CN108362606A - A kind of charcoal composite lithium iron phosphate cathode material phosphorus element content detection method - Google Patents
A kind of charcoal composite lithium iron phosphate cathode material phosphorus element content detection method Download PDFInfo
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- CN108362606A CN108362606A CN201810007606.6A CN201810007606A CN108362606A CN 108362606 A CN108362606 A CN 108362606A CN 201810007606 A CN201810007606 A CN 201810007606A CN 108362606 A CN108362606 A CN 108362606A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
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- G01N1/44—Sample treatment involving radiation, e.g. heat
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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Abstract
The invention discloses a kind of charcoal composite lithium iron phosphate cathode material phosphorus element content detection methods, include the following steps：Weigh sample to be tested；Sample to be determined is placed in equipped with 20%（V/V）In the container of hydrochloric acid, it is heated to sample to be determined and is completely dissolved, with 50%（V/V）After heating water bath, excessive quinoline molybdenum lemon ketone solution is added in nitric acid and water constant volume, and heating water bath heat preservation obtains supernatant liquor and precipitation；Postcooling that the reaction was complete is to room temperature；Drying to constant weight for sintered glass funnel, supernatant liquor and precipitation are moved into sintered glass funnel to be filtered, it is precipitated, by washing, drying, it is cooled to constant weight and weighs, it is carried out at the same time blank assay, it is dissolved by heating by sample plus hydrochloric acid, after being completely dissolved, with nitre acid-conditioning solution to appropriate acid or alkali environment, after heating is boiled, quinoline molybdenum lemon ketone solution is added, heating water bath heat preservation forms precipitation, precipitation is cleaned, is filtered, it dries, weigh, phosphorus element content is calculated, can fast and accurately detect phosphorus element content.
Description
Technical field
The present invention relates to phosphorus element content detection methods, it particularly relates to a kind of charcoal composite lithium iron phosphate cathode material
Phosphorus element content detection method.
Background technology
Lithium ion battery is high as a kind of energy density, output voltage is high, cycle performance is excellent, memory-less effect, environment
Friendly electrochmical power source system, with good economic efficiency, social benefit and strategic importance are widely used in mobile logical
The multiple fields such as news, digital product, electric vehicle.Currently, the application field with lithium ion battery is more and more extensive, difference is used
Requirement of the family to lithium ion battery also differs.In this field of low temperature lithium battery, increasingly to the capacity requirement of low temperature discharge
It is high.As the significant components for influencing lithium battery performance, the effect of the positive active material of lithium battery is most important.Lithium battery at present
Positive active material include ferrous disulfide, cobalt acid lithium, LiFePO4 etc., the wherein security performance and cycle life of LiFePO4
It is that other battery materials are incomparable.LiFePO4 is cheap, specific capacity is high, has a safety feature, and is ideal lithium ion
Cell positive material, especially its stability at relatively high temperatures can provide safety and protect as high power, high-capacity battery
Barrier, is the ideal material of power battery.
The phosphorus element content of LiFePO 4 material is an importance of its property, is that lithium ion battery before manufacture must
The step of must carrying out.P elements have certain limitation as the Main elements in material, conventional ICP tests.The present invention
Using the method for chemistry titration, phosphorus element content can be fast and accurately detected.
For the problems in the relevant technologies, currently no effective solution has been proposed.
Invention content
For above-mentioned technical problem in the related technology, the present invention proposes a kind of charcoal composite lithium iron phosphate cathode material phosphorus member
Cellulose content detection method can solve above-mentioned technical problem.
To realize the above-mentioned technical purpose, the technical proposal of the invention is realized in this way：
A kind of charcoal composite lithium iron phosphate cathode material phosphorus element content detection method, includes the following steps：
S1. sample to be tested is weighed, record quality is m；
S2. sample treatment：Sample to be determined is placed in equipped with 20%（V/V）In the container of hydrochloric acid, it is complete to be heated to sample to be determined
Dissolving；
S3. precipitation reaction is carried out：The sample solution that step S2 is completely dissolved is with 50%（V/V）Nitric acid and water constant volume, water-bath add
Supernatant liquor and precipitation is obtained by the reaction to excessive quinoline molybdenum lemon ketone solution, heating water bath heat preservation after 98-100 DEG C, is added in heat；
S4. it cools down：Postcooling that the reaction was complete is to room temperature；
S5. it filters：By sintered glass funnel, drying to constant weight, and record quality is m2, by the supernatant liquor and precipitation described in step S4
It moves into sintered glass funnel to be filtered, be precipitated, by washing, drying, be cooled to constant weight and weigh, record quality is m1；
S6. blank assay：Step S1-S5 is carried out at the same time blank assay, and wherein step S5 blank assays result is m3；
S7. phosphorus element content result calculates：Wp=（m1-m2-m3）× 0.01400/m × 100%, wherein
m1The quality of phosphomolybdic acid quinoline precipitation and sintered glass funnel is generated in-testing liquid；
m2The quality of sintered glass funnel in-experiment；
m3The quality of phosphomolybdic acid quinoline obtained by-blank assay；
The quality of m-sample；
0.01400 --- phosphomolybdic acid quinoline precipitates the coefficient for being scaled phosphorus quality.
Further, the preparation method of quinoline molybdenum lemon ketone solution described in step S3 is：70g sodium molybdates are taken to be dissolved in 100ml water,
Obtain solution A；It takes 60g citric acids to be dissolved in 150ml water and 85ml nitric acid, obtains solution B；Solution A is poured into solution B under stiring
In, mixing obtains solution C；35ml50% is added in 100ml water（V/V）Nitric acid and 5ml quinoline, obtain solution D；Solution D is poured into molten
In liquid C, mixing stands a night, is filtered with filter paper, 280ml acetone is added in filtrate, 1000ml is diluted to deionized water,
Obtain quinoline molybdenum lemon ketone solution.
Further, the quinoline molybdenum lemon ketone solution configured is stored in polyethylene bottle, is put in dark place, shading is Protected from Heat.
Further, heating temperature described in step S2 is 180 DEG C.
Further, it is precipitated after being filtered described in step S5, through water washing 5-6 times.
Further, drying temperature described in step S5 is 180 DEG C, drying time 45min.
Beneficial effects of the present invention：It is dissolved by heating by sample plus hydrochloric acid, after being completely dissolved, with nitre acid-conditioning solution to suitable
To work as acid or alkali environment, after heating is boiled, quinoline molybdenum lemon ketone solution is added, heating water bath heat preservation forms precipitation, precipitation is cleaned,
It filters, dries, weighs, phosphorus element content is calculated, can fast and accurately detect phosphorus element content.
Specific implementation mode
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
The every other embodiment that technical staff is obtained, shall fall within the protection scope of the present invention.
Embodiment 1：
Preparing experiment reagent：Sodium molybdate（AR）；Citric acid（AR）；Nitric acid：50%（V/V）Salpeter solution；Quinoline；Acetone；Hydrochloric acid：
20%（V/V）Hydrochloric acid solution；
One：Prepare quinoline molybdenum lemon ketone solution：
A. 70g sodium molybdates is taken to be dissolved in 100ml water；
B. 60g citric acids is taken to be dissolved in 150ml water and 85ml nitric acid；
C. solution a is poured into solution b under stiring, mixing；
D. 35ml nitric acid and 5ml quinoline are added in 100ml water；
E. solution d is poured into solution c, mixing, stands a night, is filtered with filter paper, 280ml acetone is added in filtrate, is spent
Ionized water is diluted to 1000ml.Solution is stored in polyethylene bottle, is put in dark place, and shading is Protected from Heat.
Two：Inspection process
1. it is m to weigh 0.04g sample records, it is positioned in 100ml beakers, a small amount of water is added to soak, 20% salt of 5ml is added along wall of cup
Acid waits for that sample is completely dissolved on hot plate with 180 DEG C of heating for dissolving samples；
2. the solution prepared is placed in 500ml beakers, beaker inner wall is rinsed with 10ml deionized waters, is added 50%（V/V）Nitric acid
Solution adds water to total volume about 100ml, and heating is boiled, and adds 45ml quinoline molybdenum lemon ketone solution, cap upper surface ware, in water-bath 100
DEG C heating and thermal insulation is added in reagent and heating process, must not use open fire, must not stir.Beaker is taken out to be cooled to room temperature, it is cooling
It stirs 3 times in the process；
3. filtering：180 DEG C dry G4 sintered glass funnels to constant weight, quality m2, by supernatant liquid filtering, decantation is rinsed with wash bottle
Precipitation several times, every time with water about 30ml, is finally moved into sintered glass funnel and is filtered, precipitation is being washed with water 6 times, be put by precipitation
Thermostatic drying chamber, 180 DEG C of drying temperature after drying 45min, move into cooling 30min in drier, until constant weight, quality of weighing are
m1。
4. blank assay：Blank assay is carried out, the quality of record blank assay gained phosphomolybdic acid quinoline precipitation is m3
5. phosphorus element content result calculates：
Wp=（m1-m2-m3）× 0.01400/m × 100%, wherein
m1The quality of phosphomolybdic acid quinoline precipitation and sintered glass funnel is generated in-testing liquid；
m2The quality of sintered glass funnel in-experiment；
m3The quality of phosphomolybdic acid quinoline obtained by-blank assay；
The quality of m-sample；
0.01400 --- phosphomolybdic acid quinoline precipitates the coefficient for being scaled phosphorus quality.
In conclusion by means of the above-mentioned technical proposal of the present invention, is dissolved by heating, be completely dissolved by sample plus hydrochloric acid
Afterwards, with nitre acid-conditioning solution to appropriate acid or alkali environment, after heating is boiled, quinoline molybdenum lemon ketone solution is added, heating water bath heat preservation is formed
Precipitation is cleaned precipitation, is filtered, dries, weighs, phosphorus element content is calculated, can fast and accurately detect P elements
Content.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
With within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention god.
Claims (6)
1. a kind of charcoal composite lithium iron phosphate cathode material phosphorus element content detection method, which is characterized in that include the following steps：
S1. sample to be tested is weighed, record quality is m；
S2. sample treatment：Sample to be determined is placed in equipped with 20%（V/V）In the container of hydrochloric acid, it is complete to be heated to sample to be determined
Dissolving；
S3. precipitation reaction is carried out：The sample solution that step S2 is completely dissolved is with 50%（V/V）Nitric acid and water constant volume, water-bath add
Supernatant liquor and precipitation is obtained by the reaction to excessive quinoline molybdenum lemon ketone solution, heating water bath heat preservation after 98-100 DEG C, is added in heat；
S4. it cools down：Postcooling that the reaction was complete is to room temperature；
S5. it filters：By sintered glass funnel, drying to constant weight, and record quality is m2, by described in step S4 supernatant liquor and precipitation move
Enter sintered glass funnel to be filtered, be precipitated, by washing, drying, be cooled to constant weight and weigh, record quality is m1；
S6. blank assay：Step S1-S5 is carried out at the same time blank assay, and wherein step S5 blank assays result is m3；
S7. phosphorus element content result calculates：Wp=（m1-m2-m3）× 0.01400/m × 100%, wherein
m1The quality of phosphomolybdic acid quinoline precipitation and sintered glass funnel is generated in-testing liquid；
m2The quality of sintered glass funnel in-experiment；
m3The quality of phosphomolybdic acid quinoline obtained by-blank assay；
The quality of m-sample；
0.01400 --- phosphomolybdic acid quinoline precipitates the coefficient for being scaled phosphorus quality.
2. a kind of charcoal composite lithium iron phosphate cathode material phosphorus element content detection method, feature exist according to claim 1
In the preparation method of quinoline molybdenum lemon ketone solution described in step S3 is：It takes 70g sodium molybdates to be dissolved in 100ml water, obtains solution A；Take 60g
Citric acid is dissolved in 150ml water and 85ml nitric acid, obtains solution B；Solution A is poured into solution B under stiring, mixing obtains solution C；
35ml50% is added in 100ml water（V/V）Nitric acid and 5ml quinoline, obtain solution D；Solution D is poured into solution C, mixing, is stood
It at one night, is filtered with filter paper, 280ml acetone is added in filtrate, 1000ml is diluted to deionized water, obtain quinoline molybdenum lemon ketone solution.
3. a kind of charcoal composite lithium iron phosphate cathode material phosphorus element content detection method, feature exist according to claim 2
In the quinoline molybdenum lemon ketone solution configured is stored in polyethylene bottle, is put in dark place, shading is Protected from Heat.
4. a kind of charcoal composite lithium iron phosphate cathode material phosphorus element content detection method, feature exist according to claim 1
In heating temperature described in step S2 is 180 DEG C.
5. a kind of charcoal composite lithium iron phosphate cathode material phosphorus element content detection method, feature exist according to claim 1
In being precipitated after being filtered described in step S5, through water washing 5-6 times.
6. a kind of charcoal composite lithium iron phosphate cathode material phosphorus element content detection method, feature exist according to claim 1
In drying temperature described in step S5 is 180 DEG C, drying time 45min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111077036A (en) * | 2019-12-30 | 2020-04-28 | 广州傲农生物科技有限公司 | Rapid determination method for detecting content of ferrous iron in various iron additives |
| CN114112783A (en) * | 2021-11-26 | 2022-03-01 | 佛山市德方纳米科技有限公司 | Method for detecting lithium content in lithium phosphate |
| CN114318009A (en) * | 2022-03-16 | 2022-04-12 | 中南大学 | Method for recovering lithium from lithium iron phosphate |
-
2018
- 2018-01-04 CN CN201810007606.6A patent/CN108362606A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111077036A (en) * | 2019-12-30 | 2020-04-28 | 广州傲农生物科技有限公司 | Rapid determination method for detecting content of ferrous iron in various iron additives |
| CN114112783A (en) * | 2021-11-26 | 2022-03-01 | 佛山市德方纳米科技有限公司 | Method for detecting lithium content in lithium phosphate |
| CN114318009A (en) * | 2022-03-16 | 2022-04-12 | 中南大学 | Method for recovering lithium from lithium iron phosphate |
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Application publication date: 20180803 |
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