CN102698650A - Bischofite double salt particle applicable to fluidization as well as preparation device and method of bischofite double salt particle - Google Patents
Bischofite double salt particle applicable to fluidization as well as preparation device and method of bischofite double salt particle Download PDFInfo
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- CN102698650A CN102698650A CN2012101541551A CN201210154155A CN102698650A CN 102698650 A CN102698650 A CN 102698650A CN 2012101541551 A CN2012101541551 A CN 2012101541551A CN 201210154155 A CN201210154155 A CN 201210154155A CN 102698650 A CN102698650 A CN 102698650A
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Abstract
The invention belongs to the technical field of particle preparation, and particularly relates to a bischofite double salt particle applicable to fluidization as well as the preparation device and method of the bischofite double salt particle. The device comprises a double salt synthesis system, a vibrating spraying system and a condensing forming system. The method comprises the following steps of: mixing bischofite with an intermediate auxiliary in a certain proportion and synthesizing double salt meltwater in the double salt synthesis system; forming double salt melted droplets by the vibrating spraying system; and preparing solid spherical double salt particles by the condensing forming system by air fluidifying cooling air. By using the device and the method, the bischofite double salt particle of which the grain diameter is from 50mu m to 1500mu m can be prepared, and the bischofite double salt particle is good in particle sphericity, high in hardness, even in size and suitable for fluidifying. The device can realize that double salt preparation and particle formation are simultaneously carried out in the same device, is low in energy consumption and high in production efficiency, can be coupled with the working procedures namely water removal and auxiliary removal in a fluidifying way, and can realize the requirement of the industrial production of magnesium chloride anhydrous.
Description
Technical field
The invention belongs to the granulate preparation technical field, be specifically related to a kind ofly be applicable to the bischofite double salt particle of fluidisation and be used to prepare described prilling granulator and the method that is applicable to the bischofite double salt particle of fluidisation.
Background technology
Magnesium is a kind of very important non-ferrous metal, and natural magnesium resource is mainly with bischofite (MgCl
26H
2O) form exists, and seawater, well mine salt bittern and salt lake bittern all contain a large amount of bischofites.The magnesium resource of China is very abundant, and the magnesium chloride reserves of Lop Nur salt lake bittern are 5.86 * 10
9Ton, Cha Er sweat salt lake magnesium chloride reserves are 1.65 * 10
9Ton.The electrolysis anhydrous magnesium chloride is the important method of producing magnesium metal, just can be used for producing magnesium metal behind the bischofite dehydration earlier formation anhydrous magnesium chloride, so dewatering bischofite has become a crucial ring in the magnesium resource utilization.Yet directly thermal dehydration is to anhydrous magnesium chloride usually for bischofite, and preceding four crystallizations water lose easily, but is prone to take place hydrolysis when latter two crystallization water is heated.Therefore it is most important to the exploitation of the western salt lake resources of reasonable utilization and China of magnesium resource how to prepare anhydrous magnesium chloride through dewatering bischofite.
Dewatering bischofite method commonly used mainly contains: the thermal dehydration method of gas shield, organic solvent distillation are decomposed evaporation etc. with molecular sieve dehydration method, double salt and complex compound.The thermal dehydration method of gas shield needs a large amount of hydrogen chloride gas or chlorine, and energy consumption is big, equipment seriously corroded under the high temperature.The organic solvent distillation needs multistep to separate with the molecular sieve dehydration method, and energy consumption is also big, and product impurity is many, and follow-up electrolysis is had adverse effect.At present, double salt or complex compound decomposition evaporation has excellent industrial application foreground.
Dolezal Henry is in U.S. Pat 3962408) in the method that proposes be a kind of double salt and decompose evaporation; This method utilizes auxiliary agent (like the hydrochloride of amines such as ethylenediamine, triethylamine, aniline) and bischofite to process double salt, and then heating sloughs the crystallization water successively and auxiliary agent obtains anhydrous magnesium chloride.This method does not produce HCl and NH
3Deng corrosive gas, and dehydration temperaturre low (≤350 ℃), therefore with the obvious advantage.Yet this patent does not have to propose concrete definite implementation method and appliance arrangement, does not see the R&D work of other bibliographical information this respect yet.
Mass-and heat-transfer efficient is high, occupation area of equipment is little because fluidization has, reduced investment, operation are convenient continuously, process is prone to advantages such as amplification; Being applied to more and more in recent years contain crystallization water inorganic salts pyrolytic process, also is to carry out the Perfected process that the double salt thermal decomposition prepares anhydrous magnesium chloride.Bischofite double salt is to obtain through the hot melting mixing reaction of bischofite and auxiliary agent, is the melt liquid state, for the dehydration of following adopted fluidization process with take off auxiliary agent, need the double salt of molten state be converted into the solid particle that is fit to fluidisation.Therefore, preparation size 50 μ m in 1500 mu m ranges and the bischofite double salt particle with certain intensity be the key of this process route.Yet prilling process resulting granules sphericities such as conventional extruded moulding, group's ball forming are poor, the ball size uneven, intensity is low, fluidisation is broken serious.In addition, because bischofite-amine hydrochloride characteristic is complicated, the method for employing mist projection granulating and crystallization granulation all is difficult to obtain being fit to the particle of fluidisation.
U.S. Pat 5266098 has proposed a kind of symmetrical liquid drop injecting technology that is applicable to the preparation metallic microspheres, and this method can be prepared the metallic particles of 10 ~ 500 μ m, but the application in the not mentioned other field of this method.
Chinese patent CN1212180C discloses a kind of prilling granulator and method of fused solution being processed the spheric granules product; This method changes into the drop form through distribution grid with liquation; Splash into then and carry out cooled and solidified in the cooling medium, finally can access the spherical particle that grain size is 1 ~ 10mm, this method has obtained success in granular urea and paraffin particles aspect preparing; But limited because of the distribution grid distribution capability, can't prepare the following particle of 1mm than low dimensional.
To the problem of above-mentioned existence, therefore need be applicable to the bischofite double salt particle of fluidisation in the practice, and preparation is applicable to the prilling granulator and the method for the bischofite double salt particle of fluidisation.
Summary of the invention
The objective of the invention is to propose a kind ofly be applicable to the bischofite double salt particle of fluidisation and be used to prepare described prilling granulator and the method that is applicable to the bischofite double salt particle of fluidisation.
Preparation of the present invention is applicable to that the device of the bischofite double salt particle of fluidisation is made up of double salt synthesis system, vibration jet system and condensation formation system three parts, specifically describes as follows:
(1) double salt synthesis system: described double salt synthesis system comprises heating furnace 11, reactor 12, nitrogen making machine 13 and agitator 14; Be connected with pressure maintaining valve 16 with stainless steel pipeline 15 between described reactor 12 and the nitrogen making machine 13; Seal by gathering polytetrafluoroethylsealed sealed circle between described reactor 12 and the agitator 14;
(2) vibration jet system: described vibration jet system comprises signal generator 21, signal amplifier 22, vibrator 23, syringe needle 24, guide rod 25 and disk 26; Described guide rod 25 upper ends and described vibrator 23 are rigidly connected, and described guide rod 25 lower ends and disk 26 are rigidly connected, and a plurality of syringe needles 24 distribute on the described disk 26; Described reactor 12 through valve 28, gather tetrafluoro conduit 27 and 24 non-rigid connections of syringe needle, double salt fused solution flow is through at described reactor 12 with gather valve 28 control between the tetrafluoro conduit 27; Wherein, described syringe needle 24, guide rod 25, disk 26, gather tetrafluoro conduit 27 and valve 28 is positioned at heating furnace 11; Signal generator 21, signal amplifier 22 and vibrator 23 are positioned at outside the heating furnace 11;
(3) condensation formation system: described condensation moulding system bits comprises air compressor 31, tower body 32, gas distribution grid 33, discharging opening 34 and gate valve 35 under described vibration jet system (both can not have connection); The cold air that described air compressor 31 produces gets into tower body 32 through the cool air inlet of described tower body 32 lower ends; Contact with double salt fused solution drop through described gas distribution grid 33 then, thereby described double salt fused solution drop cooling is formed solid spherical double salt particle; The discharging opening 34 that described solid spherical double salt particle is left from tower body 32 lower side takes out, and the switching of described discharging opening 34 is by gate valve 35 controls.
All scribble heat insulating coating on described gas distribution grid 33, guide rod 25, disk 26 and tower body 32 surfaces.The height of the tower body 32 in the described condensation formation system is at 0.5m ~ 3m.
The concrete preparation process that a kind of device that uses above-mentioned preparation to be applicable to the bischofite double salt particle of fluidisation that the present invention proposes prepares the bischofite double salt particle that is applicable to fluidisation comprises the steps:
The nitrogen of nitrogen making machine 13 outputs passes through stainless steel pipeline 15 and pressure maintaining valve 16, and behind the certain pressure that forms under the control of pressure maintaining valve 16, gets into reactor 12; The described nitrogen compressing double salt fused solution that has a certain pressure through valve 28 with gather tetrafluoro conduit 27 and spray from syringe needle 24; Signal generator 21 sends the vibration signal of certain frequency; After signal amplifier 22 amplifications; Driving vibrator 23 and disk 26 vibrates with correspondent frequency; Described vibration makes the double salt fused solution droplet that forms certain grain size from the double salt fused solution of syringe needle 24 injections, and described double salt fused solution droplet is spherical under capillary effect;
The also available device that other produces nitrogen of described nitrogen making machine 13 substitutes, such as commercial canned nitrogen.
The building-up process of bischofite double salt particle can adopt one, 12 couplings of the reactor more than two or two.
The present invention combines existing symmetrical liquid drop injecting technology; Replace distribution grid with medical needle; Introduce vibration signal; Propose a kind of symmetrical liquid drop vibration jet technology and device, can make particle diameter is the spherical bischofite double salt particle of 50 μ m ~ 1500 μ m, thereby is applicable to follow-up fluidization dehydration.This granulating technique is applicable to the cooling curing granulation of higher melt material, the factor of consideration equipment and pipeline insulation and tower height, and this method is specially adapted to the granulation of 200 ℃ of fusing points ~ 450 ℃ of materials.
Beneficial effect of the present invention is:
(1) the used process unit of the present invention has realized that double salt preparation, double salt grain forming accomplish in same device, and equipment is simple, and is easy to operate, and energy consumption is low, can large-scale production;
(2) the prepared double salt pellet hardness of the present invention is big, sphericity is high, be evenly distributed, and can satisfy the needs of follow-up fluidization process;
(3) because the evenly cooling in cold air of double salt fused solution droplet can not stick together between the solid spherical double salt particle, can directly transmit, thereby can dewater, take off the coupling of auxiliary agent operation with next step fluidization through conveyer belt.
Description of drawings
Fig. 1 is bischofite double salt particle granulating device structure and the schematic flow sheet that the present invention proposes.
Fig. 2 is the product photo of the embodiment of the invention 1, and prepared solid spherical bischofite double salt grain diameter is 600 μ m ~ 900 μ m.
The specific embodiment
The beginning of above-mentioned granulation and stopping to be to control through the opening and closing of valve 28.The aperture synthesis of stable nitrogen gas pressure size that pressure maintaining valve 16 provides, vibration frequency that signal generator 21 provides and syringe needle 24 has determined the double salt particle grain size that makes; Wherein the stable nitrogen gas pressure limit that provides of pressure maintaining valve 16 is 0.1Pa-10MPa; The vibration frequency range that signal generator 21 provides is 20Hz-1500Hz; A plurality of syringe needles 24 that on disk 26, can distribute, the syringe needle internal diameter is 40 μ m ~ 1600 μ m.
Embodiment:
1. syringe needle 24 internal diameters are that the vibration frequency that 400 μ m, signal generator 21 provide is 100Hz; When the stable nitrogen gas pressure that pressure maintaining valve 16 provides was controlled at 0.5MPa, can obtain particle diameter was solid spherical bischofite-aniline hydrochloride double salt particle of 600 μ m ~ 900 μ m.The solid spherical bischofite that makes-aniline hydrochloride double salt grain products does not contain dust, pellet hardness is big, sphericity is high, be evenly distributed, fluidized state is good.Its granulation product such as Fig. 2.
2. syringe needle 24 internal diameters are that the vibration frequency that 800 μ m, signal generator 21 provide is 50Hz; When the stable nitrogen gas pressure that pressure maintaining valve 16 provides was controlled at 0.4MPa, can obtain particle diameter was solid spherical bischofite-aniline hydrochloride double salt particle of 1000 μ m ~ 1500 μ m.
3. syringe needle 24 internal diameters are that the vibration frequency that 100 μ m, signal generator 21 provide is 400Hz; When the stable nitrogen gas pressure that pressure maintaining valve 16 provides was controlled at 0.7MPa, can obtain particle diameter was solid spherical bischofite-aniline hydrochloride double salt particle of 50 μ m ~ 200 μ m.
Used signal generator 21 is contained general instrument Science and Technology Ltd. by Nanjing and is produced in the foregoing description, and model is the SP1641B type; Signal amplifier 22 is produced by Beijing vibration measuring instrument plant, and model is GF-20; Vibrator 23 is produced by Beijing vibration measuring instrument plant; Nitrogen making machine 31 is by becoming space flight air separation plant Co., Ltd to produce in Beijing, model is CanGas.
Claims (9)
1.. a device for preparing the bischofite double salt particle that is applicable to fluidisation is characterized in that described device comprises double salt synthesis system, vibration jet system and condensation formation system:
1) double salt synthesis system: described double salt synthesis system comprises heating furnace (11), reactor (12), nitrogen making machine (13) and agitator (14); Be connected with pressure maintaining valve (16) with stainless steel pipeline (15) between described reactor (12) and the nitrogen making machine (13); Seal by gathering polytetrafluoroethylsealed sealed circle between described reactor (12) and the agitator (14);
2) vibration jet system: described vibration jet system comprises signal generator (21), signal amplifier (22), vibrator (23), syringe needle (24), guide rod (25) and disk (26); Described guide rod (25) upper end and described vibrator (23) are rigidly connected, and described guide rod (25) lower end and disk (26) are rigidly connected, and described disk (26) is gone up a plurality of syringe needles (24) that distribute; Described reactor (12) through valve (28), gather tetrafluoro conduit (27) and non-rigid connection of syringe needle (24), double salt fused solution flow is through being positioned at described reactor (12) and gathering valve (28) control between the tetrafluoro conduit (27); Wherein, described syringe needle (24), guide rod (25), disk (26), gather tetrafluoro conduit (27) and valve (28) is positioned at heating furnace (11); Signal generator (21), signal amplifier (22) and vibrator (23) are positioned at outside the heating furnace (11);
3) condensation formation system: described condensation moulding system bits comprises air compressor (31), tower body (32), gas distribution grid (33), discharging opening (34) and gate valve (35) under described vibration jet system; The cold air that described air compressor (31) produces gets into tower body (32) through the cool air inlet of described tower body (32) lower end; Contact with double salt fused solution drop through described gas distribution grid (33) then, thereby described double salt fused solution drop cooling is formed solid spherical double salt particle; The discharging opening (34) that described solid spherical double salt particle is left from tower body (32) lower side takes out, and the switching of described discharging opening (34) is controlled by gate valve (35).
2. preparation according to claim 1 is applicable to the device of the bischofite double salt particle of fluidisation, it is characterized in that, goes up a plurality of syringe needles (24) that distribute at described disk (26), and the syringe needle internal diameter is 40 μ m ~ 1600 μ m.
3. preparation according to claim 1 is applicable to the device of the bischofite double salt particle of fluidisation, it is characterized in that, the tower body of described condensation formation system (32) highly is 0.5m ~ 3m.
4. a prilling process for preparing the bischofite double salt particle that is applicable to fluidisation is characterized in that described prilling process comprises the steps:
Open heating furnace (11), make the temperature in the reactor (12) rise to 120 ℃ ~ 200 ℃; In described reactor (12), add bischofite and intermediate auxiliary agent according to certain ratio; Open agitator (14), described bischofite and intermediate auxiliary agent react under the stirring action of agitator (14) and form the double salt fused solution; Described double salt fused solution through valve (28), gather tetrafluoro conduit (27), is sprayed by syringe needle (24) under the stable nitrogen pressure effect that pressure maintaining valve (16) provides; By signal generator (21) vibration signal is provided, after signal amplifier (22) amplifies, drives vibrator (23) vibration, described vibration reaches disk (26) through guide rod (25) again, and disk (26) drives syringe needle (24) and produces vibration accordingly; Under the vibration interference of syringe needle (24), be dispersed into the even double salt fused solution droplet of certain grain size by the double salt fused solution of syringe needle (24) injection; The cool air inlet of cold air through tower body (32) lower end that is provided by air compressor (31) gets into tower body (32), after gas distribution grid (33) disperses, described double salt fused solution droplet cooled off again; Described double salt fused solution droplet becomes solid spherical double salt particle through the chilled air cools after coagulation, drops on the described gas distribution grid (33); Described solid spherical double salt particle takes out through the discharging opening (34) that is positioned at tower body (32) lower side, and the switch of described discharging opening (34) is controlled by gate valve (35).
5. preparation according to claim 4 is applicable to the prilling process of the bischofite double salt particle of fluidisation, it is characterized in that, described intermediate auxiliary agent is the amine hydrochloride, and the amount of substance of intermediate auxiliary agent and bischofite is than being 1:2 ~ 2:1.
6. preparation according to claim 4 is applicable to the prilling process of the bischofite double salt particle of fluidisation, it is characterized in that the beginning of described granulation and to stop be that opening and closing through ball valve (28) are controlled.
7. preparation according to claim 4 is applicable to the prilling process of the bischofite double salt particle of fluidisation; It is characterized in that the stable nitrogen gas pressure size that described bischofite double salt particle grain size is provided by nitrogen stabilization pressure valve (16), the vibration frequency that signal generator (21) provides and the aperture synthesis decision of syringe needle (24); The bischofite double salt particle grain size scope of preparation is 50 μ m ~ 1500 μ m.
8. preparation according to claim 4 is applicable to the prilling process of the bischofite double salt particle of fluidisation, it is characterized in that, the stable nitrogen gas pressure limit that described pressure maintaining valve (16) provides is 0.1MPa ~ 10MPa; The frequency range of the vibration signal that described signal generator (21) provides is 20Hz ~ 1500Hz.
9. preparation according to claim 4 is applicable to the prilling process of the bischofite double salt particle of fluidisation, it is characterized in that, the building-up process of described bischofite double salt particle adopts one, two or two above reactors (12) coupling.
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| CN2012101541551A CN102698650A (en) | 2012-05-17 | 2012-05-17 | Bischofite double salt particle applicable to fluidization as well as preparation device and method of bischofite double salt particle |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103274433A (en) * | 2013-05-13 | 2013-09-04 | 清华大学 | Recovery method and device for bischofite dehydration assistant by double salt method |
| CN109126625A (en) * | 2018-10-23 | 2019-01-04 | 昆明尔康科技有限公司 | A kind of sprinkling pelleting device |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5266098A (en) * | 1992-01-07 | 1993-11-30 | Massachusetts Institute Of Technology | Production of charged uniformly sized metal droplets |
| CN2683240Y (en) * | 2003-05-08 | 2005-03-09 | 武汉化工学院 | Spray column-fluidized bed pelletizer |
| CN1944261A (en) * | 2006-11-06 | 2007-04-11 | 清华大学 | Process for preparing anhydrous magnesium chloride by dewatering bischofite |
-
2012
- 2012-05-17 CN CN2012101541551A patent/CN102698650A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5266098A (en) * | 1992-01-07 | 1993-11-30 | Massachusetts Institute Of Technology | Production of charged uniformly sized metal droplets |
| CN2683240Y (en) * | 2003-05-08 | 2005-03-09 | 武汉化工学院 | Spray column-fluidized bed pelletizer |
| CN1944261A (en) * | 2006-11-06 | 2007-04-11 | 清华大学 | Process for preparing anhydrous magnesium chloride by dewatering bischofite |
Non-Patent Citations (1)
| Title |
|---|
| 杨金鑫，党杰，吴玉龙，杨明德，袁建军，多尼: "流化床脱水制无水氯化镁工艺研究", 《盐业与化工》, vol. 41, no. 4, 30 April 2012 (2012-04-30), pages 10 - 15 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103274433A (en) * | 2013-05-13 | 2013-09-04 | 清华大学 | Recovery method and device for bischofite dehydration assistant by double salt method |
| CN103274433B (en) * | 2013-05-13 | 2018-07-24 | 清华大学 | The recovery method and device of double salt method dewatering bischofite auxiliary agent |
| CN109126625A (en) * | 2018-10-23 | 2019-01-04 | 昆明尔康科技有限公司 | A kind of sprinkling pelleting device |
| CN109126625B (en) * | 2018-10-23 | 2020-12-22 | 昆明尔康科技有限公司 | Spray granulation device |
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Inventor after: Wu Yulong Inventor after: Liu Ji Inventor after: Song Yinghua Inventor after: Li Shoujiang Inventor after: Yang Mingde Inventor after: Lei Guangyuan Inventor after: Ni Qianyin Inventor after: Yao Mobai Inventor after: Dang Jie Inventor after: Hu Husheng Inventor after: Chen Zhen Inventor before: Wu Yulong Inventor before: Yang Mingde Inventor before: Ni Qianyin Inventor before: Dang Jie Inventor before: Hu Husheng Inventor before: Chen Zhen Inventor before: Liu Ji Inventor before: Song Yinghua |
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Free format text: CORRECT: INVENTOR; FROM: WU YULONG YANG MINGDE NI QIANYIN DANG JIE HU HUSHENG CHEN ZHEN LIU JI SONGYINGHUA TO: WU YULONG LI SHOUJIANG YANG MINGDE LEI GUANGYUAN NI QIANYIN YAO MOBAI DANG JIE HU HUSHENG CHEN ZHEN LIU JI SONG YINGHUA |
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Effective date of registration: 20140811 Address after: 100084 Beijing, Beijing, 100084-82 mailbox Applicant after: Tsinghua University Applicant after: SDIC Xinjiang Luobupo Potash Co., Ltd. Address before: 100084 Beijing, Beijing, 100084-82 mailbox Applicant before: Tsinghua University |
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