CN106365174B - The process units and production method of xrf analysis high-purity high-density degree lithium borate - Google Patents

The process units and production method of xrf analysis high-purity high-density degree lithium borate Download PDF

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CN106365174B
CN106365174B CN201610729752.0A CN201610729752A CN106365174B CN 106365174 B CN106365174 B CN 106365174B CN 201610729752 A CN201610729752 A CN 201610729752A CN 106365174 B CN106365174 B CN 106365174B
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atomization
purity
lithium borate
centrifugal atomizing
atomizing disk
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CN106365174A (en
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班文俊
蔡荣富
孟强
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KAIFEI HIGH ENERGY CHEM INDUCTRY CO Ltd CHENGDU CITY
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KAIFEI HIGH ENERGY CHEM INDUCTRY CO Ltd CHENGDU CITY
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B35/00Boron; Compounds thereof
    • C01B35/08Compounds containing boron and nitrogen, phosphorus, oxygen, sulfur, selenium or tellurium
    • C01B35/10Compounds containing boron and oxygen
    • C01B35/12Borates
    • C01B35/121Borates of alkali metal
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/22Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
    • G01N23/223Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/10Solid density
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

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  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)

Abstract

The invention discloses the xrf analysis process units and production method of high-purity high-density degree lithium borate, described device includes feeding unit, melting unit, atomization unit, collector unit and atomization and collects tower;Feeding unit includes the magazine and charger that communicate with each other;Melting unit includes the electric furnace with several heating elements and the crucible being arranged in electric furnace, and the bottom of crucible is connected with tremie pipe;Atomization unit is arranged on atomization and collects in tower, and atomization unit includes centrifugal atomizing disk, centrifugal atomizing disk installation shaft, electromagnetic induction heater and high-speed electric expreess locomotive;Collector unit includes funnel-form loading head and collection vessel, and the funnel-form loading head collects tower integrally connected and positioned at the lower section of atomization unit with atomization, and collection vessel is arranged on the lower section of the discharge port of funnel-form loading head.The production method carries out the production of xrf analysis high-purity high-density degree lithium borate using above device.

Description

The process units and production method of xrf analysis high-purity high-density degree lithium borate
Technical field
The present invention relates to technical fields prepared by xrf analysis fluxing agent, more particularly, are related to xrf analysis height The process units and production method of pure high density lithium borate.
Background technology
With the development of X-ray fluorescence spectra (XRF) analytical technology, borate melting prepares sample technology because it has soon It the characteristics of speed, high accuracy, finds broad application in industries such as cement, ceramics, smeltings.Common borate is mainly alkali metal The easy moisture absorption of fuse piece made of the borate of lithium, the borate of sodium but sodium cannot analyze the sodium in sample, the absorption to X ray Than containing the shortcomings of lithium flux is big, at present substantially by the borate of lithium such as lithium tetraborate, lithium metaborate and both by certain ratio The lithium borate mixed flux of example is replaced.
Lithium atom is small in the borate salt system of lithium to be arrived by X-ray detection, because without the fluorescence Spectra to analytical element Line generates interference.Lithium tetraborate in the borate of lithium is a kind of faintly acid flux, can mutually be melted with basic sample solution;Lithium metaborate is A kind of basic solvent can mutually be melted with acidic sample;For in cement, steel industry sample, often simultaneously comprising acidic oxide and Basic anhydride are unable to reach the effect for melting oxide in sample completely using only lithium tetraborate or lithium metaborate, and The mixed flux mixed using the lithium tetraborate and lithium metaborate of different proportion can effectively neutralize different in sample at high temperature Acid-base properties of oxides makes sample melted reach the uniform state of molecular level, so as to be stablized, uniformly melts sample sheet glass, Achieve the purpose that detection.
Lithium borate fusion technology has the advantages such as sample preparation is uniform, with high accuracy, the period is short, analysis cost is low, by state Inside and outside assay laboratory uses.With the raising of analysis automated level, abroad melts sample process using automation at present Operation claims sample, auto feed automatically, this proposes higher requirement to the particle uniformity of xrf analysis reagent and mobility. At present, high density xrf analysis is mainly high-temperature melting method with the production method of lithium borate flux:By lithium tetraborate, metaboric acid Lithium or lithium carbonate obtain lithium borate flux with boric acid as raw material, through the processes such as high temperature melting, quenching, broken, screening.The method The utensil that the chemical index of product relies on the purity of raw material and uses, is easily made high-purity using high-purity raw material and platinum utensil Degree, Song dress Mi Du≤1.0g/cm3Product, foreign countries' xrf analysis lithium borate fluxing agent is largely method production at present Product.
After domestic patent CN102838125.A is purified respectively using lithium hydroxide in industrial grade and technical grade boric acid, in proportion By the lithium hydroxide of purification and boric acid neutralization reaction, reaction solution is concentrated into after whitening and pours into stainless steel disc and be evaporated, crush, is secondary Drying obtains lithium tetraborate powder, in 930~950 DEG C of high-temperature fusions 4~5 hours, water quenching cold cut, then dries to obtain high density boron Sour crystalline lithium, the technological process is complicated, and batch is small, it is most important that the impurity of raw material will all remain on production in the process route Product, product purity are extremely difficult to the requirement of xrf analysis reagent.
Invention content
In order to solve the problems in the existing technology, the object of the present invention is to provide one kind can high temperature, high rotating speed, Continuous production is realized under the conditions of high corrosion, without crushing or crushing and disclosure satisfy that xrf analysis high-purity high-density degree boric acid The process units and production method of lithium.
An aspect of of the present present invention provides the process units of xrf analysis high-purity high-density degree lithium borate, described to prepare dress It puts and collects tower including feeding unit, melting unit, atomization unit, collector unit and atomization;
Feeding unit includes the magazine and charger that communicate with each other;Melting unit includes having several heating elements Electric furnace and the crucible that is arranged in electric furnace, the bottom of crucible is connected with tremie pipe, several described heating elements Ring is located at the surrounding of crucible and tremie pipe, wherein, the discharge port of charger is arranged on the top or direct of the feed inlet of crucible It is connect with the feed inlet of crucible;
Atomization unit is arranged on atomization and collects in tower, atomization unit includes centrifugal atomizing disk, centrifugal atomizing disk installs shaft, Electromagnetic induction heater and high-speed electric expreess locomotive, centrifugal atomizing disk are mounted on the top of centrifugal atomizing disk installation shaft, centrifugal atomizing disk Installation shaft is connect with high-speed electric expreess locomotive, and electromagnetic induction heater is installed around centrifugal atomizing disk is arranged in shaft and close to centrifugation Atomizing disk is set, wherein, the discharge port of the tremie pipe of melting unit is also disposed at atomization and collects in tower and positioned at centrifugal atomizing The surface of disk;
Collector unit includes funnel-form loading head and collection vessel, and funnel-form loading head is arranged on the lower section of atomization unit, Collection vessel is arranged on the lower section of the discharge port of funnel-form loading head.
According to xrf analysis of the present invention one embodiment of the process units of high-purity high-density degree lithium borate, the feeding Unit further includes auto feed control system, what the auto feed control system was fed by the height of melt in crucible It automatically controls;The process units further includes control system, and the control system controls the action of entire process units.
According to xrf analysis of the present invention one embodiment of the process units of high-purity high-density degree lithium borate, the crucible For platinum yellow crucible, the heating element is Elema or Si-Mo rod.
According to xrf analysis of the present invention one embodiment of the process units of high-purity high-density degree lithium borate, the centrifugation Atomizing disk is platinum yellow centrifugal atomizing disk, and the centrifugal atomizing disk installation shaft is high temperature alloy centrifugal atomizing disk installation axle.
According to xrf analysis of the present invention one embodiment of the process units of high-purity high-density degree lithium borate, the atomization Unit further includes the bearing being arranged on the high-speed electric expreess locomotive and the motor protecting cover for accommodating the high-speed electric expreess locomotive and bearing, described Centrifugal atomizing disk installation shaft is arranged in the centre bore of the bearing and is rotatably coupled by bearing and the bearing.
According to xrf analysis of the present invention one embodiment of the process units of high-purity high-density degree lithium borate, the collection Unit further includes the hydraulic elevator platform for placing the collection vessel.
Another aspect provides a kind of xrf analysis production methods of high-purity high-density degree lithium borate, use Above-mentioned xrf analysis carries out the life of xrf analysis high-purity high-density degree lithium borate with the process units of high-purity high-density degree lithium borate Production, the production method include the following steps:
The raw material stored in feeding unit is sent into the crucible of melting unit;
The raw material in the crucible is heated to 1200~1350 DEG C by electric furnace and obtains melt;
The melt is made to be flowed out by tremie pipe and flows to the centrifugation mist that rotating speed in atomization unit is 5000~30000rmp Change panel surface to be atomized;
By the atomization melt drop that centrifugal atomizing disk is thrown away cools down in tower and collector unit are collected in atomization, collection obtains institute State xrf analysis high-purity high-density degree lithium borate;
Wherein, the raw material is high-purity hydrated lithium borate, high-pure anhydrous lithium borate or high-purity boracic acid and pure Lithium Carbonate Mixture.
According to xrf analysis of the present invention one embodiment of the production method of high-purity high-density degree lithium borate, pass through electromagnetism The surface temperature of centrifugal atomizing disk is 800~900 DEG C during sensing heater control atomization.
It is described high-purity according to xrf analysis of the present invention one embodiment of the production method of high-purity high-density degree lithium borate Lithium borate or high-pure anhydrous lithium borate are hydrated as lithium tetraborate, lithium metaborate or lithium tetraborate and the mixture of lithium metaborate.
According to xrf analysis of the present invention one embodiment of the production method of high-purity high-density degree lithium borate, the X-fluorescence The purity of analysis high-purity high-density degree lithium borate is more than 99.99%, and density is 1.2~1.4g/cm3, granularity is 200~600 micro- Rice.
Compared with prior art, the production method of xrf analysis high-purity high-density degree lithium borate of the present invention and device can Continuous production is realized under the conditions of high temperature, high rotating speed, high corrosion, without broken or crushing, the high density lithium borate energy produced Enough meet the requirement of xrf analysis.Product apparent density height, good fluidity, particle are uniform, self raising flour dirt, meet it is automatic claim sample, from Dynamic charging is to lithium borate quality requirement.
Description of the drawings
Fig. 1 shows the production dress of xrf analysis high-purity high-density degree lithium borate according to an exemplary embodiment of the present invention The structure diagram put.
Fig. 2 shows the production dresses of xrf analysis according to an exemplary embodiment of the present invention high-purity high-density degree lithium borate Put the structure diagram of middle melting unit.
Fig. 3 shows the production dress of xrf analysis high-purity high-density degree lithium borate according to an exemplary embodiment of the present invention Put the structure diagram of middle atomization unit.
Reference sign:
10- feeding units, 11- magazines, 12- chargers, 20- melting units, 21- crucibles, 22- electric furnaces, 23- Heating element, 24- tremie pipes, 30- atomization units, 31- centrifugal atomizings disk, 32- centrifugal atomizings disk installation shaft, 33- electromagnetism senses Answer heater, 34- motor shafts, 35- high-speed electric expreess locomotives, 36- bearings, 37- motor protecting covers, 38- bearings, 40- atomization collect tower, 50- collector units, 51- funnel-forms loading head, 52- collection vessels, 60- hydraulic elevator platforms.
Specific embodiment
All features or disclosed all methods disclosed in this specification or in the process the step of, in addition to mutually exclusive Feature and/or step other than, can combine in any way.
Any feature of this disclosure, unless specifically stated, can or replacing with similar purpose equivalent by other It is replaced for feature.That is, unless specifically stated, each feature be an example in a series of equivalent or similar characteristics and .
The present invention is actually lithium borate (such as lithium tetraborate, lithium metaborate or two for being directly based upon and being prepared The mixed solvent that person mixes according to a certain ratio) or boric acid based on stoichiometric ratio and 200~300 DEG C of lithium carbonate low temperature it is low The mixture that warm solid phase reaction obtains for 3~5 hours carries out the preparation of high density lithium borate microballon, it is made to be more applicable for X-fluorescence Analysis.Wherein, the above-mentioned lithium borate being prepared may be used method of the prior art and be made, such as may be used Prepared by method disclosed in CN104016358B, the present invention is not limited thereto.
First have below to the structure and principle of the xrf analysis of the present invention process units of high-purity high-density degree lithium borate Body explanation.
Fig. 1 shows the production dress of xrf analysis high-purity high-density degree lithium borate according to an exemplary embodiment of the present invention The structure diagram put, Fig. 2 shows xrf analysis according to an exemplary embodiment of the present invention high-purity high-density degree lithium borates The structure diagram of melting unit in process units, Fig. 3 show that xrf analysis according to an exemplary embodiment of the present invention is high The structure diagram of atomization unit in the process units of pure high density lithium borate.
As shown in Figure 1, exemplary embodiment according to the present invention, xrf analysis high-purity high-density degree lithium borate Process units includes feeding unit 10, melting unit 20, atomization unit 30, collector unit 50 and atomization and collects tower 40.Wherein, it send For raw material to be stored and conveyed, melting unit 20 is used to melt raw material molten with what is melted material unit 10 Body, atomization unit 30 are used to carry out atomization process to melt to obtain spherical lithium borate microballon, and collector unit 50 is used to collect The high density lithium borate being prepared, atomization collect tower 40 and are used to form atomization process and collect the confined space of processing.
Specifically, feeding unit 10, which includes the magazine 11 to communicate with each other and charger 12, charger 12, will store up Of short duration storage or the raw material stored for a long time are sent to melting unit 20 in material container 11.Preferably, feeding unit can also be included certainly Dynamic Loading Control System (not shown), auto feed control system can be fed by the height of melt in crucible 21 from Dynamic control, such as infrared range-measurement system may be used or radar range finder judges the height of melt in crucible.
As shown in Fig. 2, melting unit 20 includes the electric furnace 22 with several heating elements 23 and is arranged on electric add Crucible 21 in hot stove 22, the bottom of crucible 21 are connected with tremie pipe 24, several 23 rings of heating element are located at crucible 21 under The surrounding of expects pipe 24, wherein, the discharge port of charger 12 be arranged on the feed inlet of crucible 21 top or directly with crucible 21 Feed inlet connection.Wherein, since lithium borate melt has corrosion function to the other materials in addition to platinum at high temperature, in order to protect The quality of product is demonstrate,proved, therefore platinum yellow material is used with the position of melt contacts in melt unit, then crucible 21 is preferably platinum yellow Crucible.In addition, heating element 23 is preferably Elema or Si-Mo rod, to reach 1200 DEG C or more of heating temperature.
As shown in figures 1 and 3, atomization unit 30 and collector unit 50 be arranged at atomization collect tower 40 in, with formed compared with For closed atomization and collection space.Wherein, atomization unit 30 includes centrifugal atomizing disk 31, centrifugal atomizing disk installs shaft 32, Electromagnetic induction heater 33 and high-speed electric expreess locomotive 35, centrifugal atomizing disk 31 are mounted on the top of centrifugal atomizing disk installation shaft 32, example The top of centrifugal atomizing disk installation shaft 32, centrifugal atomizing disk installation shaft 32 and high speed can be such as fixed on by riveting method Motor 35 is connected and (is connected by motor shaft 34), and thus centrifugal atomizing disk installation shaft 32 can be in high-speed electric expreess locomotive 35 and motor shaft High speed rotation and 32 high speed rotation of centrifugal atomizing disk is driven under 34 drive;Electromagnetic induction heater 33 surrounds and is arranged on centrifugation mist Change in disk installation shaft 32 and set close to centrifugal atomizing disk 31 so that centrifugal atomizing disk 31 keep certain temperature and ensure plus Work efficiency fruit.Wherein, the discharge port of the tremie pipe 24 of melting unit 20 is also disposed at atomization and collects in tower 40 and positioned at centrifugation mist Change the top of disk 31, so that melt accurately can controllably fall in the upper surface of centrifugal atomizing disk 31 and realize atomization.
Similarly, since lithium borate is fluxing agent, particularly lithium borate melt is at high temperature to other materials in addition to platinum Matter has corrosion function, in order to ensure the quality of product, therefore also preferably uses platinum with the component of melt contacts in atomization unit Yellow material.If but if entire rotary shaft uses platinum yellow material, just not saying it is of high cost, mainly in electromagnetic induction heating process The mechanical property of middle material does not reach requirement, therefore the present invention selects material of the high temperature alloy as rotary shaft, and on the rotary shaft The centrifugal atomizing disk of platinum yellow material is installed, efficiently solves the above problem.Specifically, centrifugal atomizing disk 31 is preferably platinum yellow alloy Centrifugal atomizing disk, centrifugal atomizing disk installation shaft 32 is preferably high temperature alloy centrifugal atomizing disk installation axle.
In order to ensure the stability of atomization unit, atomization unit 30 further includes 36 He of bearing being arranged on high-speed electric expreess locomotive 35 The motor protecting cover 37 of high-speed electric expreess locomotive 35 and bearing 36 is accommodated, centrifugal atomizing disk installation shaft 32 is arranged on the centre bore of bearing 36 In and be rotatably coupled by bearing 38 and bearing 36, centrifugal atomizing disk installation shaft is mainly stablized in the effect of bearing 36 32 and its shaking during running at high speed is limited, centrifugal atomizing disk installation shaft 32 is connect simultaneously by keyway with motor shaft 34 And centrifugal atomizing disk 31 is driven to rotate under the rotation of motor shaft, so that the high-speed rotation of centrifugal atomizing disk 31 is more flat Surely, the quality of final products is helped to ensure that.
Collector unit 50 includes funnel-form loading head 51 and collection vessel 52, and funnel-form loading head 51 is arranged on atomization unit 30 lower section, collection vessel 52 are arranged on the lower section of the discharge port of funnel-form loading head 51.Wherein, funnel-form loading head 51 can be with Tower 40 is collected with atomization to be wholely set, and can also be provided separately within atomization and be collected in tower 40.As shown in Figure 1, funnel-form loading head The feed inlet of 51 upper ends is bigger and the discharge port of lower end is smaller, and thus it can effectively throw away centrifugal atomizing disk 31 Lithium borate microballon is collected and is collected in the collection vessel 52 of lower section.In addition, collector unit 50 can also include receiving for placing Collect the hydraulic elevator platform 60 of container 52, to facilitate the height and position of adjustment collection vessel 52.
According to the present invention, in order to realize the automation of production, process units of the invention can also include control system with The action of entire process units is controlled, which may be used the control system of this field routine, and the present invention is not This is defined.
The present invention additionally provides the production method of xrf analysis high-purity high-density degree lithium borate simultaneously, specifically using upper State the production that xrf analysis carries out xrf analysis high-purity high-density degree lithium borate with the process units of high-purity high-density degree lithium borate.
Exemplary embodiment according to the present invention, the production method include following multiple steps:
First, the raw material stored in feeding unit 10 is sent into the crucible 21 of melting unit 20.Wherein, the present invention uses Raw material be high-purity hydrated lithium borate (99.99%), high-pure anhydrous lithium borate (99.99%) or high-purity boracic acid (99.99%) With the mixture of pure Lithium Carbonate (99.99%), so as to ensure the high-purity of final products, specifically, above-mentioned high-purity hydrated boron Sour lithium or high-pure anhydrous lithium borate all can be lithium tetraborate, lithium metaborate or lithium tetraborate and lithium metaborate different proportions Mixture.
Secondly, the raw material in crucible 21 is heated to 1200~1350 DEG C by electric furnace 22 and obtains melt.
Again, make melt pass through tremie pipe 24 flow out and flow to rotating speed in atomization unit 30 be 5000~30000rmp from 31 surface of heart atomizing disk is atomized.Wherein, in order to ensure atomization quality, when need to control atomization by electromagnetic induction heater 32 The surface temperature of centrifugal atomizing disk 31 is 800~900 DEG C.During control atomization centrifugal atomizing disk 31 surface temperature primarily to The rate of temperature fall of lithium borate melt is controlled, ensures the viscosity and mobility of melt, improves atomization balling ratio, if temperature is low, melt Easy formation filiform during viscosity high atomization.
Finally, it is the atomization melt drop that centrifugal atomizing disk 31 is thrown away is cold in tower 40 and collector unit 50 are collected in atomization But it, collects and obtains xrf analysis high-purity high-density degree lithium borate.Wherein, the xrf analysis that is prepared of the present invention is with high-purity high The purity of density lithium borate is more than 99.99%, and density is 1.2~1.4g/cm3, and granularity is 200~600 microns.
It should be understood that the above embodiment and following embodiment that the present invention is described in detail are merely to illustrate the present invention rather than limit The scope of the present invention processed, some nonessential improvement and tune that those skilled in the art's the above according to the present invention is made It is whole to all belong to the scope of protection of the present invention.Following specific parameters of example etc. are also only an examples in OK range, i.e., originally Field technology personnel can be done in suitable range by the explanation of this paper and be selected, and not really want to be defined in the tool of Examples below Body numerical value.
With reference to specific embodiment, the invention will be further described.
Embodiment 1:
By high-pure anhydrous lithium tetraborate powder storage in the magazine 11 of feeding unit 10, charger is opened by raw material It is sent into the crucible 21 of melting unit 20.The raw material in crucible 21 is heated to 1300 DEG C by electric furnace 22 and obtains four boron Sour lithium melt.The melt of melting by tremie pipe 24 flows out and falls the centrifugal atomizing that the rotating speed in atomization unit 30 is 10000rmp 31 surface of disk carries out centrifugal atomizing.It is 900 wherein to control the surface temperature of centrifugal atomizing disk 31 by electromagnetic induction heater 32 ℃.The drop of atomization cools down in tower 40 is collected in atomization and after the convergence of funnel-form loading head 51, into collection vessel 52 Further xrf analysis high-purity high-density degree lithium borate is obtained after cooling.The high density lithium tetraborate that the present embodiment obtains it is pure It is 99.993% to spend, density 1.4g/cm3, granularity is 300~400 microns.
Embodiment 2:
The mixed-powder of quality composition 50% high-pure anhydrous lithium tetraborate and 50% high-pure anhydrous lithium metaborate is stored in In the magazine 11 of feeding unit 10, open charger and be sent into powder in the crucible 21 of melting unit 20.Pass through electrical heating Raw material in crucible 21 is heated to 1250 DEG C and obtains lithium tetraborate melt by stove 22.The melt of melting is flowed out by tremie pipe 24 And it falls 31 surface of centrifugal atomizing disk that the rotating speed in atomization unit 30 is 15000rmp and carries out centrifugal atomizing.Wherein pass through electromagnetism sense It is 850 DEG C that heater 32 is answered, which to control the surface temperature of centrifugal atomizing disk 31,.The drop of atomization cools down simultaneously in tower 40 is collected in atomization After the convergence of funnel-form loading head 51, xrf analysis high-purity high-density is obtained after further being cooled down into collection vessel 52 Spend lithium borate.The purity of high density lithium borate mixed flux that the present embodiment obtains is 99.993%, density 1.3g/cm3, grain Spend is 200~300 microns.
Embodiment 3:
By high-pure anhydrous lithium metaborate powder storage in the magazine 11 of feeding unit 10, feeder is opened by powder It is sent into the crucible 21 of melting unit 20.The raw material in crucible 21 is heated to 1200 DEG C by electric furnace 22 and obtains inclined boron Sour lithium melt.The melt of melting by tremie pipe 24 flows out and falls the centrifugal atomizing that the rotating speed in atomization unit 30 is 20000rmp 31 surface of disk carries out centrifugal atomizing.It is 850 wherein to control the surface temperature of centrifugal atomizing disk 31 by electromagnetic induction heater 32 ℃.The drop of atomization cools down in tower 40 is collected in atomization and after the convergence of funnel-form loading head 51, into collection vessel 52 Further xrf analysis high-purity high-density degree lithium borate is obtained after cooling.The high density lithium borate mixing that the present embodiment obtains is molten The purity of agent is 99.993%, density 1.2g/cm3, granularity is 200~300 microns.
Embodiment 4:
Quality is formed into 37.5% pure Lithium Carbonate and the mixed-powder of 62.5% high-purity boracic acid is stored in feeding unit 10 In, it opens feeder and is sent into powder in the crucible 21 of melting unit 20.The raw material in crucible 21 is added by electric furnace 22 Heat is to 1250 DEG C and obtains lithium tetraborate melt.The melt of melting is flowed out by tremie pipe 24 and falls the rotating speed in atomization unit 30 31 surface of centrifugal atomizing disk for 5000rmp carries out centrifugal atomizing.Centrifugal atomizing is wherein controlled by electromagnetic induction heater 32 The surface temperature of disk 31 is 850 DEG C.The drop of atomization is cooled down in tower 40 is collected in atomization, is converged by funnel-form loading head 51 Afterwards, xrf analysis high-purity high-density degree lithium borate is obtained into after further cooling down in collection vessel 52.What the present embodiment obtained The purity of high density lithium borate mixed flux is 99.995%, density 1.3g/cm3, granularity is 400~600 microns.
In conclusion the production method and device of xrf analysis high-purity high-density degree lithium borate of the present invention being capable of the companies of realization Continuous production disclosure satisfy that the requirement of xrf analysis without broken or crushing, the high density lithium borate produced.
The invention is not limited in aforementioned specific embodiments.The present invention, which expands to, any in the present specification to be disclosed The step of new feature or any new combination and any new method or process disclosed or any new combination.

Claims (10)

1. a kind of xrf analysis process units of high-purity high-density degree lithium borate, which is characterized in that the preparation facilities includes sending Tower is collected in material unit, melting unit, atomization unit, collector unit and atomization;
Feeding unit includes the magazine and charger that communicate with each other;Melting unit includes the electricity with several heating elements Heating furnace and the crucible being arranged in electric furnace, the bottom of crucible are connected with tremie pipe, several described heating element rings are set In the surrounding of crucible and tremie pipe, wherein, the discharge port of charger is arranged on the top or directly and earthenware of the feed inlet of crucible The feed inlet connection of crucible;
Atomization unit is arranged on atomization and collects in tower, and atomization unit includes centrifugal atomizing disk, centrifugal atomizing disk installation shaft, electromagnetism Sensing heater and high-speed electric expreess locomotive, centrifugal atomizing disk are mounted on the top of centrifugal atomizing disk installation shaft, the installation of centrifugal atomizing disk Shaft is connect with high-speed electric expreess locomotive, and electromagnetic induction heater is installed around centrifugal atomizing disk is arranged in shaft and close to centrifugal atomizing Disk is set, wherein, the discharge port of the tremie pipe of melting unit is also disposed at atomization and collects in tower and positioned at centrifugal atomizing disk Surface;
Collector unit includes funnel-form loading head and collection vessel, and funnel-form loading head is arranged on the lower section of atomization unit, collects Container is arranged on the lower section of the discharge port of funnel-form loading head.
2. the xrf analysis according to claim 1 process units of high-purity high-density degree lithium borate, which is characterized in that institute It states feeding unit and further includes auto feed control system, the auto feed control system is carried out by the height of melt in crucible Charging automatically controls;The process units further includes control system, the control system to the action of entire process units into Row control.
3. the xrf analysis according to claim 1 process units of high-purity high-density degree lithium borate, which is characterized in that institute Crucible is stated as platinum yellow crucible, the heating element is Elema or Si-Mo rod.
4. the xrf analysis according to claim 1 process units of high-purity high-density degree lithium borate, which is characterized in that institute Centrifugal atomizing disk is stated as platinum yellow centrifugal atomizing disk, the centrifugal atomizing disk installation shaft is installed for high temperature alloy centrifugal atomizing disk Axis.
5. the xrf analysis according to claim 1 process units of high-purity high-density degree lithium borate, which is characterized in that institute It states atomization unit and further includes the bearing being arranged on the high-speed electric expreess locomotive and the electric motor protecting for accommodating the high-speed electric expreess locomotive and bearing Cover, centrifugal atomizing disk installation shaft are arranged in the centre bore of the bearing and rotatable by bearing and the bearing Ground connects.
6. the xrf analysis according to claim 1 process units of high-purity high-density degree lithium borate, which is characterized in that institute It states collector unit and further includes hydraulic elevator platform for placing the collection vessel.
7. a kind of xrf analysis production method of high-purity high-density degree lithium borate, which is characterized in that using in claim 1 to 6 Any one of them xrf analysis carries out xrf analysis high-purity high-density degree boron with the process units of high-purity high-density degree lithium borate The production of sour lithium, the production method include the following steps:
The raw material stored in feeding unit is sent into the crucible of melting unit;
The raw material in the crucible is heated to 1200~1350 DEG C by electric furnace and obtains melt;
The melt is made to be flowed out by tremie pipe and flows to the centrifugal atomizing disk that rotating speed in atomization unit is 5000~30000rmp Surface is atomized;
By the atomization melt drop that centrifugal atomizing disk is thrown away cools down in tower and collector unit are collected in atomization, collection obtains the X Fluorescence analysis high-purity high-density degree lithium borate;
Wherein, the raw material is the mixed of high-purity hydrated lithium borate, high-pure anhydrous lithium borate or high-purity boracic acid and pure Lithium Carbonate Close object.
8. the xrf analysis according to claim 7 production method of high-purity high-density degree lithium borate, which is characterized in that logical The surface temperature of centrifugal atomizing disk is 800~900 DEG C when crossing electromagnetic induction heater control atomization.
9. the xrf analysis according to claim 7 production method of high-purity high-density degree lithium borate, which is characterized in that institute High-purity hydrated lithium borate or high-pure anhydrous lithium borate are stated as the mixed of lithium tetraborate, lithium metaborate or lithium tetraborate and lithium metaborate Close object.
10. the xrf analysis according to claim 7 production method of high-purity high-density degree lithium borate, which is characterized in that institute The purity for stating xrf analysis high-purity high-density degree lithium borate is more than 99.99%, and density is 1.2~1.4g/cm3, granularity 200 ~600 microns.
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CN104016368A (en) * 2014-05-30 2014-09-03 成都开飞高能化学工业有限公司 Preparation method of anhydrous lithium borate flux for X-ray fluorescence analysis
CN204841627U (en) * 2015-05-27 2015-12-09 南京杰博宏镓新型材料有限公司 Refractory compound powder material's preparation facilities

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CN104016368A (en) * 2014-05-30 2014-09-03 成都开飞高能化学工业有限公司 Preparation method of anhydrous lithium borate flux for X-ray fluorescence analysis
CN204841627U (en) * 2015-05-27 2015-12-09 南京杰博宏镓新型材料有限公司 Refractory compound powder material's preparation facilities

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