CN102838125B - Preparation method of high-purity and high-density lithium tetraborate - Google Patents
Preparation method of high-purity and high-density lithium tetraborate Download PDFInfo
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- CN102838125B CN102838125B CN201210347200.5A CN201210347200A CN102838125B CN 102838125 B CN102838125 B CN 102838125B CN 201210347200 A CN201210347200 A CN 201210347200A CN 102838125 B CN102838125 B CN 102838125B
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- lithium hydroxide
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- PSHMSSXLYVAENJ-UHFFFAOYSA-N dilithium;[oxido(oxoboranyloxy)boranyl]oxy-oxoboranyloxyborinate Chemical compound [Li+].[Li+].O=BOB([O-])OB([O-])OB=O PSHMSSXLYVAENJ-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims abstract description 39
- 239000013078 crystal Substances 0.000 claims abstract description 27
- 238000001035 drying Methods 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000004327 boric acid Substances 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 13
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 238000002425 crystallisation Methods 0.000 claims abstract description 7
- 238000002844 melting Methods 0.000 claims abstract description 7
- 230000008018 melting Effects 0.000 claims abstract description 7
- 239000007787 solid Substances 0.000 claims abstract description 5
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 20
- GLXDVVHUTZTUQK-UHFFFAOYSA-M lithium;hydroxide;hydrate Chemical compound [Li+].O.[OH-] GLXDVVHUTZTUQK-UHFFFAOYSA-M 0.000 claims description 20
- 239000000843 powder Substances 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 13
- 239000003153 chemical reaction reagent Substances 0.000 claims description 12
- 238000001704 evaporation Methods 0.000 claims description 12
- 230000008020 evaporation Effects 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 12
- 238000005119 centrifugation Methods 0.000 claims description 11
- 239000012535 impurity Substances 0.000 claims description 11
- 238000006386 neutralization reaction Methods 0.000 claims description 11
- 229910001220 stainless steel Inorganic materials 0.000 claims description 11
- 239000010935 stainless steel Substances 0.000 claims description 11
- 238000001953 recrystallisation Methods 0.000 claims description 10
- 238000012360 testing method Methods 0.000 claims description 10
- 229910052742 iron Inorganic materials 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 8
- 230000004927 fusion Effects 0.000 claims description 7
- 238000009835 boiling Methods 0.000 claims description 6
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 5
- 238000004061 bleaching Methods 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 235000012054 meals Nutrition 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 238000001556 precipitation Methods 0.000 claims description 4
- 238000000034 method Methods 0.000 abstract description 12
- 230000008569 process Effects 0.000 abstract description 5
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 238000000746 purification Methods 0.000 abstract description 2
- 230000008025 crystallization Effects 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 230000007935 neutral effect Effects 0.000 abstract 1
- 238000010791 quenching Methods 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 15
- 238000005516 engineering process Methods 0.000 description 11
- 238000004458 analytical method Methods 0.000 description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000007844 bleaching agent Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 230000008676 import Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 150000001642 boronic acid derivatives Chemical class 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 238000005464 sample preparation method Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000002061 vacuum sublimation Methods 0.000 description 1
- 239000000037 vitreous enamel Substances 0.000 description 1
- 238000004857 zone melting Methods 0.000 description 1
Abstract
The invention relates to the technical field of preparation of lithium tetraborate, and particularly discloses a preparation method of high-purity and high-density lithium tetraborate. The preparation method comprises the following steps of: carrying out purification on industrial-grade lithium hydroxide by the steps of low-temperature dissolving, filtering, evaporative concentration, cooling crystallization, centrifugal separation and the like; dissolving the purified lithium hydroxide in boiled pure water according to the mass ratio 1:2 of solid and liquid; and according to the content of the lithium hydroxide in the solution, adding the lithium hydroxide into industrial-grade boric acid for neutral reaction according to the rate 105%-120% of stoichiometric numbers in reaction, and then preparing the high-purity and high-density lithium tetraborate by the processes of evaporative concentration, primary drying, crushing, secondary drying, high-temperature melting, water-quenching and cooling and the like. The prepared lithium tetraborate is about 1.4g/cm<3> in crystal density, and is more suitable for the current market demand.
Description
Technical field
The present invention relates to the preparing technical field of lithium tetraborate, relate in particular to a kind of preparation method of high-purity high-density degree lithium tetraborate.
Background technology
Lithium tetraborate has another name called lithium tetraborate, and molecular formula is Li
2b
4o
7, molecular weight is 169.12.High-purity, high-density lithium tetraborate is a kind of New temperature offset-type surface-duided wave substrate chip and piezoelectric monocrystal substrate material, in many fields such as microelectronics, digital technology, photoelectron science and technology, novel computer, video transmission, military science and technology, aerospace, satellite communication, defense technologies, has extensive and important application.As far back as 20 beginnings of the century, people have just made lithium tetraborate, but at that time because application Chemical Engineering Technology is weaker, lithium tetraborate is not widely used in all trades and professions, until just progressively start to be applied to the glaze of porcelain enamel industry the eighties in last century, lubricating grease component, later stage is along with the popularization of materials chemistry, lithium tetraborate is progressively applied to buffer reagent and sanitas, and be also applied to the exploitation of novel material, until 21 century, innovation along with smelting iron and steel technology, lithium tetraborate is used to wavelength dispersion X RF fluorescence spectrophotometer, the sample preparations such as AA atomic absorption and ICP are to detect iron and steel component, this is the arrival in intimation lithium tetraborate the new year, but along with constantly striding forward of technology paces, (density is about 0.7g/ ㎝ to high-purity lithium tetraborate of produced in conventional processes
3) can not meet the use that detects industry, the lithium tetraborate of various high-purity high-density degree is more and more welcome.
At present with regard to the production technique of lithium tetraborate, developed country produces this series products and mainly adopts Technologies such as " reduction, electrolysis, zone melting, vacuum distilling, vacuum-sublimations ", though there is certain using value, but that technology very complicated, technical process length, apparatus expensive, processing condition require is very harsh, production cost is high, contaminate environment and be difficult to administer, and is not suitable for the technical qualification of Current Domestic.
Summary of the invention
For the deficiencies in the prior art, the object of the present invention is to provide a kind of work simplification, processing condition require low, with low cost, easy to operate, quality index can be reached advanced world standards and the little preparation method who is easy to the high-purity high-density degree lithium tetraborate of improvement of environmental pollution.
To achieve these goals, technical conceive of the present invention is as follows:
By lithium hydroxide in industrial grade through dissolution in low temperature, filter, evaporation concentration, crystallisation by cooling, the steps such as centrifugation are purified, lithium hydroxide after purification is dissolved in the pure water boiling by solid-liquid mass ratio 1:2, according to the content of lithium hydroxide in solution, by 105%～120% of the ratio (hereinafter to be referred as " stoichiometric ratio ") of the stoichiometric number of reaction, add technical grade boric acid neutralization reaction (add excessive 5～20% boric acid), then through evaporation concentration, first drying, broken, secondary drying, high-temperature fusion, the flow processs such as shrend is cooling make the lithium tetraborate of high-purity high-density degree, its principal reaction principle is:
2LiOH+4H
3BO
3＝Li
2B
4O
7+7H
2O （1）
Li
2b
4o
7(powder)
li
2b
4o
7(melt) (2)
Concrete, the preparation method of a kind of high-purity high-density degree lithium tetraborate of the present invention, step is as follows:
A, lithium hydroxide purifying: primary industry stage monohydrate lithium hydroxide is dissolved in pure water with solid-liquid mass ratio 1:5 ratio; Add impurity removal reagents and remove by filter insolubles; Filtrate evaporation concentration is to visible obviously crystal; After being cooled to room temperature, centrifugation obtains recrystallization monohydrate lithium hydroxide;
Described impurity removal reagents by ethylenediamine tetraacetic acid (EDTA) and bicarbonate of ammonia in mass ratio 1:0.54 mix;
The amount of substance of the ethylenediamine tetraacetic acid (EDTA) in described impurity removal reagents is the twice of foreign metal Ca, Mg, Fe, the total amount of substance of Pb in described primary industry stage monohydrate lithium hydroxide;
B, neutralization batching: recrystallization monohydrate lithium hydroxide is dissolved with the pure water boiling with solid-liquid mass ratio 1:2, then according to 105%～120% of stoichiometric ratio, add boric acid neutralization, obtain neutralizer;
C, neutralizer is bleached with stainless steel cask evaporation concentration to solution;
D, first drying: by being evaporated to the lithium tetraborate solution bleaching, pour into while hot in stainless steel drip pan, first at 100-150 ℃, dry 3-4h, then dry 8-10h at 200-240 ℃;
E, secondary drying: the material after first drying is crushed to granularity between 10-60 orders, at 400-450 ℃, under 4-5h condition, carries out secondary drying;
F, the lithium tetraborate powder after secondary drying is carried out to melting, melt temperature 930-950 ℃, time 4--5h in electrothermal oven;
Material after G, melting carries out shrend crystallisation by cooling among pouring the pure water circulating into, and centrifugation obtains high-density Lithium Tetraborate Single Crystals;
H, step G gained crystal is dried to 1-2h at 60-80 ℃, remove plane of crystal moisture.
Described boric acid is Russian BOR MCC import boric acid (boric acid/% >=99.9; Water insoluble matter content/%≤0.010; Vitriol/%≤0.10; Muriate/%≤0.050; Iron/%≤0.0020; Ammonia/%≤0.30; Heavy metal/%≤0.0010).
Compared with prior art, advantage of the present invention and beneficial effect are:
1, adopt and first to prepare technical process that lithium tetraborate powder goes out Lithium Tetraborate Single Crystals by powder high-temperature fusion again to have solved lithium tetraborate chemical structure unstable than directly synthesizing Lithium Tetraborate Single Crystals technique with lithium hydroxide and boric acid high temperature, be mingled with other borates or Quilonum Retard, product purity is not high enough, the problem that process control condition is inaccurate;
2, directly the lithium tetraborate strong solution after concentrated is carried out to liquid oven dry, improved the yield of lithium tetraborate;
3, technique of the present invention other operations except high-temperature fusion operation are all carried out at normal pressure, middle low temperature, employing common stainless steel chemical industry equipment, and technique is greatly simplified, easy to operate succinct, environmentally safe, and production cost is well below external existing technique;
4, the lithium tetraborate density that adopts traditional technology to produce only has 0.7g/ ㎝
3left and right, and the made Lithium Tetraborate Single Crystals density of this technique is at 1.4g/ ㎝
3left and right, density is close to double, is more adapted to the market requirement now.
Embodiment
Applicant is described in further detail the inventive method in connection with specific embodiment below; should understand; following examples are only set forth technical scheme of the present invention for clear, and should in any degree, not be interpreted as the restriction of the claims in the present invention book being asked for protection to scope.
In embodiment 1-3, boric acid used is Russian BOR MCC import boric acid (boric acid/% >=99.9; Water insoluble matter content/%≤0.010; Vitriol/%≤0.10; Muriate/%≤0.050; Iron/%≤0.0020; Ammonia/%≤0.30; Heavy metal/%≤0.0010).
Embodiment 1
A preparation method for high-purity high-density degree lithium tetraborate, its step is as follows:
A, lithium hydroxide purifying: primary industry stage monohydrate lithium hydroxide is dissolved in pure water with solid-liquid mass ratio 1:5 ratio; Add impurity removal reagents (by ethylenediamine tetraacetic acid (EDTA) and bicarbonate of ammonia in mass ratio 1:0.54 mix) and remove by filter insolubles; Filtrate evaporation concentration is to visible obviously crystal; After being cooled to room temperature, centrifugation obtains recrystallization monohydrate lithium hydroxide;
The amount of substance of the ethylenediamine tetraacetic acid (EDTA) in described impurity removal reagents is the twice of foreign metal Ca, Mg, Fe, the total amount of substance of Pb in described primary industry stage monohydrate lithium hydroxide;
B, neutralization batching: get 6Kg recrystallization monohydrate lithium hydroxide with solid-liquid mass ratio 1:2 by the pure water stirring and dissolving of boiling to without obvious solid precipitation, under stirring, according to 105% times of stoichiometric ratio, slowly add boric acid (being 18.54Kg) neutralization, with wide pH value test paper, recording endpoint pH is 8-9, obtains neutralizer;
C, by neutralizer with stainless steel cask evaporation concentration to solution bleach (that is: have lithium tetraborate to separate out, now solution is sticky, 230 ℃ of left and right of temperature);
D, first drying: by being evaporated to the lithium tetraborate solution bleaching, pour into while hot in stainless steel drip pan, first at 100 ℃, dry 4h, then dry 10h at 200 ℃;
E, secondary drying: the material after first drying is dried to 5h with (raw meal particle size, between 10-60 orders, goes out lithium tetraborate powder 14Kg altogether after broken) after jaw crusher and roller pair breaking crusher machine at 400 ℃;
F, the lithium tetraborate powder after secondary drying is carried out to high-temperature fusion in tubular type electrothermal oven, 930 ℃ of melt temperatures, time 5h;
Material after G, melting carries out shrend crystallisation by cooling among pouring the pure water circulating into, and centrifugation obtains high-density Lithium Tetraborate Single Crystals;
H, step G gained crystal is dried to 2h at 60 ℃, remove plane of crystal moisture.
Step e gained lithium tetraborate powder is carried out to ultimate analysis, step H gained Lithium Tetraborate Single Crystals is carried out to densimetric analysis, result is as follows:
| Test item | Content (wt%) | Test item | Content (wt%) |
| Li 2B 4O 7 | ≥99.99 | Na | 0.001 |
| K | <0.001 | Ca | 0.001 |
| Mg | 0.001 | Fe | 0.0008 |
| Si | 0.0016 | Pb | 0.0004 |
| PO 4 3- | 0.001 | Proportion | 1.38g/㎝ 3 |
Embodiment 2
A preparation method for high-purity high-density degree lithium tetraborate, its step is as follows:
A, lithium hydroxide purifying: primary industry stage monohydrate lithium hydroxide is dissolved in pure water with solid-liquid mass ratio 1:5 ratio; Add impurity removal reagents (by ethylenediamine tetraacetic acid (EDTA) and bicarbonate of ammonia in mass ratio 1:0.54 mix) and remove by filter insolubles; Filtrate evaporation concentration is to visible obviously crystal; After being cooled to room temperature, centrifugation obtains recrystallization monohydrate lithium hydroxide;
The amount of substance of the ethylenediamine tetraacetic acid (EDTA) in described impurity removal reagents is the twice of foreign metal Ca, Mg, Fe, the total amount of substance of Pb in described primary industry stage monohydrate lithium hydroxide;
B, neutralization batching: get 6Kg recrystallization monohydrate lithium hydroxide with solid-liquid mass ratio 1:2 by the pure water stirring and dissolving of boiling to without obvious solid precipitation, under stirring, according to 110% times of stoichiometric ratio, slowly add boric acid (being 19.43Kg) neutralization, with wide pH value test paper, record endpoint pH 7.5-8, obtain neutralizer;
C, by neutralizer with stainless steel cask evaporation concentration to solution bleach (that is: have lithium tetraborate to separate out, now solution is sticky, 230 ℃ of left and right of temperature);
D, first drying: by being evaporated to the lithium tetraborate solution bleaching, pour into while hot in stainless steel drip pan, first at 130 ℃, dry 4h, then dry 9h at 220 ℃;
E, secondary drying: the material after first drying is dried to 4h with (raw meal particle size, between 10-60 orders, goes out lithium tetraborate powder 14.2Kg altogether after broken) after jaw crusher and roller pair breaking crusher machine at 430 ℃;
F, the lithium tetraborate powder after secondary drying is carried out to high-temperature fusion in tubular type electrothermal oven, 940 ℃ of melt temperatures, time 5h;
Material after G, melting carries out shrend crystallisation by cooling among pouring the pure water circulating into, and centrifugation obtains high-density Lithium Tetraborate Single Crystals;
H, step G gained crystal is dried to 2h at 70 ℃, remove plane of crystal moisture.
Step e gained lithium tetraborate powder is carried out to ultimate analysis, step H gained Lithium Tetraborate Single Crystals is carried out to densimetric analysis, result is as follows:
| Test item | Content (wt%) | Test item | Content (wt%) |
| Li 2B 4O 7 | ≥99.99 | Na | <0.001 |
| K | <0.001 | Ca | 0.001 |
| Mg | 0.0008 | Fe | 0.0007 |
| Si | 0.0013 | Pb | 0.0003 |
| PO 4 3- | 0.001 | Proportion | 1.39g/㎝ 3 |
Embodiment 3
A preparation method for high-purity high-density degree lithium tetraborate, its step is as follows:
A, lithium hydroxide purifying: primary industry stage monohydrate lithium hydroxide is dissolved in pure water with solid-liquid mass ratio 1:5 ratio; Add impurity removal reagents (by ethylenediamine tetraacetic acid (EDTA) and bicarbonate of ammonia in mass ratio 1:0.54 mix) and remove by filter insolubles; Filtrate evaporation concentration is to visible obviously crystal; After being cooled to room temperature, centrifugation obtains recrystallization monohydrate lithium hydroxide;
The amount of substance of the ethylenediamine tetraacetic acid (EDTA) in described impurity removal reagents is the twice of foreign metal Ca, Mg, Fe, the total amount of substance of Pb in described primary industry stage monohydrate lithium hydroxide;
B, neutralization batching: get 6Kg recrystallization monohydrate lithium hydroxide with solid-liquid mass ratio 1:2 by the pure water stirring and dissolving of boiling to without obvious solid precipitation, under stirring, according to 120% times of stoichiometric ratio, slowly add boric acid (being 21.19Kg) neutralization, with wide pH value test paper, survey endpoint pH 7-7.5, obtain neutralizer;
C, by neutralizer with stainless steel cask evaporation concentration to solution bleach (that is: have lithium tetraborate to separate out, now solution is sticky, 230 ℃ of left and right of temperature);
D, first drying: by being evaporated to the lithium tetraborate solution bleaching, pour into while hot in stainless steel drip pan, first at 150 ℃, dry 4h, then dry 10h at 240 ℃;
E, secondary drying: the material after first drying is dried to 4h with (raw meal particle size, between 10-60 order, goes out lithium tetraborate powder 14.3Kg altogether after broken) after jaw crusher and roller pair breaking crusher machine at 450 ℃;
F, the lithium tetraborate powder after secondary drying is carried out to high-temperature fusion in tubular type electrothermal oven, 950 ℃ of melt temperatures, time 4h;
Material after G, melting carries out shrend crystallisation by cooling among pouring the pure water circulating into, and centrifugation obtains high-density Lithium Tetraborate Single Crystals;
H, step G gained crystal is dried to 1h at 80 ℃, remove plane of crystal moisture.
Step e gained lithium tetraborate powder is carried out to ultimate analysis, step H gained Lithium Tetraborate Single Crystals is carried out to densimetric analysis, result is as follows:
| Test item | Content (wt%) | Test item | Content (wt%) |
| Li 2B 4O 7 | ≥99.99 | Na | <0.001 |
| K | <0.001 | Ca | <0.001 |
| Mg | <0.001 | Fe | 0.0005 |
| Si | 0.0012 | Pb | 0.0003 |
| PO 4 3- | 0.001 | Proportion | 1.41g/㎝ 3 |
Claims (1)
1. a preparation method for high-purity high-density degree lithium tetraborate, its step is as follows:
A, lithium hydroxide purifying: primary industry stage monohydrate lithium hydroxide is dissolved in pure water with solid-liquid mass ratio 1:5 ratio; Add by ethylenediamine tetraacetic acid (EDTA) and the bicarbonate of ammonia impurity removal reagents that 1:0.54 mixes in mass ratio and remove by filter insolubles; Filtrate evaporation concentration is to visible obviously crystal; After being cooled to room temperature, centrifugation obtains recrystallization monohydrate lithium hydroxide;
The amount of substance of the ethylenediamine tetraacetic acid (EDTA) in described impurity removal reagents is the twice of foreign metal Ca, Mg, Fe, the total amount of substance of Pb in described primary industry stage monohydrate lithium hydroxide;
B, neutralization batching: get 6kg recrystallization monohydrate lithium hydroxide with solid-liquid mass ratio 1:2 by the pure water stirring and dissolving of boiling to without obvious solid precipitation, under stirring, according to 120% times of stoichiometric ratio, slowly add boric acid neutralization, with wide pH value test paper, survey endpoint pH 7-7.5, obtain neutralizer;
C, neutralizer is bleached with stainless steel cask evaporation concentration to solution;
D, first drying: by being evaporated to the lithium tetraborate solution bleaching, pour into while hot in stainless steel drip pan, first at 150 ℃, dry 4h, then dry 10h at 240 ℃;
E, secondary drying: by the material after first drying, with drying 4h after jaw crusher and roller pair breaking crusher machine at 450 ℃, broken rear raw meal particle size, between 10-60 orders, goes out lithium tetraborate powder 14.3kg altogether;
F, the lithium tetraborate powder after secondary drying is carried out to high-temperature fusion in tubular type electrothermal oven, 950 ℃ of melt temperatures, time 4h;
Material after G, melting carries out shrend crystallisation by cooling among pouring the pure water circulating into, and centrifugation obtains high-density Lithium Tetraborate Single Crystals;
H, step G gained crystal is dried to 1h at 80 ℃, remove plane of crystal moisture.
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| CN104016368B (en) * | 2014-05-30 | 2015-11-11 | 成都开飞高能化学工业有限公司 | The xrf analysis preparation method of anhydrous boric acid lithium flux |
| EP2966039B1 (en) * | 2014-07-08 | 2018-04-18 | Malvern Panalytical B.V. | Preparation of samples for XRF using flux and platinum crucible |
| CN105294071B (en) * | 2015-11-05 | 2017-07-28 | 武汉科技大学 | It is a kind of for lined container of noble metal crucible and preparation method thereof |
| CN106006653B (en) * | 2016-07-22 | 2018-05-29 | 中国科学院青海盐湖研究所 | A kind of method for preparing high specific surface area porous lithium magnesium silicate powder using salt lake bittern after potassium is carried |
| CN106732849B (en) * | 2016-12-20 | 2019-07-09 | 武汉科技大学 | A kind of preparation method of flux crucible cover |
| CN108910907A (en) * | 2018-07-20 | 2018-11-30 | 上海中锂实业有限公司 | A kind of preparation method of anhydrous lithium tetraborate |
| CN115304074B (en) * | 2022-08-25 | 2023-05-12 | 江西赣锋锂业股份有限公司 | Preparation method of anhydrous lithium tetraborate |
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| CN1818149A (en) * | 2005-06-22 | 2006-08-16 | 广州锐鑫锂能新材料科技有限公司 | Production of high-purity lithium tetraborate crystal by industrial lithium hydroxide and boric acid |
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| CN1818149A (en) * | 2005-06-22 | 2006-08-16 | 广州锐鑫锂能新材料科技有限公司 | Production of high-purity lithium tetraborate crystal by industrial lithium hydroxide and boric acid |
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