CN109856315A - The detection method of free amine content in a kind of NMP - Google Patents
The detection method of free amine content in a kind of NMP Download PDFInfo
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- CN109856315A CN109856315A CN201811543271.6A CN201811543271A CN109856315A CN 109856315 A CN109856315 A CN 109856315A CN 201811543271 A CN201811543271 A CN 201811543271A CN 109856315 A CN109856315 A CN 109856315A
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Abstract
The present invention relates to a kind of detection methods of free amine content in NMP, including (1) to stock up；(2) indicator solution is prepared；(3) conical flask is put on an electronic balance, peeling, measures 50mLNMP with graduated cylinder and pour into conical flask, accurately weighs the quality of NMP, be denoted as m；(4) 50mL dehydrated alcohol and 3-4 drop bromocresol green-methyl red indicator are sequentially added into conical flask, steady shake makes it uniformly；(5) with the titration of the hydrochloric acid standard solution of 0.01mol/L by green to yellowish and keep the consumption volume V of the colour-fast record hydrochloric acid standard solution of 30s；(6) make blank test simultaneously, record the consumption volume V of hydrochloric acid standard solution0；(7) it calculates.Diluent is made using dehydrated alcohol in the detection method of unhindered amina in NMP of the invention, instead of original method using isopropanol as diluent, dehydrated alcohol has many advantages, such as that safety and environmental protection, low toxicity, chemical property be not stable, oxidizable, cheap relative to other diluents, is the good diluent that unhindered amina detects in NMP.
Description
Technical field
The invention belongs to chemicals detection technique field, it is related to detecting the detection of lithium battery industry raw material, more particularly to
The detection method of free amine content in a kind of NMP.
Background technique
New energy industry national policy support at present is quickly grown, and the new energy battery development as core is also prominent winged violent
Into, but regardless of be binder or cathode are done to PVDF main material graphite and conductive agent in terms of, all can't do without raw material NMP
(N-Methyl pyrrolidone) can effectively dissolve PVDF and it is enabled to have better caking property, in graphite material in intermediate effect
A small amount of NMP, which is added, also can improve the wellability of graphite, mix it preferably with binder, the final quality for improving battery.
But NMP can contain a small amount of raw material unhindered amina due to its production technology, but belong to impurity in finished product, contain
The problems such as measuring the excessively high quality that will affect lithium battery, causing self-discharge of battery.There are no effective for the detection of unhindered amina in NMP at present
Efficiently detection method cannot accurately evaluate NMP performance.
Summary of the invention
In order to solve the above technical problem, the present invention provides a kind of detection methods of free amine content in NMP, with realization pair
The accurate detection of unhindered amina in NMP.Diluent is made using dehydrated alcohol in the detection method of unhindered amina in NMP of the invention, is taken
For original method using isopropanol as diluent, dehydrated alcohol has safety and environmental protection, low toxicity, change relative to other diluents
The advantages that property is not stable, oxidizable, cheap is learned, is the good diluent that unhindered amina detects in NMP.
The present invention is achieved through the following technical solutions, and the present invention provides a kind of detection side of free amine content in NMP
Method includes the following steps:
(1) it stocks up: hydrochloric acid standard solution, bromocresol green-methyl red indicator, dehydrated alcohol, NMP finished product；
(2) indicator solution is prepared:
Solution I: the ethanol solution of bromocresol green, concentration 0.1g/100mL are prepared；
Solution II: the ethanol solution of methyl red, concentration 0.1g/50mL are prepared；
30ml solution I, 10ml solution II are taken, is uniformly mixed；
Solution III: hydrochloric acid solution is prepared；
(3) conical flask is put on an electronic balance, peeling, measures 50mLNMP with graduated cylinder and pour into conical flask, accurately weighs
The quality of NMP, is denoted as m；
(4) 50mL dehydrated alcohol and 3-4 drop bromocresol green-methyl red indicator are sequentially added into conical flask, are steadily shaken
It is dynamic to make it uniformly；
(5) with the titration of the hydrochloric acid standard solution of 0.01mol/L by green to yellowish and keep the colour-fast record hydrochloric acid of 30s
The consumption volume V of standard solution；
(6) make blank test simultaneously, record the consumption volume V of hydrochloric acid standard solution0；
(7) it calculates
In formula:
C-hydrochloric acid standard solution concentration, mol/L；
V-titration consumption hydrochloric acid standard solution volume, mL；
V0- blank assay consumes the volume of hydrochloric acid standard solution, mL；
M-monomethyl amine molal weight, 31.06g/mol；
The quality of the weighed NMP sample of m-, g.
Preferably, it in step (2), the preparation of solution I: accurately weighs 0.1g bromocresol green and is dissolved in dehydrated alcohol, use is anhydrous
Ethyl alcohol is diluted to 100mL.
Preferably, in step (2), the preparation of solution II: accurately weighing 0.2g methyl red, is dissolved in dehydrated alcohol, and use is anhydrous
Ethyl alcohol is diluted to 100mL.
Preferably, in step (2), it is desirable that the concentration of hydrochloric acid of preparation is in 0.01mol/L.
Preferably, in step (2), solution III: hydrochloric acid solution prepares the hydrochloric acid for providing to measure respective numbers according to following table, uses
Volumetric flask constant volume shakes up to 1000mL；
| The concentration c (HCl) of Hydrochloric Standard Titration]/(mol/L) | The volume V/mL of hydrochloric acid solution |
| 0.2 | 18 |
| 0.05 | 4.5 |
| 0.01 | 0.9 |
Preferably, in step (2), the calibration of HCl
The regulation of according to the form below weighs in 270 DEG C of -300 DEG C of high temperature furnaces calcination to the working standard reagent Carbon Dioxide of constant weight
Sodium is dissolved in 50mL water, adds 10 drop bromocresol green-methyl red indicators, is titrated to solution by green with prepared hydrochloric acid solution
Discoloration is kermesinus, boils 2min, continues to be titrated to solution to be again in kermesinus after cooling, while doing blank test；
| Concentration [c (HCl)]/(mol/L) of hydrochloric acid standard solution | The quality m/g of natrium carbonicum calcinatum |
| 0.2 | 0.2 |
| 0.05 | 0.05 |
| 0.01 | 0.01 |
The concentration [c (HCL)] of Hydrochloric Standard Titration, numerical value are indicated with mole every liter (moI/L)；Calculation formula:
The exact value of m-natrium carbonicum calcinatum quality, unit are (g)；
V1The numerical value of the volume of-hydrochloric acid solution, unit are milliliter (mL)；
V2The numerical value of the volume of-blank test hydrochloric acid solution, unit are milliliter (mL)；
The numerical value of M-natrium carbonicum calcinatum molal weight, unit be gram every mole (g/mol) [M (and 1 2Na2CO3)=
52.994]。
The invention has the benefit that
Diluent is made using dehydrated alcohol in the detection method of unhindered amina in NMP of the invention, instead of original with isopropyl
Method of the alcohol as diluent, dehydrated alcohol have safety and environmental protection, low toxicity, chemical property stable, no relative to other diluents
The advantages that oxidizable, cheap is the good diluent that unhindered amina detects in NMP.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
It obtains other drawings based on these drawings.
Fig. 1 is the very poor curve graph that alcohol and isopropanol do unhindered amina in embodiment 2.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
Application principle of the invention is further described combined with specific embodiments below.
Embodiment 1, the detection method of unhindered amina, includes the following steps: in a kind of couple of NMP
(1) it stocks up: hydrochloric acid standard solution, bromocresol green-methyl red indicator, dehydrated alcohol (content >=99.7%), NMP
Finished product；
(2) indicator solution is prepared:
Solution I: it accurately weighs 0.1g bromocresol green and is dissolved in dehydrated alcohol, be diluted to 100mL with dehydrated alcohol；
Solution II: accurately weighing 0.2g methyl red, be dissolved in dehydrated alcohol, is diluted to 100mL with dehydrated alcohol；
30ml solution I, 10ml solution II are taken, is uniformly mixed.
Solution III: hydrochloric acid solution is prepared
Provide that the acid hydrochloride salt for measuring respective numbers is shaken up with volumetric flask constant volume to 1000mL according to following table.
| The concentration c (HCl) of Hydrochloric Standard Titration]/(mol/L) | The volume V/mL of hydrochloric acid solution |
| 0.2 | 18 |
| 0.05 | 4.5 |
| 0.01 | 0.9 |
The calibration of HCl
The regulation of according to the form below weighs in 270 DEG C of -300 DEG C of high temperature furnaces calcination to the working standard reagent Carbon Dioxide of constant weight
Sodium is dissolved in 50mL water, adds 10 drop bromocresol green-methyl red indicators, is titrated to solution by green with prepared hydrochloric acid solution
Discoloration is kermesinus, boils 2min, continues to be titrated to solution to be again in kermesinus after cooling, while doing blank test.
| Concentration [c (HCl)]/(mol/L) of hydrochloric acid standard solution | The quality m/g of natrium carbonicum calcinatum |
| 0.2 | 0.2 |
| 0.05 | 0.05 |
| 0.01 | 0.01 |
The concentration [c (HCL)] of Hydrochloric Standard Titration, numerical value are indicated with mole every liter (moI/L).
Calculation formula:
The exact value of m-natrium carbonicum calcinatum quality, unit are (g)；
V1The numerical value of the volume of-hydrochloric acid solution, unit are milliliter (mL)；
V2The numerical value of the volume of-blank test hydrochloric acid solution, unit are milliliter (mL)；
The numerical value of M-natrium carbonicum calcinatum molal weight, unit be gram every mole (g/mol) [M (and 1 2Na2CO3)=
52.994]。
(3) conical flask is put on an electronic balance, peeling, measures 50mLNMP with graduated cylinder and pour into conical flask, accurately weighs
The quality of NMP, is denoted as m；
(4) 50mL dehydrated alcohol and 3-4 drop bromocresol green-methyl red indicator are sequentially added into conical flask, are steadily shaken
It is dynamic to make it uniformly；
(5) with the titration of the hydrochloric acid standard solution of 0.01mol/L by green to yellowish and keep the colour-fast record hydrochloric acid of 30s
The consumption volume V of standard solution；
(6) make blank test simultaneously, record the consumption volume V of hydrochloric acid standard solution0；
(7) it calculates
In formula:
C-hydrochloric acid standard solution concentration, mol/L (it is required that the concentration of hydrochloric acid prepared is in 0.01mol/L)；
V-titration consumption hydrochloric acid standard solution volume, mL；
V0- blank assay consumes the volume of hydrochloric acid standard solution, mL；
M-monomethyl amine molal weight, 31.06g/mol；
The quality of the weighed NMP sample of m-, g.
(1) indicator solution is prepared:
Solution I: it accurately weighs 0.1g bromocresol green and is dissolved in dehydrated alcohol, be diluted to 100mL with dehydrated alcohol；
Solution II: accurately weighing 0.2g methyl red, be dissolved in dehydrated alcohol, is diluted to 100mL with dehydrated alcohol；
30ml solution I, 10ml solution II are taken, is uniformly mixed.
Solution III: hydrochloric acid solution is prepared
Provide that the acid hydrochloride salt for measuring respective numbers is shaken up with volumetric flask constant volume to 1000mL according to following table.
(2) conical flask is put on an electronic balance, peeling, measures 50mLNMP with graduated cylinder and pour into conical flask, accurately weighs
The quality of NMP, is denoted as m；
(3) 50mL dehydrated alcohol and 3-4 drop bromocresol green-methyl red indicator are sequentially added into conical flask, are steadily shaken
It is dynamic to make it uniformly；
(4) with the titration of the hydrochloric acid standard solution of 0.01mol/L by green to yellowish and keep the colour-fast record hydrochloric acid of 30s
The consumption volume V of standard solution；
(5) make blank test simultaneously, record the consumption volume V of hydrochloric acid standard solution0；
(6) it calculates
In formula:
C-hydrochloric acid standard solution concentration, mol/L (it is required that the concentration of hydrochloric acid prepared is in 0.01mol/L)；
V-titration consumption hydrochloric acid standard solution volume, mL；
V0- blank assay consumes the volume of hydrochloric acid standard solution, mL；
M-monomethyl amine molal weight, 31.06g/mol；
The quality of the weighed NMP sample of m-, g.
Embodiment 2, original alcohol and isopropanol do the comparative experiments of unhindered amina
1, experiment purpose: analyzing alcohol and isopropanol does the gap of unhindered amina
2, experiment equipment: balance, 250ml conical flask
3, experimental procedure: 10 different samples of selection do unhindered amina.
Unhindered amina additive amount is divided into are as follows: 30 milliliters of NMP+30 milliliters of alcohol；30 milliliters of NMP+30 milliliters of isopropanols；
4, experimental result
Alcohol blank titration is 0.05ml；Isopropanol blank titration is 0.5ml
5, attached drawing 1, very poor average are as follows: 0.383 are shown in data processing
6, experiment conclusion: when doing unhindered amina, adding 30ml alcohol and when 30ml isopropanol, detection error zone of reasonableness it
It is interior.
Certainly, above description is also not limited to the example above, technical characteristic of the present invention without description can by or
It is realized using the prior art, details are not described herein；Above embodiments and attached drawing are only used to illustrate the technical scheme of the present invention not
It is limitation of the present invention, is described the invention in detail referring to preferred embodiment, the ordinary skill people of this field
Member is it should be appreciated that variation, remodeling, the addition that those skilled in the art are made within the essential scope of the present invention
Or replacement also should belong to claims of the invention without departure from spirit of the invention.
Claims (6)
1. the detection method of free amine content in a kind of NMP, characterized by the following steps:
(1) it stocks up: hydrochloric acid standard solution, bromocresol green-methyl red indicator, dehydrated alcohol, NMP finished product；
(2) indicator solution is prepared:
Solution I: the ethanol solution of bromocresol green, concentration 0.1g/100mL are prepared；
Solution II: the ethanol solution of methyl red, concentration 0.1g/50mL are prepared；
30ml solution I, 10ml solution II are taken, is uniformly mixed；
Solution III: hydrochloric acid solution is prepared；
(3) conical flask is put on an electronic balance, peeling, measures 50mLNMP with graduated cylinder and pour into conical flask, accurately weighs NMP
Quality, be denoted as m；
(4) 50mL dehydrated alcohol and 3-4 drop bromocresol green-methyl red indicator are sequentially added into conical flask, steady shake makes
It is uniformly；
(5) with the titration of the hydrochloric acid standard solution of 0.01mol/L by green to yellowish and keep the colour-fast record normal hydrochloric acid of 30s
The consumption volume V of solution；
(6) make blank test simultaneously, record the consumption volume V of hydrochloric acid standard solution0；
(7) it calculates
In formula:
C-hydrochloric acid standard solution concentration, mol/L；
V-titration consumption hydrochloric acid standard solution volume, mL；
V0- blank assay consumes the volume of hydrochloric acid standard solution, mL；
M-monomethyl amine molal weight, 31.06g/mol；
The quality of the weighed NMP sample of m-, g.
2. the detection method of free amine content in a kind of NMP according to claim 1, it is characterised in that: in step (2),
The preparation of solution I: it accurately weighs 0.1g bromocresol green and is dissolved in dehydrated alcohol, be diluted to 100mL with dehydrated alcohol.
3. the detection method of free amine content in a kind of NMP according to claim 1, it is characterised in that: in step (2),
The preparation of solution II: accurately weighing 0.2g methyl red, be dissolved in dehydrated alcohol, is diluted to 100mL with dehydrated alcohol.
4. the detection method of free amine content in a kind of NMP according to claim 1, it is characterised in that: in step (2),
It is required that the concentration of hydrochloric acid prepared is in 0.01mol/L.
5. the detection method of free amine content in a kind of NMP according to claim 1, it is characterised in that: in step (2),
Solution III: hydrochloric acid solution, which is prepared, provides that the hydrochloric acid for measuring respective numbers is shaken up with volumetric flask constant volume to 1000mL according to following table；
6. the detection method of free amine content in a kind of NMP according to claim 5, it is characterised in that: in step (2),
The calibration of HCl
The regulation of according to the form below weighs the working standard reagent natrium carbonicum calcinatum of in 270 DEG C of -300 DEG C of high temperature furnaces calcination to constant weight,
It is dissolved in 50mL water, adds 10 drop bromocresol green-methyl red indicators, be titrated to solution with prepared hydrochloric acid solution and become by green
For kermesinus, 2min is boiled, continues to be titrated to solution to be again in kermesinus after cooling, while doing blank test；
The concentration [c (HCL)] of Hydrochloric Standard Titration, numerical value are indicated with mole every liter (moI/L)；Calculation formula:
The exact value of m-natrium carbonicum calcinatum quality, unit are (g)；
V1The numerical value of the volume of-hydrochloric acid solution, unit are milliliter (mL)；
V2The numerical value of the volume of-blank test hydrochloric acid solution, unit are milliliter (mL)；
The numerical value of M-natrium carbonicum calcinatum molal weight, unit be gram every mole (g/mol) [M (and 1 2Na2CO3)=52.994].
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111638213A (en) * | 2020-07-14 | 2020-09-08 | 山东京博石油化工有限公司 | Method for detecting content of heat-stable salt in ethanolamine desulfurization solution |
| CN113702473A (en) * | 2021-08-26 | 2021-11-26 | 中国科学院青岛生物能源与过程研究所 | Method for measuring alkalinity of surfactant based on potentiometric titration method |
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| CN103134796A (en) * | 2011-12-02 | 2013-06-05 | 天津市捷威动力工业有限公司 | Method of testing content of free amine in nuclear matrix protein (NMP) |
| CN104458732A (en) * | 2014-12-15 | 2015-03-25 | 内蒙古包钢钢联股份有限公司 | Method for calibrating hydrochloric acid and sulfuric acid standard liquids by adopting sodium carbonate reference |
| CN107907625A (en) * | 2017-11-03 | 2018-04-13 | 山西长征动力科技有限公司 | A kind of detection method of lithium electricity tertiary cathode material surface residual alkali content |
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2018
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102243181A (en) * | 2011-04-08 | 2011-11-16 | 湖北富邦科技股份有限公司 | Method for detecting ammonia value of powdered anticaking agent |
| CN103134796A (en) * | 2011-12-02 | 2013-06-05 | 天津市捷威动力工业有限公司 | Method of testing content of free amine in nuclear matrix protein (NMP) |
| CN104458732A (en) * | 2014-12-15 | 2015-03-25 | 内蒙古包钢钢联股份有限公司 | Method for calibrating hydrochloric acid and sulfuric acid standard liquids by adopting sodium carbonate reference |
| CN107907625A (en) * | 2017-11-03 | 2018-04-13 | 山西长征动力科技有限公司 | A kind of detection method of lithium electricity tertiary cathode material surface residual alkali content |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111638213A (en) * | 2020-07-14 | 2020-09-08 | 山东京博石油化工有限公司 | Method for detecting content of heat-stable salt in ethanolamine desulfurization solution |
| CN113702473A (en) * | 2021-08-26 | 2021-11-26 | 中国科学院青岛生物能源与过程研究所 | Method for measuring alkalinity of surfactant based on potentiometric titration method |
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