device of anhydrous magnesium chloride powder, the magnesium chloride is melted at a temperature above the melting point of the magnesium chloride, the fused mass of the magnesium chloride is sprayed out by an inert gas and the fusing liquid of the magnesium chloride is atomized by the dry compressed air, and the anhydrous magnesium chloridepowder is obtained through condensation. The device comprises a melting furnace, a crucible, a feeding fused mass pipeline, a nozzle, a compressor and a collecting bin; and the method includes following steps of: (1) putting the magnesium chloride into the furnace, (2) melting the magnesium chloride, (3) high-frequency heating to the magnesium chloride feeding pipeline and the nozzle, (4) atomization, and (5) collection and packaging. The atomization of the invention adopts the dried high pressure compressed air to impact the liquid jets of the molten magnesium chloride strongly so as to reach the atomization effect, and the process and operation are simple and convenient, thereby obtaining relative pure anhydrous magnesium chloride powder; the atomized products are spherical and the particle-size distribution is even; and the particle sizes of the products can be adjusted flexibly according to the demands of customers.
Description
Technical field
The present invention relates to the muriate of magnesium, particularly atomization prepares anhydrous magnesium chloride.
Background technology
Anhydrous magnesium chloride is mainly used in the electrolytic magnesium industrial raw material, the flux of refined magnesium and make far-infrared compound electric-heating element, and composite decorating board, the material of thermal insulating etc., the anhydrous chlorides of rase magnesium granules can be used for the olefin catalytic agent carrier.
Industrially adopt the dehydration of two steps when being raw material production magnesium with seawater or salt lake brine: the one, with about 200 ℃ hot gas flows Mgcl
26H
2O at first takes off to Mgcl
21～2H
2O; The 2nd, low aqueous magnesium chloride dehydration fully under hydrogenchloride atmosphere again through dehydration, obtain the granulous Magnesium Chloride Anhydrous, as the electrolytic magnesium industrial raw material, Chinese patent application 02224408.5 " is utilized magnesium chloride dihydrate to produce the device of Magnesium Chloride Anhydrous " and has been announced a kind of production equipment.
The production method of anhydrous magnesium chloride, announced in Chinese patent application 02146192.9 " Magnesium Chloride Anhydrous particulate working method " and to have used the centrifugal atomizing process for granulating that centrifugal dispersive Magnesium Chloride Anhydrous grain drops in and forms spherical with the airflow back condensation of meeting in the granulation chamber; Chinese patent ZL91101047.5 " preparation method of magnesium chloride granules " is dissolved in magnesium chloride in a kind of alcohol, makes emulsion liquid-phase precipitation granulation again, is used for the olefin catalytic agent carrier.
The production method and the equipment of prior art are targeted, are restricted at aspects such as granularity, particle shapes, often can not reach customer requirements.
Summary of the invention
In order to overcome prior art problems, obtain purified anhydrous magnesium chloride, the object of the present invention is to provide a kind of preparation method and equipment of anhydrous magnesium chloride, temperature more than the magnesium chloride fusing point makes the magnesium chloride fusing, makes the ejection of magnesium chloride melt and with dried compressed air the atomizing of magnesium chloride melt liquid, condensation is obtained anhydrous magnesium chloride with rare gas element.
To achieve these goals, technical scheme of the present invention is as follows: a kind of preparation equipment of anhydrous magnesium chloride, it is characterized in that comprising smelting furnace, crucible, the melt conveying pipeline, nozzle, air compressor machine, collecting bin, described crucible places in the smelting furnace, crucible is for covering sealed crucible, the ring flange of crucible cover is connected sealing with the ring flange of crucible body with screw, crucible has the rare gas element pneumatic tube to be connected with the rare gas element gas cylinder, be connected to the melt conveying pipeline on the crucible, described melt conveying pipeline other end connects nozzle, set up the pipeline radio-frequency heater on the melt conveying pipeline, described nozzle is the linear pattern jet pipe, outlet aperture 4～8mm, nozzle has been set up the nozzle radio-frequency heater outward, nozzle enters the collecting bin head, nozzle side has the pressurized air tracheae, nozzle and compressed air inlet pipe form V-type at an angle to each other and spray, angle is 35 °～42 °, pressurized air tracheae other end connects pneumatics jar and air compressor machine, described collecting bin is a multi-chamber, its bottom, every storehouse is provided with board plug type and collects mouth, and the collecting bin afterbody connects gas cyclone device and vacuum fan by pipeline.
Described smelting furnace is an electric furnace.
Crucible places in the smelting furnace, and smelting furnace is in order to the heat fused magnesium chloride; The melt conveying pipeline makes the magnesium chloride of molten state be transported to nozzle under inert gas pressure and is sprayed by nozzle, air compressor machine is used for providing atomizing required high pressure dried compressed air, pressurized air is the propulsion source that magnesium chloride liquid stream is smashed, and is again a kind of refrigerant; Collecting bin is made up of several storehouses, and varigrained powder is deposited to different feed bins during sedimentation, and the powder that atomizing obtains can just can reach the effect of different grain size separate collection without screening; The high-frequency heating apparatus rate of heating is fast, and melt conveying pipeline and nozzle are heated, and prevents that melt liquid from causing plugging when piping and nozzle; All operations carries out on supervisory control desk, comprises control of pressurized air, inert gas pressure Flow-rate adjustment, the control of smelting furnace power supply, high-frequency apparatus oscillating current, automatic valve or the like, and is simple, convenient.
A kind of preparation method of anhydrous magnesium chloride is characterized in that comprising the following steps:
(1) go into stove:
With magnesium chloride melt or solid is raw material, and it is added in the crucible, tightens the ring flange screw of crucible, and sealed crucible hangs in electric furnace with crucible again;
(2) magnesium chloride fusing:
Electric furnace send electricity, heating, fusing; Make the interior magnesium chloride melt temperature of crucible be heated to 800～900 ℃;
(3) magnesium chloride transport pipe and nozzle are carried out ratio-frequency heating:
Making melt conveying pipeline medial temperature is 790～810 ℃, and nozzle temperature is 870～900 ℃;
(4) atomizing:
Open collecting bin afterbody vacuum fan, the rare gas element with certain pressure intensity feeds in the crucible again, and the pressure that rare gas element produces makes the interior magnesium chloride melt of crucible along the nozzle ejection of melt conveying pipeline by pipe end; Feed pressurized air simultaneously; Make the molten magnesium chloride atomization of liquid;
(5) collect and packing:
Magnesium chloride powder enters the collecting bin bottom, and the air communication of entrained fines is crossed the gas cyclone device of collecting bin afterbody, emptying after gathering dust; The board plug type that is provided with from the collecting bin bottom is collected a mouthful bottom and is emitted magnesium chloride powder, packs with plastic bag sealing.
The present invention compared with prior art has the following advantages and effect:
1, atomization adopts the exsiccant high pressure air that molten magnesium chloride liquid beam intense impact is reached atomizing effect, and technology is simple, easy to operate;
2, owing to adopt molten magnesium chloride to atomize, can obtain purified relatively anhydrous magnesium chloride;
3, atomised product is spherical, even particle size distribution;
4, can regulate product granularity neatly by the method for adjusting pressurized air and rare gas element according to customer requirement;
The preparation method of a kind of Magnesium Chloride Anhydrous powder of the present invention can be applicable to titanium sponge manufacturing enterprise and other produces the place of magnesium chloride, has the advantage that technology is simple, easy to operate, cost is low, product is spherical, epigranular, be purified relatively anhydrous magnesium chloride, operating process is simple, convenient.
Description of drawings
The present invention is described in detail below in conjunction with accompanying drawing.
Fig. 1 connects schematic top plan view for embodiment of the invention equipment;
Fig. 2 installs connection diagram for collecting bin;
Fig. 3 is the influence of compressed air require to the aerosol granularity;
Fig. 4 is one of product enlarged photograph;
Fig. 5 is two of a product enlarged photograph;
Among each figure: 1 is the rare gas element gas cylinder, and 2 is air compressor machine, and 3 is the pneumatics jar, and 4 is the pressurized air tracheae, and 5 is vacuum fan, 6 is the gas cyclone device, and 7 is collecting bin, and 8 is the melt conveying pipeline, and 9 is smelting furnace, 10 is crucible, and 11 is the rare gas element pneumatic tube, and 12 are board plug type collection mouth, and 13 is nozzle.
Embodiment
Embodiment
Equipment connects vertical view as shown in Figure 1: equipment of the present invention comprises smelting furnace 9, crucible 10, melt conveying pipeline 8, nozzle 13, air compressor machine 2, collecting bin 7, crucible 10 places in the smelting furnace 9, crucible 10 is for covering sealed crucible 10, crucible 10 has rare gas element pneumatic tube 11 to be connected with argon gas body gas cylinder 1, be connected to melt conveying pipeline 8 on the crucible 10, melt conveying pipeline 8 other ends connect nozzle 13, set up pipeline radio-frequency heater (not shown) on the melt conveying pipeline 8, nozzle 13 is the linear pattern jet pipe, the nozzle 13 outer nozzle radio-frequency heater (not shown)s of having set up, nozzle 13 enters collecting bin 7 heads, nozzle 13 sides have pressurized air tracheae 4, nozzle 13 forms V-type at an angle to each other with compressed air inlet pipe 4 and sprays, angle is 35 °～42 °, and pressurized air tracheae 4 other ends connect pneumatics jar 3 and air compressor machine 2, as Fig. 1, shown in 2: described collecting bin 7 is four storehouse formulas, its bottom, every storehouse is provided with board plug type and collects mouth 12, and the collecting bin afterbody connects gas cyclone device 6 and vacuum fan 5 by pipeline.
Smelting furnace 9 is electric furnaces,
Nozzle 13 is the linear pattern jet pipe, outlet aperture 6mm.
Preparation method of the present invention comprises the following steps:
(1) goes into stove
Molten magnesium chloride liquid with the discharging of the reduction reactor in the titanium sponge production is raw material, and it is added in the crucible 10, tightens the ring flange screw of crucible 10, and sealed crucible 10 hangs in electric furnace 9 with crucible 10 again; (used magnesium chloride impurity component: MgO＜0.25%, Ti＜0.003%, KCl＜0.01%, NaCl＜0.15%)
(2) magnesium chloride fusing:
Electric furnace 9 send electricity, heating, fusing; Make crucible 10 interior magnesium chloride melt temperatures be heated to 820 ℃, this moment, electric furnace 9 bodies of heater were 910 ℃.
(3) magnesium chloride transport pipe 8 and nozzle 13 are carried out ratio-frequency heating:
Open pipeline radio-frequency heater and the nozzle 13 outer nozzle radio-frequency heaters of setting up set up on the melt conveying pipeline 8, making melt conveying pipeline 8 medial temperatures is 800 ℃, and nozzle 13 temperature are 890 ℃;
(4) atomizing:
Open collecting bin afterbody vacuum fan 5, the argon gas with certain pressure intensity feeds in the crucible 10 again, and making crucible 10 interior positive pressures is 0.12MP, and the pressure that rare gas element produces makes crucible 10 interior magnesium chloride melts along nozzle 13 ejections of melt conveying pipeline 8 by pipe end; Feed pressurized air simultaneously, the control compressed air pressure is 0.43Mpa; Make the molten magnesium chloride atomization of liquid; Electric furnace 9 outages in the atomization process utilize furnace body temperature melt in crucible 10 to continue to transmit heat; The temperature that atomizing finishes rear nozzle 13 also should keep certain hour, the magnesium chloride that prevents nozzle 13 remnants of place solidify and melt conveying pipeline 8 in remaining magnesium chlorides to cause melt conveying pipeline 8 to reflux when being back to fusion crucible 10 under action of gravity not smooth, operation is next time added to the difficulties.The contract size of the common decision of size magnesium chloride powder granularity of air inlet pressure/flow and crucible 10 internal pressures of nozzle 13 side pressures.Different compressed air requires atomizing observation on effect is down found at flow 40m by to positive pressure 0.12MPa in the crucible 10 (this moment, the melt bundle of ejection was ejected into the storehouse No. 4) time
3When/h was following, the powder size major part of collecting was bigger, and distributed pole is inhomogeneous.When flow reaches 96m
3During/h, granularity accounts for more than 82% at-60 orders～+ 140 purpose particles, mainly concentrates on feed bin 2, No. 3, so compressed air require is controlled at 96M
3/ h the left and right sides is proper.Fig. 3 is positive pressure 0.12MPa in the crucible, and when compressed air pressure was 0.43Mpa, at compressed air require the influence of granularity is tested: the X-coordinate of Fig. 3 was compressed air require M
3/ h, ordinate zou are-60 orders～shared per-cent of+140 orders.
(5) collect and packing:
Magnesium chloride powder enters collecting bin 7 bottoms, and the air communication of entrained fines is crossed the gas cyclone device 6 of collecting bin 7 afterbodys, emptying after gathering dust; The board plug type that is provided with from collecting bin 7 bottoms is collected mouthful 12 bottoms and is emitted magnesium chloride powder, packs with plastic bag sealing.
The product magnesium chloride powder of making is subsphaeroidal, and Fig. 4 is that one of product photo is 10 order product enlarged photographs, and Fig. 5 is that two of product photo is one 100 order product enlarged photographs.
Claims (3)
1. the preparation equipment of an anhydrous magnesium chloride is characterized in that comprising smelting furnace (9), crucible (10), melt conveying pipeline (8), nozzle (13), air compressor machine (2), collecting bin (7); Described crucible (10) places in the smelting furnace (9), crucible (10) is for covering sealed crucible (10), the ring flange of crucible cover is connected sealing with the ring flange of crucible body with screw, crucible (10) has rare gas element pneumatic tube (11) to be connected with rare gas element gas cylinder (1), be connected to melt conveying pipeline (8) on the crucible (10), described melt conveying pipeline (8) other end connects nozzle (13), and the melt conveying pipeline has been set up the pipeline radio-frequency heater on (8); Described nozzle (13) is the linear pattern jet pipe, the outlet aperture is 4～8mm, the outer nozzle radio-frequency heater of having set up of nozzle (13), nozzle (13) enters collecting bin (7) head, nozzle (13) side has pressurized air tracheae (4), nozzle (13) forms V-type at an angle to each other with compressed air inlet pipe (4) and sprays, angle is 35 °～42 °, pressurized air tracheae (4) other end connects pneumatics jar (3) and air compressor machine (2), described collecting bin (7) is a multi-chamber, its bottom, every storehouse is provided with board plug type and collects mouthful (12), and the collecting bin afterbody connects gas cyclone device (6) and vacuum fan (5) by pipeline.
2. the preparation equipment of a kind of anhydrous magnesium chloride according to claim 1 is characterized in that described nozzle (13) is the linear pattern jet pipe, and the outlet aperture is 6mm.
3. the preparation method of an anhydrous magnesium chloride is characterized in that comprising the following steps:
(1) go into stove:
With magnesium chloride melt or solid is raw material, and it is added in the crucible (10), tightens the ring flange screw of crucible (10), and sealed crucible (10) hangs in electric furnace (9) with crucible (10) again;
(2) magnesium chloride fusing:
Electric furnace (9) send electricity, heating, fusing; Make the interior magnesium chloride melt temperature of crucible (10) be heated to 800～900 ℃;
(3) magnesium chloride transport pipe (8) and nozzle (13) are carried out ratio-frequency heating:
Making melt conveying pipeline (8) medial temperature is 790～810 ℃, and nozzle (13) temperature is 870～900 ℃;
(4) atomizing:
Open collecting bin (7) afterbody vacuum fan (5), the rare gas element with certain pressure intensity feeds in the crucible (10) again, and the pressure that rare gas element produces makes the interior magnesium chloride melt of crucible (10) along nozzle (13) ejection of melt conveying pipeline (8) by pipe end; Feed pressurized air simultaneously; Make the molten magnesium chloride atomization of liquid;
(5) collect and packing:
Magnesium chloride powder enters collecting bin (7) bottom, and the air communication of entrained fines is crossed the gas cyclone device (6) of collecting bin (7) afterbody, emptying after gathering dust; The board plug type that is provided with from collecting bin (7) bottom is collected mouthful (a 12) bottom and is emitted magnesium chloride powder, packs with plastic bag sealing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710078065A CN100586860C (en) | 2007-12-24 | 2007-12-24 | Preparation for anhydrous magnesium chloride powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710078065A CN100586860C (en) | 2007-12-24 | 2007-12-24 | Preparation for anhydrous magnesium chloride powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101279753A CN101279753A (en) | 2008-10-08 |
| CN100586860C true CN100586860C (en) | 2010-02-03 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200710078065A Expired - Fee Related CN100586860C (en) | 2007-12-24 | 2007-12-24 | Preparation for anhydrous magnesium chloride powder |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104828848B (en) * | 2015-04-17 | 2017-05-10 | 国家***天津海水淡化与综合利用研究所 | Preparation method for magnesium chloride particles |
| CN108516808B (en) * | 2018-07-10 | 2021-03-02 | 哈尔滨工业大学 | Method for preparing aluminum oxide-based nano eutectic composite micro powder by high-temperature melt aerosol method |
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| CN101279753A (en) | 2008-10-08 |
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Granted publication date: 20100203 Termination date: 20161224 |
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