CN110018219A - The quantitative and qualitative analytic systems and method of black carbon surface functional group - Google Patents
The quantitative and qualitative analytic systems and method of black carbon surface functional group Download PDFInfo
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- CN110018219A CN110018219A CN201811540642.5A CN201811540642A CN110018219A CN 110018219 A CN110018219 A CN 110018219A CN 201811540642 A CN201811540642 A CN 201811540642A CN 110018219 A CN110018219 A CN 110018219A
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Abstract
The present invention relates to the system and methods for quantitative and qualitative analysis black carbon surface functional group.According to the present invention, it compared to previous analysis method, can be quantified and the surface functional group of qualitative analysis carbon black with high accuracy and reliability.
Description
Technical field
The present invention relates to the system and methods of quantitative and qualitative analysis carbon black surface functional group.
Background technique
Recently, in order to using adjustment carbon black surface functional group carbon black or carbon black surface functional group chemical property,
Lasting research and development technology related with preparation and the carbon black for using surface modified.
In general, there is the surface functional group of carboxyl, lactone, phenolic hydroxyl group and carbonyl etc. on the surface of carbon black, it is well known that carbon
Black characteristic will generate big variation by the amount of this various surface functional groups.
For example, the hydrophily of carbon black improves, the phase with water solvent in the case where the surface of carbon black has many carboxyls
Capacitive is improved, and dispersibility is made to improve.On the other hand, in the case where the surface of carbon black has many phenolic group or hydroxyl, with
The related dieing activity such as cellulosic fibre and protein fibre is improved.
The type and content for adjusting the surface functional group of carbon black according to the purposes of desired carbon black as a result, is particularly important,
For this purpose, attempting the surface functional group of quantitative analysis carbon black.
The method of the surface functional group of previous quantitative analysis carbon black has elemental analysis method, titration, spectrum analysis side
Method etc..
Elemental analysis method is a kind of method that elemental analysis is carried out after being heat-treated at various temperatures to carbon black,
Belong to the method that surface functional group can be predicted by elemental analysis result difference.But have can not be by for elemental analysis method
The limitation of quantitative analysis is carried out according to surface functional group.
Also, representative most commonly used titration (titration) method is selecting solvent according to each surface functional group
The method to analyze surface functional group is titrated later, and the analysis method of titration has following limitation, that is, step is multiple
Miscellaneous, a part of surface functional group can not be titrated due to no solvent appropriate, and reproducibility is insufficient.
Frequency spectrum analysis method has point using x-ray photoelectron spectroscopy (XPS) or Fourier infrared spectrograph (FT-IR)
Analysis method.
Analysis method using x-ray photoelectron spectroscopy (X-ray photoelectron spectroscopy) is to carbon
The method that black X-ray irradiation (X-ray) carrys out quantitative analysis surface functional group to detect from the kinetic energy of the electronics of atom generation.But
It is that X-ray not only irradiates black carbon surface, also irradiates the inside of carbon black, therefore, have and be not suitable for use in being only used for analysis surface official
The problem of method that can be rolled into a ball.
Also, since carbon black has light absorbing property, have using the analysis method of Fourier infrared spectrograph
The low problem of the reliability of analysis.
Therefore, it is badly in need of research and development with higher Quantitative Reliability and the technology of the surface functional group of qualitative analysis carbon black.
Summary of the invention
The technical problem to be solved in the present invention
The object of the present invention is to provide with high accuracy and reliability and can make up previous analysis method as a result,
Low reproducibility quantitatively and qualitative analysis carbon black surface functional group system and method.
Technical solution
According to the one embodiment of the present invention for solving the above problems, a kind of quantifying for black carbon surface functional group is provided
And qualitative analytic systems, comprising: chamber accommodates carbon black sample；Temperature regulation section adjusts the internal temperature of above-mentioned chamber；Pressure
Test section detects the internal pressure of above-mentioned chamber；Gas outflow portion makes one in the mixed gas generated in above-mentioned chamber
It distributes；And quality analysis portion, analyze the quality of the mixed gas flowed out by above-mentioned gas outflow portion.
Also, another embodiment according to the present invention provides a kind of quantitative and qualitative analysis of black carbon surface functional group
Method, comprising: step (a) puts into carbon black sample into chamber；Step (b) makes the internal temperature of above-mentioned chamber heat up stage by stage
And cooling thermally decomposes come the surface functional group of the carbon black to each temperature range；Step (c) detects each temperature range
The internal pressure of above-mentioned chamber；And step (d), make a part outflow in the indoor mixed gas of above-mentioned chamber and according to structure
Above-mentioned mixed gas is divided at atom detects volume related with each gas divided later.
Beneficial effect
The analysis method of previous black carbon surface functional group has and can not carry out quantitative analysis or again according to surface functional group
The existing insufficient limitation of property.
But the present invention has the advantage that, that is, can each thermal decomposition temperature section of quantitative analysis carbon black surface
Functional group is contained in each of mixed gas carrying out four-electrode spectrum to the mixed gas obtained by thermal decomposition carbon black to divide
Qualitative analysis is carried out after kind gas.
Also, the quantitative and qualitative analysis of the surface functional group of carbon black as described above can in a system rapidly into
Row, to can provide the analysis result with more high accuracy and reliability.
Detailed description of the invention
Fig. 1 is quantitative and qualitative analytic systems the signal for schematically illustrating the black carbon surface functional group of one embodiment of the invention
Figure.
Fig. 2 is quantitative and method for qualitative analysis the process for schematically illustrating the black carbon surface functional group of one embodiment of the invention
Figure.
Fig. 3 is the humidity province for schematically illustrating an embodiment according to the present invention and being thermally decomposed to the surface functional group of carbon black
Between curve graph.
Specific embodiment
Specific term is defined in this application in order to be easier to understand the present invention for the sake of convenient.Unless another in this application
Row definition, the scientific term and technical term being used in the present invention are generally understood with those of ordinary skill in the art
Meaning.Also, unless particularly pointing out on context, the term of singular form further includes its plural form, the art of plural form
Language further includes its singular form.
Hereinafter, to it is of the invention quantitatively and the system and method for the surface functional group of qualitative analysis carbon black carry out it is more detailed
Explanation.
Fig. 1 be schematically illustrate the black carbon surface functional group of one embodiment of the invention quantitative and qualitative analytic systems (hereinafter,
Referred to as analysis system) schematic diagram.
Referring to Fig.1, the quantitative and qualitative analytic systems 100 of black carbon surface functional group include: chamber 110, receiving carbon black examination
Sample；Temperature regulation section 120 adjusts the internal temperature of chamber 110；And pressure detecting portion 130, the inside pressure of detection chambers 110
Power.
Chamber 110 have receiving carbon black sample space, accommodate carbon black sample after it is salable be vacuum state.Also,
Preferably, chamber 110 is ceramics or aluminium oxide chamber, not to be modified internal temperature maintains the condition of high temperature.
Temperature regulation section 120 is the unit for adjusting the internal temperature of chamber 110, makes chamber with the state of sealed chamber 110
110 internal temperature rises be thermal decomposited the surface functional group of carbon black.As the internal temperature of chamber 110 rises, carbon black
Surface functional group can be thermal decomposited as gas phase (gas phase).
Specifically, there can be various functional groups on the surface of carbon black, the thermal decomposition temperature of this functional group is former according to constituting
Son is different.
For example, the functional group of carboxyl, lactone group and-C-C-O-O-C- etc. can at a temperature of between 200 DEG C to 700 DEG C quilt
Thermal decomposition.
As a result, in order to by functional group as described above be used as target, make the internal temperature of chamber 110 be warming up to 700 DEG C it
Maintain the stipulated time afterwards to be decomposed into gas phase and then the secondary internal temperature for making chamber 110 by cooling from the surface heat of carbon black
Decline to analyze the gas phase for the inside for being present in chamber 110.
Also, the functional group of carbonyl, phenol and hydroxyl etc. can be thermal decomposited at a temperature of between 500 DEG C to 1200 DEG C.
As a result, in order to by functional group as described above be used as target, make the internal temperature of chamber 110 be warming up to 1200 DEG C it
Maintain the stipulated time afterwards to be decomposed into gas phase and then the secondary internal temperature for making chamber 110 by cooling from the surface heat of carbon black
Decline to analyze the gas phase for the inside for being present in chamber 110.
Also, the functional group of hydroxyl and hydrogen etc. can be thermal decomposited at a temperature of between 600 DEG C to 1600 DEG C.
As a result, in order to by functional group as described above be used as target, make the internal temperature of chamber 110 be warming up to 1600 DEG C it
Maintain the stipulated time afterwards to be decomposed into gas phase and then the secondary internal temperature for making chamber 110 by cooling from the surface heat of carbon black
Decline to analyze the gas phase for the inside for being present in chamber 110.
Therefore, in one embodiment of this invention, temperature regulation section 120 make the internal temperature of chamber 110 disposably from
Room temperature is warming up to 1600 DEG C be thermal decomposited the surface functional group of carbon black as described above all.Also, of the invention another
In one embodiment, it is considered as the thermal decomposition temperature of the surface functional group of the carbon black of target, temperature regulation section 120 can be so that chamber
110 internal temperature heats up stage by stage and cooling mode works.
In the case, temperature regulation section 120 can work in following temperature range, that is, at 200 DEG C to 700 DEG C
Temperature range heating after carry out the first temperature range t1 of cooling (for example, being cooled to room temperature), at 500 DEG C to 1200 DEG C
The second temperature section t2 that cooling (for example, being cooled to room temperature) is carried out after temperature range heating, in 600 DEG C to 1600 DEG C of temperature
The third temperature range t3 of cooling (for example, being cooled to room temperature) is carried out after degree range heating.But as described above by temperature
The upper and lower bound for spending temperature range range and temperature range that adjustment portion 120 is adjusted is the illustration of the preferred embodiment of the present invention,
Can the characteristic according to carbon black and the carbon black as target surface functional group type for solving the problems, such as scope of the invention
Within be suitably adjusted.
Also, temperature regulation section 120 can be after the surface functional group to carbon black thermally decomposes in cooling chamber 110
It is detected in the state of interrupting the thermal decomposition of surface functional group of carbon black to interrupt the thermal decomposition of the surface functional group of carbon black in portion
The internal pressure of chamber 110 flows out the gas being present in chamber 110.
Pressure detecting portion 130 is the unit of the internal pressure of detection chambers 110, on the internal temperature with chamber 110
It rises and to thermally decompose the surface functional group of carbon black be gas phase come in the case where being present in chamber, in the internal pressure of chamber 110
It rises, the detection of pressure detecting portion 130 carrys out quantitative analysis surface functional group in the increased pressure in the inside of chamber 110.
In the case, with the prominent form of pressure sensor in the inside of chamber 110, pressure passes pressure detecting portion 130
The position of sensor and form can be properly selected according to the shape etc. of chamber 110.
Pressure detecting portion 130 can be quantitatively identified through as the surface functional group of carbon black thermally decomposes as gas phase and increased chamber
The internal pressure of room 110 is come the molal quantity for the gas for being thermal decomposited and generating.
In the case, in one embodiment of this invention, pressure detecting portion 130 can make chamber in temperature regulation section 120
110 internal temperature is disposably warming up to 1600 DEG C from room temperature and examines later be thermal decomposited the surface functional group of carbon black all
Survey the internal pressure of chamber 110.Also, it in another embodiment of the invention, can consider to be used as target in temperature regulation section 120
Carbon black surface functional group thermal decomposition temperature come after making the internal temperature of chamber 110 heat up stage by stage and is cooling, by pressing
The internal pressure of 130 detection chambers 110 of power test section.
Preferably, through the internal pressures of 130 detection chambers 110 of pressure detecting portion, in order to prevent by
The pollution of outside atmosphere, in carrying out thermal decomposition to carbon black by temperature regulation section 120 and being detected by pressure detecting portion 130
During portion's pressure, chamber 110 maintains vacuum state.
If by 130 detection chambers 110 of pressure detecting portion after the surface functional group to carbon black completes thermal decomposition
Portion's pressure then will make the mixture with various gases be present in chamber 110.
Gas outflow portion 140 make the mixed gas in chamber 110 all or part of to quality analysis portion 150 flow
Out.
In this case it is preferably to which the mixed gas flowed out in order to prevent to quality analysis portion 150 is by outside atmosphere
Pollution, chamber 110, quality analysis portion 150 and connection chamber 110 and the gas outflow portion 140 in quality analysis portion 150 maintain
Vacuum state.
Also, gas outflow portion 140 may make temperature regulation section 120 make the internal temperature of chamber 110 disposably from
Room temperature be warming up to 1600 DEG C come make the surface functional group of carbon black be all thermal decomposited after generate mixed gas disposably to
It flows out in quality analysis portion 150.Also, in another embodiment of the invention, gas outflow portion 140 may make in temperature regulation section
120 make the internal temperature of chamber 110 heat up stage by stage in view of the thermal decomposition temperature of the surface functional group of the carbon black as target
And the cooling mixed gas generated later is flowed out according to each temperature range to quality analysis portion 150.
Quality analysis is carried out to the mixed gas flowed out in quality analysis portion 150, to confirm that the composition of gas is former
Son.
As a result, according to the present invention, it quantitatively determines the gas flow generated by pressure detecting portion 130 and distinguishes in quality analysis
The type for the gas that portion 150 generates to quantify and the surface functional group of qualitative analysis carbon black.
For this purpose, quality analysis portion 150 divided according to constituting atom from gas outflow portion 140 supply mixed gas it
Volume related with each gas divided is detected afterwards.
In one embodiment, it is preferable that quality analysis portion 150 is by quadrupole mass spectrometer (quadrupole mass
spectrometer；QMS it) realizes.
Quadrupole mass spectrometer is following mass spectrograph, that is, by make heat silk come thermoelectron outstanding and acceleration, in
Property particle encounter form ion, apply DC voltage to each pole and alternating voltage be pass through ion specific by only making to have
The mass filter that the four-electrode spectrum that the particle of mass/charge ratio passes through is formed, to detect the quality of neutral particle and ion.
The mass spectrum of gas phase in low-temperature plasma is simple, therefore, is contained in mixed gas to understanding fully using quadrupole mass spectrometer
Various gases and detect they amount it is very useful.
It wherein, include whole situation such as carbon dioxide, carbon monoxide and hydrogen in mixed gas in quadrupole mass spectrometer
Under, detection is related with each gas after mixed gas is respectively divided into carbon dioxide, carbon monoxide and hydrogen by quadrupole mass spectrometer
Volume so that can quantitatively and qualitative analysis carbon black surface functional group.
Fig. 2 is quantitative and method for qualitative analysis the flow chart of the black carbon surface functional group of one embodiment of the invention.
Referring to Fig. 2, the method for quantitative and qualitative analysis carbon black the surface functional group of one embodiment of the invention includes: step
(a), carbon black sample is put into chamber；Step (b) makes the internal temperature of above-mentioned chamber heat up and cool down to come to each stage by stage
The surface functional group of the carbon black of temperature range is thermally decomposed；Step (c) detects the inside of the above-mentioned chamber of each temperature range
Pressure；And step (d), so that a part in the indoor mixed gas of above-mentioned chamber is flowed out and is being divided according to constituting atom
It states mixed gas and detects volume related with each gas divided later.
The step of step (a) is puts into carbon black sample to the accommodating space being formed in chamber 110, can be in chamber 110
Chamber 110 is set to be sealed into vacuum state after receiving carbon black sample.
Then, step (b) is the step of thermal decomposition to the surface functional group of carbon black, to belong to temperature regulation section 120 and exist
Chamber 110 rises the internal temperature of chamber 110 to make the surface functional group of carbon black by heat point
The step of solution is gas phase (gas phase).
In the case, in one embodiment of this invention, the internal temperature of chamber 110 can be made primary by step (b)
Property risen to after 1600 DEG C from room temperature and be thermal decomposited the surface functional group of carbon black as described above all.Also, at this
It, can be by step (b) come in the thermal decomposition temperature of the surface functional group in view of the carbon black as target in another embodiment of invention
It spends to make the internal temperature of chamber 110 heat up and cool down stage by stage.
Fig. 3 is to schematically illustrate the humidity province thermally decomposed according to surface functional group of the embodiment as described above to carbon black
Between curve graph, referring to Fig. 3, in step (b), it may include cooled down after 200 DEG C to 700 DEG C of temperature ranges heating
The first temperature range t1,500 DEG C to 1200 DEG C temperature ranges heating after carry out cooling second temperature section t2 with
And cooling third temperature range t3 is carried out after 600 DEG C to 1600 DEG C of temperature range heating.
Specifically, there can be various functional groups on the surface of carbon black, the thermal decomposition temperature of this functional group can be according to composition
Atom and it is different.
For example, such as the functional group of carboxyl, lactone group and-C-C-O-O-C- can be at a temperature of between 200 DEG C to 700 DEG C
It is thermal decomposited.Functional group's thermal decomposition as described above is carbon dioxide.As a result, in order to functional group as described above to be used as
Target maintains the stipulated time to be decomposed into gas from the surface heat of carbon black after making the internal temperature of chamber 110 be warming up to 700 DEG C
Phase and then the secondary gas phase that the inside for being present in chamber 110 is analyzed by the cooling internal temperature decline for making chamber 110.
Also, the functional group of carbonyl, phenol and hydroxyl etc. can be thermal decomposited at a temperature of between 500 DEG C to 1200 DEG C.
Functional group's thermal decomposition as described above is carbon monoxide.
As a result, in order to by functional group as described above be used as target, make the internal temperature of chamber 110 be warming up to 1200 DEG C it
Maintain the stipulated time afterwards to be decomposed into gas phase and then the secondary internal temperature for making chamber 110 by cooling from the surface heat of carbon black
Decline to analyze the gas phase for the inside for being present in chamber 110.
Also, the functional group of hydroxyl and hydrogen etc. can be thermal decomposited at a temperature of between 600 DEG C to 1600 DEG C.As described above
Functional group's thermal decomposition be carbon monoxide or hydrogen.
As a result, in order to by functional group as described above be used as target, make the internal temperature of chamber 110 be warming up to 1600 DEG C it
Maintain the stipulated time afterwards to be decomposed into gas phase and then the secondary internal temperature for making chamber 110 by cooling from the surface heat of carbon black
Decline to analyze the gas phase for the inside for being present in chamber 110.
In the case, step (b) can work within the scope of following temperature, that is, in 200 DEG C to 700 DEG C of temperature
The first temperature range for carrying out cooling (for example, being cooled to room temperature) in degree range after heating, in 500 DEG C to 1200 DEG C of temperature
The second temperature section for carrying out cooling (for example, being cooled to room temperature) in range after heating, in 600 DEG C to 1600 DEG C of temperature model
Enclose the third temperature range that interior heating carries out cooling (for example, being cooled to room temperature) later.
But the upper and lower bound of the range of temperature range as described above and temperature range is the preferred embodiment of the present invention
Illustration, can the characteristic according to carbon black and the carbon black as target surface functional group type of the invention for solving the problems, such as
Scope within be suitably adjusted.
It, can be after the surface functional group to carbon black thermally decomposes in cooling chamber 110 also, in step (b)
Portion can examine in the state of interrupting the thermal decomposition of surface functional group of carbon black to interrupt the thermal decomposition of the surface functional group of carbon black
Survey the internal pressure of chamber 110.
The step of step (c) is the internal pressure of detection chambers 110 rises in the internal temperature with chamber 110 and is made
The surface functional group thermal decomposition of carbon black is gas phase come in the case where being present in chamber, the internal pressure of chamber 110 rises, detection
In the inside of chamber 110, increased pressure carrys out quantitative analysis surface functional group.
That is, can be quantitatively identified through by step (c) as the surface functional group thermal decomposition of carbon black is increased for gas phase
The internal pressure of chamber 110 is come the molal quantity for the gas for being thermal decomposited and generating.
After the internal pressure by step (c) detection chambers 110, the mixture of various gases is present in chamber 110.
Then, it in order to which qualitative analysis is present in the gas in chamber 110, executes so that the whole of the mixed gas in chamber 110 or one
The step of part is flowed out and is analyzed to quality analysis portion 150 (d).
In this case it is preferably to which the mixed gas flowed out in order to prevent to quality analysis portion 150 is by outside atmosphere
Pollution maintains analysis space and the external sealing state separated.
In step (d), 150 pairs of quality analysis portion, the mixed gas flowed out carries out quality analysis, so as to confirm
The constituting atom of gas.
As a result, according to the present invention, quantitative confirmation produces in the amount of the gas of generation and division in step (d) in step (c)
The type of raw gas, so as to quantitative and qualitative analysis carbon black surface functional group.
For this purpose, being divided according to constituting atom after the mixed gas that quality analysis portion 150 supplies in step (d)
Detect volume related with each gas divided.Wherein it is preferred to use quadrupole mass spectrometer in step (d)
(quadrupole mass spectrometer；QMS).It wherein, include carbon dioxide, carbon monoxide and hydrogen in mixed gas
In the case where, detection and each gas after mixed gas is respectively divided into carbon dioxide, carbon monoxide and hydrogen by quadrupole mass spectrometer
The related volume of body, so as to quantitative and qualitative analysis carbon black surface functional group.
More than, one embodiment of the invention is illustrated, those skilled in the art can be no more than
The present invention is carry out various modifications by additional, change, deletion or additional structural element etc. in the range of thought of the invention
And change, this also belongs to interest field of the invention.
Claims (10)
1. a kind of quantitative and qualitative analytic systems of black carbon surface functional group characterized by comprising
Chamber accommodates carbon black sample；
Temperature regulation section adjusts the internal temperature of above-mentioned chamber；
Pressure detecting portion detects the internal pressure of above-mentioned chamber；
Gas outflow portion makes a part outflow in the mixed gas generated in above-mentioned chamber；And
Quality analysis portion analyzes the type and quality of the mixed gas flowed out by above-mentioned gas outflow portion.
2. the quantitative and qualitative analytic systems of black carbon surface functional group according to claim 1, which is characterized in that above-mentioned temperature
Spend the thermal decomposition temperature for the surface functional group that adjustment portion makes the internal temperature of above-mentioned chamber rise to above-mentioned carbon black.
3. the quantitative and qualitative analytic systems of black carbon surface functional group according to claim 1, which is characterized in that above-mentioned pressure
Power test section detects the internal pressure of above-mentioned chamber after the thermal decomposition for carrying out above-mentioned carbon black.
4. the quantitative and qualitative analytic systems of black carbon surface functional group according to claim 1, which is characterized in that above-mentioned matter
Amount analysis portion detects volume related with each gas divided after dividing above-mentioned mixed gas according to constituting atom.
5. the quantitative and qualitative analytic systems of black carbon surface functional group according to claim 1, which is characterized in that above-mentioned chamber
Room, above-mentioned gas outflow portion and above-mentioned quality analysis portion maintain vacuum state.
6. a kind of quantitative and method for qualitative analysis of black carbon surface functional group characterized by comprising
Step (a) puts into carbon black sample into chamber；
Step (b) makes the internal temperature of above-mentioned chamber heat up and cool down the surface come to the carbon black of each temperature range stage by stage
Functional group is thermally decomposed；
Step (c) detects the internal pressure of the above-mentioned chamber of each temperature range；And
Step (d) makes a part outflow in the indoor mixed gas of above-mentioned chamber and is dividing above-mentioned mix according to constituting atom
It closes gas and detects volume related with each gas divided later.
7. the quantitative and method for qualitative analysis of black carbon surface functional group according to claim 6, which is characterized in that above-mentioned
In step (b), including carrying out the first cooling temperature range after heating up within the temperature range of 200 DEG C to 700 DEG C, 500
DEG C to carrying out cooling second temperature section after heating within the temperature range of 1200 DEG C and in 600 DEG C to 1600 DEG C of temperature
Cooling third temperature range is carried out in range after heating.
8. the quantitative and method for qualitative analysis of black carbon surface functional group according to claim 7, which is characterized in that above-mentioned
In first temperature range, heat point is carried out at least one functional group for being selected from carboxyl and ester group in the surface functional group of carbon black
Solution.
9. the quantitative and method for qualitative analysis of black carbon surface functional group according to claim 7, which is characterized in that above-mentioned
In second temperature section, heat point is carried out at least one functional group for being selected from carbonyl and hydroxyl in the surface functional group of carbon black
Solution.
10. the quantitative and method for qualitative analysis of black carbon surface functional group according to claim 7, which is characterized in that upper
It states in third temperature range, heat point is carried out at least one functional group for being selected from hydroxyl and hydrogen in the surface functional group of carbon black
Solution.
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| KR102444774B1 (en) | 2022-09-19 |
| KR20190078971A (en) | 2019-07-05 |
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