CN109298128A - Propene carbonate catalyst for synthesizing detection method of content and device - Google Patents
Propene carbonate catalyst for synthesizing detection method of content and device Download PDFInfo
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- CN109298128A CN109298128A CN201811300796.7A CN201811300796A CN109298128A CN 109298128 A CN109298128 A CN 109298128A CN 201811300796 A CN201811300796 A CN 201811300796A CN 109298128 A CN109298128 A CN 109298128A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
- G01N31/162—Determining the equivalent point by means of a discontinuity
- G01N31/164—Determining the equivalent point by means of a discontinuity by electrical or electrochemical means
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
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Abstract
The present invention relates to a kind of propene carbonate catalyst for synthesizing detection method of content and devices.Its technical solution is: beaker is installed in the top of temperature control magnetic agitation, beaker is provided with sample and mixing match solvent, magnetic rotor drives stirring, and brown buret, glass calomel reference electrode, silver electrode are installed in beaker, and glass calomel reference electrode and the other end of silver electrode are connect with pH meter respectively.The present invention has the advantage that using pH meter and calomel reference electrode, silver electrode as main current potential monitoring device, using chemistry titration as means, stoichiometric point is judged by constant-current titration, indicator electrode response is rapid, energy fast and stable, it reappears good, conventional method ratio, it is obvious with terminal, it avoids using indicator, the interference artificially not judged, data directly objectively reflect actual result, the exact level for accurately having detected propylene carbonate ester catalyst is realized to analyze data and instruct industrial important meaning.
Description
Technical field
The present invention relates to a kind of analysis test method of new energy field and device, in particular to a kind of propene carbonate closes
At with catalyst content detection method and device.
Background technique
Propene carbonate has consequence as one of in lithium ion battery five big solvents, in new energy industry,
Iodide catalyst content affects the quality of product and produces steady and process units energy consumption, material consumption, accurately detects it
Content has important role to product with stable quality and control production cost.
Propene carbonate is a kind of flammable liquid of no color or smell, is dissolved each other with ether, acetone, benzene, chloroform, vinyl acetate etc., molten
Very strong to the absorbability of carbon dioxide in water and carbon tetrachloride, property is stablized, and industrially takes propylene oxide and carbon dioxide
Addition under a certain pressure, then vacuum distillation is made, and can be used for oil-based solvent, spin solvent, alkene, aromatic hydrocarbons extraction agent, two
Absorbent carbon is aoxidized, water-soluble dye and the dispersing agent of pigment etc. are equally the important components of lithium-ion battery electrolytes.
Analysis in industry about catalyst active component iodide ion is argentometry, carries out judging chemical meter using indicator
Measure the terminal of point.But in actually detected, the iodide catalyst newly prepared passes through using polymerizeing at high temperature under high pressure, out
Now change colour, solution colour becomes dark brown from yellow and solubility in water reduces, and solution rate is slack-off, interferes in titration
Terminal colour judgement.In addition, the iodide catalyst will appear polymerization in use in the industrial production, using conventional molten
Agent cannot be completely dissolved, and a kind of proportion solvent of mixing need to be used quickly to dissolve the propene carbonate of catalyst and its absorption.
The present invention routinely uses indicator and artificial using the kits such as pH meter, reference electrode, silver electrode combination replacement
Judge terminal, uses a kind of solvent substitution of mixing match is conventional to use water as solvent in dissolved samples.
Summary of the invention
The purpose of the present invention is to drawbacks described above of the existing technology, a kind of propylene carbonate Lipase absobed is provided with urging
Agent detection method of content and device.
A kind of propene carbonate catalyst for synthesizing content detection device that the present invention mentions, technical solution is: detection
Device includes brown buret (1), glass calomel reference electrode (2), silver electrode (3), pH meter (4), beaker (5), temperature control magnetic force
(6), magnetic rotor (7) are stirred, the beaker (5) is installed in the top of temperature control magnetic agitation (6), and beaker (5) is provided with sample
And mixing match solvent, magnetic rotor (7) drive stirring, and brown buret (1), glass calomel ginseng are installed in beaker (5)
Than electrode (2), silver electrode (3), and glass calomel reference electrode (2) and the other end of silver electrode (3) connect with pH meter (4) respectively
It connects.
Preferably, above-mentioned brown buret (1) is using the brown buret that 0.05mol/L silver nitrate is housed.
Preferably, above-mentioned glass calomel reference electrode (2) uses 232 type glass calomel reference electrodes.
The propene carbonate catalyst for synthesizing detection method of content that the present invention mentions, technical solution be include following step
It is rapid:
(1) sample to be tested is taken, is placed in 250 milliliters of beakers；
(2) 150 milliliters of mixing match solvents are added, its ratio be ethyl alcohol: isopropanol: water=1:1.5:1；
(3) it is put into magnetic rotor, is placed on temperature control magnetic stirring apparatus, temperature setting is 25 degree；It opens stirring and slowly adjusts revolving speed
Fluid center is set to generate suitable whirlpool, the catalyst of beaker bottom has been stirred and catalyst is dissolved almost completely or is all crushed
After uniform fragment, speed of agitator is slowly adjusted to stopping is stirred, moving down electrode support makes the lower part of electrode away from beaker bottom
Distance is properly to guarantee that rotor will not encounter any electrode, then slowly tunes up revolving speed to suitable mixing speed；
(4) pH meter power switch is opened, gear is converted to " m v " shelves, starts to instill silver nitrate standard drop after current potential is stablized
Determine 1.0 milliliters of solution, record titration volumes and current potential millivolt number after current potential is basicly stable every time drip silver nitrate standard before titration
Solution is determined full of buret and adjusting liquid level makes reading be zeroed；Continue to titrate, and records titration volumes and current potential；Become according to current potential
Volume is added dropwise in the size degree appropriate adjustment of change, the drop that 0.10 milliliter of standard solution is added dropwise when potential change being made to be more than or equal to 60mV
The average value for determining volume and last time titration volumes is terminal volume V；There there is no buret tip during titration iodide catalyst
The part for falling into titrated solution can be flushed in titrated solution with a small amount of distilled water；
(5) after the completion of titrating, electrode is taken out after slowly stopping stirring, wipes reference electrode and silver electrode with filter paper, then with distilling
Water is rinsed well, and the electrode distilled water immersion cleaned up is spare；
(6) catalyst content X:
In formula: X-catalyst content, %；
C-silver nitrate standard titration solution volume V-titration end-point volume, ml.
Preferably, above-mentioned sample to be tested weighs 0.2 to 0.3 gram using the new iodide catalyst just prepared.
Preferably, above-mentioned sample to be tested, which is used, weighs 0.9 in the used iodide catalyst of propylene carbonate ester apparatus
To 1.1 grams.
Preferably, in step 3, basicly stable standard is that potential change per minute is no more than 6mV.
Preferably, in step 4, potential change increase when, gradually interval volume shorten to 0.50 milliliter, 0.30 milliliter,
0.20 milliliter, 0.10 milliliter.
The beneficial effects of the present invention are:
(1) experimental method provides a kind of effective ways for detection propylene carbonate catalyst for ester synthesis content, solves industry
Propene carbonate catalyst content is unable to the problem of accurate quantitative analysis in production；
(2) for this method using chemistry titration as analysis means, cooperation pH meter, reference electrode, silver electrode take silver electricity in monitoring solution
The potential difference of pole and silver ion overcomes conventional method using indicator, and terminal colour is not easy to judge, the disadvantage of reproducibility difference；
(3) it in addition to using instrument combination, using mixing match solvent, dissolves sample quickly, thoroughly, saves analysis time, protect
The authentic and valid of analysis data is demonstrate,proved.
Detailed description of the invention
Attached drawing 1 is structural schematic diagram of the invention；
In upper figure: brown buret 1, glass calomel reference electrode 2, silver electrode 3, pH meter 4, beaker 5, temperature control magnetic agitation 6, magnetic
Power rotor 7.
Specific embodiment
Hereinafter, preferred embodiments of the present invention will be described with reference to the accompanying drawings, it should be understood that preferred reality described herein
Apply example only for the purpose of illustrating and explaining the present invention and is not intended to limit the present invention.
Embodiment 1, referring to attached drawing 1, a kind of propene carbonate catalyst for synthesizing content detection device that the present invention mentions,
Its technical solution is: detection device include brown buret (1), glass calomel reference electrode (2), silver electrode (3), pH meter (4),
Beaker (5), temperature control magnetic agitation (6), magnetic rotor (7), the beaker (5) are installed in the top of temperature control magnetic agitation (6), burn
Cup (5) is provided with sample and mixing match solvent, and magnetic rotor (7) drives stirring, and installs brown buret in beaker (5)
(1), glass calomel reference electrode (2), silver electrode (3), and glass calomel reference electrode (2) and the other end of silver electrode (3) point
It is not connect with pH meter (4).
Preferably, above-mentioned brown buret (1) is using the brown buret that 0.05mol/L silver nitrate is housed.
Preferably, above-mentioned glass calomel reference electrode (2) uses 232 type glass calomel reference electrodes.
The propene carbonate catalyst for synthesizing detection method of content that the present invention mentions, comprising the following steps:
(1) weighing certain mass sample to be tested, (note: the new iodide catalyst just prepared weighs 0.2 to 0.3 gram, is placed in
In 250 milliliters of beakers；
(2) 150 milliliters of mixing match solvents (ethyl alcohol: isopropanol: water=1:1.5:1) are added；
(3) it is put into magnetic rotor, is placed on temperature control magnetic stirring apparatus, temperature setting is 25 degree.It opens stirring and slowly adjusts revolving speed
Fluid center is set to generate suitable whirlpool, the catalyst of beaker bottom has been stirred and catalyst is dissolved almost completely or is all crushed
After uniform fragment, speed of agitator is slowly adjusted to stopping is stirred, moving down electrode support makes the lower part of electrode away from beaker bottom
Distance is properly to guarantee that rotor will not encounter any electrode, then slowly tunes up revolving speed to suitable mixing speed.
(4) pH meter power switch is opened, gear is converted to " m v " shelves, (the basicly stable standard after current potential is stablized
It is that potential change per minute is no more than 6mV) start to instill 1.0 milliliters of silver nitrate standard titration solution, the basicly stable postscript of current potential
Silver nitrate standard titration solution (note: full of buret and is adjusted liquid level before titration every time by record titration volumes and current potential millivolt number
Reading is set to be zeroed)；Continue to titrate, and records titration volumes and current potential.It is added dropwise according to the size degree appropriate adjustment of potential change
Interval volume (when potential change increases, is gradually shortened to 0.50 milliliter, 0.30 milliliter, 0.20 milliliter, 0.10 milliliter) by volume,
The average value of 0.10 milliliter of standard solution is added dropwise when potential change being made to be more than or equal to 60mV titration volumes and last time titration volumes
For terminal volume V.The part that buret tip does not fall into titrated solution during titration iodide catalyst can be with less
Amount distilled water is flushed in titrated solution.
(5) after the completion of titrating, electrode is taken out after slowly stopping stirring, wipes reference electrode and silver electrode with filter paper, then use
Distilled water flushing is clean, and the electrode distilled water immersion cleaned up is spare.
(6) catalyst content X:
In formula: X-catalyst content, %；
C-silver nitrate standard titration solution volume；V-titration end-point volume, ml；M-weighs sample to be tested and mixing match
The gross mass of solvent.
The present invention, which has the advantage that, uses pH meter and calomel reference electrode, silver electrode as main current potential monitoring device,
Using chemistry titration as means, stoichiometric point is judged by constant-current titration.Rapidly, energy fast and stable reappears for indicator electrode response
Well.Conventional method ratio is had terminal obvious, avoids the interference artificially not judged using indicator, data are directly objective
Reflect actual result.
Solution rate is accelerated by using proportion solvent, improves dissolubility.By using standard solution and instrument combination essence
The exact level for really having detected propylene carbonate ester catalyst is realized to analyze data and instruct industrial important meaning.
Embodiment 2, the propene carbonate catalyst for synthesizing detection method of content that the present invention mentions, comprising the following steps:
(1) certain mass sample to be tested is weighed, for weighing 0.9 in the used iodide catalyst of propylene carbonate ester apparatus
To 1.1 grams, it is placed in 250 milliliters of beakers；
(2) 150 milliliters of mixing match solvents (ethyl alcohol: isopropanol: water=1:1.5:1) are added；
(3) it is put into magnetic rotor, is placed on temperature control magnetic stirring apparatus, temperature setting is 25 degree.It opens stirring and slowly adjusts revolving speed
Fluid center is set to generate suitable whirlpool, the catalyst of beaker bottom has been stirred and catalyst is dissolved almost completely or is all crushed
After uniform fragment, speed of agitator is slowly adjusted to stopping is stirred, moving down electrode support makes the lower part of electrode away from beaker bottom
Distance is properly to guarantee that rotor will not encounter any electrode, then slowly tunes up revolving speed to suitable mixing speed.
(4) pH meter power switch is opened, gear is converted to " m v " shelves, (the basicly stable standard after current potential is stablized
It is that potential change per minute is no more than 6mV) start to instill 1.0 milliliters of silver nitrate standard titration solution, the basicly stable postscript of current potential
Silver nitrate standard titration solution (note: full of buret and is adjusted liquid level before titration every time by record titration volumes and current potential millivolt number
Reading is set to be zeroed)；Continue to titrate, and records titration volumes and current potential.It is added dropwise according to the size degree appropriate adjustment of potential change
Interval volume (when potential change increases, is gradually shortened to 0.50 milliliter, 0.30 milliliter, 0.20 milliliter, 0.10 milliliter) by volume,
The average value of 0.10 milliliter of standard solution is added dropwise when potential change being made to be more than or equal to 60mV titration volumes and last time titration volumes
For terminal volume V.The part that buret tip does not fall into titrated solution during titration iodide catalyst can be with less
Amount distilled water is flushed in titrated solution.
(5) after the completion of titrating, electrode is taken out after slowly stopping stirring, wipes reference electrode and silver electrode with filter paper, then use
Distilled water flushing is clean, and the electrode distilled water immersion cleaned up is spare.
(6) catalyst content X:
In formula: X-catalyst content, %；
C-silver nitrate standard titration solution volume；V-titration end-point volume, ml；M-weighs sample to be tested and mixing match
The gross mass of solvent.
The above, is only part preferred embodiment of the invention, and anyone skilled in the art may benefit
Equivalent technical solution is modified or is revised as with the technical solution of above-mentioned elaboration.Therefore, technology according to the present invention
Any simple modification or substitute equivalents that scheme is carried out, belong to the greatest extent the scope of protection of present invention.
Claims (8)
1. a kind of propene carbonate catalyst for synthesizing content detection device, it is characterized in that: detection device includes brown buret
(1), glass calomel reference electrode (2), silver electrode (3), pH meter (4), beaker (5), temperature control magnetic agitation (6), magnetic rotor
(7), the beaker (5) is installed in the top of temperature control magnetic agitation (6), and beaker (5) is provided with sample and mixing match solvent,
Magnetic rotor (7) drives stirring, and installs brown buret (1), glass calomel reference electrode (2), silver electrode in beaker (5)
(3), and glass calomel reference electrode (2) and the other end of silver electrode (3) are connect with pH meter (4) respectively.
2. propene carbonate catalyst for synthesizing content detection device according to claim 1, it is characterized in that: the brown
Buret (1) is using the brown buret that 0.05mol/L silver nitrate is housed.
3. propene carbonate catalyst for synthesizing content detection device according to claim 1, it is characterized in that: the glass
Calomel reference electrode (2) uses 232 type glass calomel reference electrodes.
4. a kind of propene carbonate catalyst for synthesizing detection method of content as claimed in any one of claims 1-3, special
Sign be the following steps are included:
(1) sample to be tested is taken, is placed in 250 milliliters of beakers；
(2) 150 milliliters of mixing match solvents are added, its ratio be ethyl alcohol: isopropanol: water=1:1.5:1；
(3) it is put into magnetic rotor, is placed on temperature control magnetic stirring apparatus, temperature setting is 25 degree；It opens stirring and slowly adjusts revolving speed
Fluid center is set to generate suitable whirlpool, the catalyst of beaker bottom has been stirred and catalyst is dissolved almost completely or is all crushed
After uniform fragment, speed of agitator is slowly adjusted to stopping is stirred, moving down electrode support makes the lower part of electrode away from beaker bottom
Distance is properly to guarantee that rotor will not encounter any electrode, then slowly tunes up revolving speed to suitable mixing speed；
(4) pH meter power switch is opened, gear is converted to " m v " shelves, starts to instill silver nitrate standard drop after current potential is stablized
Determine 1.0 milliliters of solution, record titration volumes and current potential millivolt number after current potential is basicly stable every time drip silver nitrate standard before titration
Solution is determined full of buret and adjusting liquid level makes reading be zeroed；Continue to titrate, and records titration volumes and current potential；Become according to current potential
Volume is added dropwise in the size degree appropriate adjustment of change, the drop that 0.10 milliliter of standard solution is added dropwise when potential change being made to be more than or equal to 60mV
The average value for determining volume and last time titration volumes is terminal volume V；There there is no buret tip during titration iodide catalyst
The part for falling into titrated solution can be flushed in titrated solution with a small amount of distilled water；
(5) after the completion of titrating, electrode is taken out after slowly stopping stirring, wipes reference electrode and silver electrode with filter paper, then with distilling
Water is rinsed well, and the electrode distilled water immersion cleaned up is spare；
(6) catalyst content X:
In formula: X-catalyst content, %；
C-silver nitrate standard titration solution volume V-titration end-point volume, ml.
5. propene carbonate catalyst for synthesizing detection method of content according to claim 4, it is characterized in that: it is described to
Sample weighs 0.2 to 0.3 gram using the new iodide catalyst just prepared.
6. propene carbonate catalyst for synthesizing detection method of content according to claim 4, it is characterized in that: it is described to
Sample, which is used, weighs 0.9 to 1.1 gram in the used iodide catalyst of propylene carbonate ester apparatus.
7. propene carbonate catalyst for synthesizing detection method of content according to claim 4, it is characterized in that: in step 3
In, basicly stable standard is that potential change per minute is no more than 6mV.
8. propene carbonate catalyst for synthesizing detection method of content according to claim 4, it is characterized in that: step 4
In, when potential change increases, interval volume is gradually shortened to 0.50 milliliter, 0.30 milliliter, 0.20 milliliter, 0.10 milliliter.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114113458A (en) * | 2020-08-25 | 2022-03-01 | 中国石油化工股份有限公司 | Test device for evaluating mutual dissolution rate of acidified mutual solvent and use method |
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