CN1100807A - Sodium fluoride sintering method for determinating molecular ratio of aluminium electrolyte - Google Patents
Sodium fluoride sintering method for determinating molecular ratio of aluminium electrolyte Download PDFInfo
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- CN1100807A CN1100807A CN 93115818 CN93115818A CN1100807A CN 1100807 A CN1100807 A CN 1100807A CN 93115818 CN93115818 CN 93115818 CN 93115818 A CN93115818 A CN 93115818A CN 1100807 A CN1100807 A CN 1100807A
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- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 title claims abstract description 44
- 239000003792 electrolyte Substances 0.000 title claims abstract description 24
- 239000011775 sodium fluoride Substances 0.000 title claims abstract description 22
- 235000013024 sodium fluoride Nutrition 0.000 title claims abstract description 22
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 19
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 238000005245 sintering Methods 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 17
- 239000004411 aluminium Substances 0.000 title claims abstract description 16
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims abstract description 15
- 239000000243 solution Substances 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000012086 standard solution Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 239000011734 sodium Substances 0.000 claims description 20
- 229910004261 CaF 2 Inorganic materials 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 239000012556 adjustment buffer Substances 0.000 claims description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 4
- 230000007935 neutral effect Effects 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 229910016569 AlF 3 Inorganic materials 0.000 claims description 2
- 229960000583 acetic acid Drugs 0.000 claims description 2
- 239000012362 glacial acetic acid Substances 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- 238000005259 measurement Methods 0.000 claims 1
- 239000001509 sodium citrate Substances 0.000 claims 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 230000003750 conditioning effect Effects 0.000 abstract 1
- 150000002500 ions Chemical class 0.000 abstract 1
- 239000007784 solid electrolyte Substances 0.000 abstract 1
- 230000002378 acidificating effect Effects 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000002671 adjuvant Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229910001610 cryolite Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminium flouride Chemical compound F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 description 1
- 244000248349 Citrus limon Species 0.000 description 1
- 235000005979 Citrus limon Nutrition 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical compound Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- -1 fully stirs Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000007704 wet chemistry method Methods 0.000 description 1
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- Electrolytic Production Of Metals (AREA)
Abstract
The measuring method includes the steps of sintering 0.25-0.5g sodium fluoride and 0.5-1.5g solid electrolyte sample in muffle furnace, sintering temperature is controlled in the range of 550-700 deg.C after cooling, putting the sample into 200-300 ml of fluorine ion standard solution, after stirring, adding 8-15 ml the said solution into a vessel of 50 ml, then adding 25 ml of ion intensity conditioning agent, using deionic water to dilute to scale, then measuring the solution in a beaker of fluorine ion selective electrode to obtain electromotive force, E, based on the measured E value, log C value can be obtained from E-log C standard curve of present invention, and then calculating the molecular ratio of aluminium electrolyte.
Description
The invention belongs to metallurgical technology field, particularly a kind of sodium fluoride sintering method is measured the analytical approach of aluminium electrolyte molecule.
The molecular proportion of aluminium electrolyte has significant impact for the current efficiency and the energy consumption of aluminium electroloysis.The method of measuring the aluminium electrolyte molecular proportion now is a lot, as crystal optics method, conductance method, x-ray diffraction method, thermal titration etc.On the modern aluminum industry,, adopt several adjuvants, as CaF in order to improve electrolytical character
2, MgF
2, LiF etc. obtains good effect on producing.But, having brought the complicated of electrolyte composition, the assay method of molecular proportion need be done corresponding improvement thereupon.Germany Ke Deman and Bu Laosi have provided at Na on the 288-292 page or leaf at " the metallurgical magazine of digging up mine " 1980
3AlF
6-Al
2O
3Add AlF in the system
3, CaF
2, MgF
2Facies analysis result with LiF.People such as U.S. Lv Chazi are at " light metal " 1983, and the 379-388 page or leaf has at length been reported the relevant reaction of acidic electrolyte bath.Norway in 1984 how people such as dagger-axe has delivered the method that a kind of wet chemistry is measured molecular proportion at " light metal " 1984 on the 501-502 page or leaf.The principle of people's methods such as Nai Ge is bath sample directly to be put into the alkaline solution that contains NaF dissolve, and thinks free AlF in the sample
3Will react with NaF and generate neutral cryolite (Na
3AlF
6).Then, with the NaF concentration in the fluoride ion selective electrode mensuration surplus solution, the NaF amount to determine to be consumed in above-mentioned chemical reaction calculates molecular proportion at last.Through the inventor's research and comparison, think that the method majority of existing mensuration molecular proportion is undesirable after the electrolyte composition is complicated, because the thing in the sample with tissue great change has taken place mutually.Though wherein how the analytical approach of dagger-axe is comparatively easy, the precision of analyzing is very low, and its main cause is: too low with containing the aqueous solution of NaF with the temperature that bath sample carries out chemical reaction, so that reaction is incomplete, causes the molecule ratio deviation that records very big.
In view of measuring the deficiency that aluminium electrolyte molecular proportion prior art exists, the object of the present invention is to provide a kind of measuring accuracy height, simple equipments is with the analytical approach of sodium fluoride sintering method mensuration aluminium electrolyte molecular proportion.
For achieving the above object, the present invention adopts following method step to realize.
Same 0.5～1.5g solid electrolytic quality sample the sintering in muffle furnace of first solid NaF with 0.25～0.5g, the control sintering temperature is at 550 ℃～700 ℃, be lower than this temperature and then react not exclusively, be higher than the then electrolytical component volatilization of this temperature, the degree of accuracy that influence is measured.After the cooling, sample is put into 200-300ml fluorine ion standard solution, fully stir, make in the sample residue NaF soluble in water fully.Get this solution of 8～15ml to the 50ml volumetric flask, add 25ml total ionic strength adjustment buffer degree correctives, be diluted to the scale of volumetric flask then with deionized water, again this solution is moved in the beaker of fluoride ion selective electrode determinator and measure, obtain potential value E.With the E value of measuring, obtain the logC value on Yan Zhi the E-logC typical curve in the present invention then, calculate the C value again,, can calculate the molecule ratio of sample at last by Computing.The available following formula of residue NaF amount (N) calculates in the sample: N=2.5C.Electrolytical molecular proportion (K) value is calculated as follows:
K＝ (3Wβ-2(N′-N))/(Wβ+(N′-N))
W-bath sample weight in the formula, g
The g-corrected value
N '-be used for the NaF total amount of sintering, g
The remaining NaF amount of N-, g
Corrected value β calculates by following situation in the formula:
(I) adds CaF
2: because CaF
2Reality does not react in alkalescence and neutral electrolyte, therefore, and β=1-Al
2O
3%-CaF
2%.
(II) adds CaF
2+ MgF
2: MgF
2With Na
3AlF
6React, form NaMgF
3, 1%(weight) and MgF
2Form 1.68%NaMgF
3So, β=1-Al
2O
3%-CaF
2%-1.68%MgF
2
(III) adds CaF
2+ LiF+MgF
2: LiF forms Li
3AlF
6, 1%(weight) and LiF generates 2.08%Li
3AlF
3So,, β=1-Al
2O
3%-CaF
2%-1.68MgF
2%-2.08LiF%.
Because of MgF in the industrial aluminum electrolyte
2Generally lower with LiF content, above-mentioned definition and formula are suitable substantially.
The solution compound method is as follows: with deionized water preparation fluorine ion standard solution, its concentration is 1gF
-/ dm
3Total ionic strength adjustment buffer degree correctives is to join sodium+57ml glacial acetic acid with the 58gNaCl+10g lemon, is dissolved in the 500ml deionized water, adjusts pH to 5.0～5.5 with 5N NaOH solution, is diluted to 1000ml with deionized water again.
Principle of the present invention is: the electrolytical original set of industrial aluminum becomes: cryolite (Na
3AlF
6), free aluminum fluoride (AlF
3) and aluminium oxide (Al
2O
3), wherein add CaF
2, MgF
2After LiF, in the acidic electrolyte bath scope, form multiple new thing phase, as shown in table 1 below.
And in 550 ℃ of-700 ℃ of temperature ranges,, then originally be present in the Na in the acidic electrolyte bath if there is excess of fluoride
5Al
3F
14, NaCaAlF
6, Na
2MgAlF
7And Na
2LiAlF
6Will resolve into Na Deng compound
3AlF
6, CaF
2, NaMgF
3And Li
3AlF
6According to these thing phase change rules, can calculate the molecular proportion of aluminium electrolyte sample.
Table 1 Na
3AlF
6-AlF
3-Al
2O
3Thing phase composition in (acidic electrolyte bath) system behind the adding adjuvant
| Adjuvant | The thing phase composition | |||
| Do not have | ?Na 3AlF 6, Al 2o 3, Na 5Al 3F 14 | |||
| 5%?CaF 2 | ?Na 3AlF 6, Al 2O 3, Na 5Al 3F 14, NaCaAlF 6 | |||
| 5%MgF 2 | ?Na 3AlF 6, Al 2O 3, Na 5Al 3F 14, Na 2MgAlF 6 | |||
| 5%LiF | ?Na 3AlF 6, Al 2O 3, Na 5Al 3F 14, Na 2LiAlF 6 | |||
The present invention compared with prior art has following advantage and effect.
1. analysis precision height.Use the obtained precision of this method, with thermal titration be benchmark compares, its deviate is in ± 0.05 unit, has satisfied the needs on producing.Concrete data are as shown in table 2.
2. in operation, sodium fluoride sintering method only needs easy instrument and equipment, and about 2000 yuan, the muffle furnace of sintering is general in the common laboratory.Used drug expenditure is cheap.Therefore, cost is low, is applicable to the electrolytic aluminium factory of various scales.
Below in conjunction with drawings and Examples the present invention is further described.
Fig. 1 is a testing apparatus installation drawing provided by the invention.
Fig. 2 is a fluoride electrode canonical plotting provided by the invention.
From shown in Figure 1, as can be seen, liquid to be measured is contained in the beaker that magnetic stirring apparatus 7 is housed, and the fluoride ion selective electrode 3, reference mercurous chloride electrode 2 and the thermometer 4 that support with support 5 insert respectively in the solution to be measured, connect digital ionometer 1 with lead, constitute and measure the loop.
Embodiment one
Use 1.0g electrolyte sample powder (100 order) with 0.3g NaF sintering earlier, sintering temperature is 600 ℃, and sintering time is 30 minutes, after the cooling, sample is put into 250ml fluorine ion standard solution, fully stirs, and NaF remaining in the sample is dissolved fully.Get this solution of 10ml to the 50ml volumetric flask, add the total ionic strength adjustment buffer degree correctives solution of 25ml.Be diluted to scale with deionized water, again this solution be transferred in the beaker shown in the accompanying drawing 1, measure, obtain potential value E.Find corresponding 1gC value from standard electrode potential figure (Fig. 2) then, converse the C value.Calculate at last the molecule ratio of sample after the electrolysis according to the formula of molecular proportion.
Embodiment two
Operation and step are with embodiment one.Sintering temperature is 550 ℃, and sample is put into 150ml fluorine ion standard solution.
Embodiment three
Operation and step are with embodiment one.Sintering temperature is 700 ℃, and sample is put into 300ml fluorine ion standard solution.
Claims (4)
1, a kind of sodium fluoride sintering method is measured the analytical approach of aluminium electrolyte molecular proportion, it is characterized in that: elder generation is sintering in muffle furnace with 0.25～0.5g sodium fluoride and 0.5～1.5g solid electrolytic quality sample, the control sintering temperature is at 550 ℃～700 ℃, after the cooling, again sample is put into 200～300ml fluorine ion standard solution, fully stir, make in the sample remaining sodium fluoride soluble in water fully, get this solution of 8～15ml to the 50ml volumetric flask, add 25ml total ionic strength adjustment buffer degree correctives, be diluted to scale with deionized water then, again this solution is moved in the beaker of fluoride ion selective electrode determinator and measure, obtain potential value E, with the E value of measuring, obtain the logC value on the E-logC typical curve of Hui Zhiing in the present invention and calculate the C value again, at last by calculating the molecule ratio that can obtain aluminium electrolyte.
2, the analytical approach of measurement aluminium electrolyte molecular proportion according to claim 1 is characterized in that: said fluorine ion standard solution with the deionized water preparation, its concentration is 1gF
-/ dm
3, said total ionic strength adjustment buffer degree correctives is with 58gNaCl+10g sodium citrate+57ml glacial acetic acid, is dissolved in the 500ml deionized water, adjusts pH to 5.0～5.5 with 5N NaOH solution, is diluted to 1000ml with deionized water again.
3, the analytical approach of mensuration aluminium electrolyte molecular proportion according to claim 1 is characterized in that: said being meant by calculating remains the available following formula calculating of NaF amount (N), N=2.5C in the sample.Electrolytical molecular proportion is calculated as follows:
K＝ (3Wβ-2(N′-N))/(Wβ+(N′-N))
4, the analytical approach of mensuration aluminium electrolyte molecular proportion according to claim 3, it is characterized in that: β is a corrected value in the said calculating formula, calculates by following situation:
(I) adds CaF
2: because CaF
2Reality does not react in alkalescence and neutral electrolyte, therefore, and β=1-Al
2O
3%-CaF
2%.
(II) adds CaF
2+ MgF
2: MgF
2With Na
3AlF
6React, form NaMgF
3, 1%(weight) and MgF
2Form 1.68%NaMgF
3So, β=1-Al
2O
3%-CaF
2%-1.68%MgF
2
(III) adds CaF
2+ LiF+MgF
2: LiF forms Li
3AlF
6, 1%(weight) and LiF generates 2.08%Li
3AlF
3So,, β=1-Al
2O
3%-CaF
2%-1.68MgF
2%-2.08LiF%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93115818 CN1100807A (en) | 1993-09-23 | 1993-09-23 | Sodium fluoride sintering method for determinating molecular ratio of aluminium electrolyte |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93115818 CN1100807A (en) | 1993-09-23 | 1993-09-23 | Sodium fluoride sintering method for determinating molecular ratio of aluminium electrolyte |
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| Publication Number | Publication Date |
|---|---|
| CN1100807A true CN1100807A (en) | 1995-03-29 |
Family
ID=4991353
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 93115818 Pending CN1100807A (en) | 1993-09-23 | 1993-09-23 | Sodium fluoride sintering method for determinating molecular ratio of aluminium electrolyte |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100514055C (en) * | 2006-08-30 | 2009-07-15 | 中国铝业股份有限公司 | Analysing method of excess alumina content in aluminium electrolyte |
| RU2550861C1 (en) * | 2014-01-23 | 2015-05-20 | Общество с ограниченной ответственностью "Объединенная Компания РУСАЛ Инженерно-технологический центр" | Method for determining component composition and cryolite ratio of solid samples of potassium-containing electrolyte of aluminium production by xpa method |
| CN105353001A (en) * | 2015-11-23 | 2016-02-24 | 中国铝业股份有限公司 | Analysis method of high lithium potassium aluminum electrolyte molecular ratio |
| CN105543504A (en) * | 2015-12-21 | 2016-05-04 | 东北大学 | Method for extracting lithium salt from aluminum electrolyte by utilizing fluoride roasting and acid leaching |
| CN106062541A (en) * | 2015-02-04 | 2016-10-26 | 俄罗斯工程技术中心 | Method for determining the composition and cryolite ratio of solid samples of potassium-containing electrolyte in aluminium production by XRD |
-
1993
- 1993-09-23 CN CN 93115818 patent/CN1100807A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100514055C (en) * | 2006-08-30 | 2009-07-15 | 中国铝业股份有限公司 | Analysing method of excess alumina content in aluminium electrolyte |
| RU2550861C1 (en) * | 2014-01-23 | 2015-05-20 | Общество с ограниченной ответственностью "Объединенная Компания РУСАЛ Инженерно-технологический центр" | Method for determining component composition and cryolite ratio of solid samples of potassium-containing electrolyte of aluminium production by xpa method |
| WO2015112059A1 (en) * | 2014-01-23 | 2015-07-30 | Общество с ограниченной ответственностью "Объединенная Компания РУСАЛ Инженерно-технологический центр" | Method for determining the composition and cryolite ratio of solid samples of potassium-containing electrolyte in aluminium production by xrd |
| US10073049B2 (en) | 2014-01-23 | 2018-09-11 | United Company RUSAL Engineering and Technology Centre LLC | Method for determining the composition and cryolite ratio of solid samples of potassium-containing electrolyte in aluminum production by XRD |
| CN106062541A (en) * | 2015-02-04 | 2016-10-26 | 俄罗斯工程技术中心 | Method for determining the composition and cryolite ratio of solid samples of potassium-containing electrolyte in aluminium production by XRD |
| CN106062541B (en) * | 2015-02-04 | 2019-04-30 | 俄铝工程技术中心有限责任公司 | The method for measuring the composition and cryolite ratio of the solid sample of electrolyte containing potassium |
| CN105353001A (en) * | 2015-11-23 | 2016-02-24 | 中国铝业股份有限公司 | Analysis method of high lithium potassium aluminum electrolyte molecular ratio |
| CN105543504A (en) * | 2015-12-21 | 2016-05-04 | 东北大学 | Method for extracting lithium salt from aluminum electrolyte by utilizing fluoride roasting and acid leaching |
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