CN213633310U - System for detecting carbon black surface functional groups - Google Patents
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- CN213633310U CN213633310U CN202022343598.8U CN202022343598U CN213633310U CN 213633310 U CN213633310 U CN 213633310U CN 202022343598 U CN202022343598 U CN 202022343598U CN 213633310 U CN213633310 U CN 213633310U
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Abstract
The utility model relates to a system for detecting carbon black surface functional groups, which comprises a heating subsystem (1), a degassing subsystem (2), a separating subsystem (3) and a detecting subsystem (4) which are connected in sequence; the heating subsystem (1) is a pulse electrode furnace; the degassing subsystem (2) comprises an oxidation unit (21), an absorption unit (22) and a dehydration unit (23) which are arranged in sequence; the separation subsystem (3) is a chromatographic separation column; the detection subsystem (4) is a thermal conductivity detector. Compared with the prior art, the utility model has the advantages of the degree of accuracy is high, good reproducibility, carbon black surface activity sign is effectual.
Description
Technical Field
The utility model relates to a belong to the chemical industry field, relate to a carbon black for rubber, concretely relates to system for detecting carbon black surface functional group.
Background
The basic properties of carbon black measured by the traditional method are low-temperature nitrogen adsorption, the oil absorption value of the carbon black, the pH value of the carbon black, the tinting strength of the carbon black and the like, and the traditional method is difficult to reveal the activity of the surface of the carbon black, particularly the mechanism of reinforcing rubber by the carbon black. The surface activity is an important factor influencing the interaction between carbon black and between carbon black and rubber, and is a leading factor of carbon black with reinforcing capacity. The surface activity of the carbon black has obvious effect on the influence of filler networks in the filled natural rubber and the interaction degree of the fillers and the rubber.
In the past decades, many schools have appeared in research literature on surface activity of carbon black at home and abroad, and a great deal of research work has been focused on the determination of the surface functional groups of carbon black. The Wanmeng flood of the Cambet company has been studied for many years and adopts the reversed phase gas chromatography, but the data measurement error is larger, and the theory has no necessary connection to the improvement of the wear resistance of the tire as proved by practice.
The invention patent CN110018219A discloses a system and a method for quantitatively and qualitatively analyzing carbon black surface functional groups, wherein the analysis system comprises: the device comprises a cavity for accommodating a carbon black sample in the cavity, a temperature adjusting part for detecting the temperature in the cavity, a pressure detecting part for detecting the pressure in the cavity, a gas outflow part for enabling part of mixed gas generated in the cavity to flow out, and a mass analysis part for analyzing the type and the quality of the mixed gas flowing out of the gas outflow part. In this aspect, the surface functional groups of the carbon black in each thermal decomposition temperature range can be quantitatively analyzed, and the mixed gas obtained by thermally decomposing the carbon black is subjected to quadrupole mass spectrometry to classify various gases contained in the mixed gas, and then subjected to qualitative analysis. The detection technology needs to accurately determine the temperature wave band of each functional group, even the temperature wave bands of partial functional groups overlap, so that different temperature rise rates are set to separate various functional groups, and finally, accurate quantification is carried out.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing a system for detect carbon black surface functional group in order to overcome the defect that above-mentioned prior art exists, can solve among the prior art survey carbon black surface functional group's method and device loaded down with trivial details, the not high technical problem of accuracy of data.
The purpose of the utility model can be realized through the following technical scheme: a system for detecting carbon black surface functional groups comprises a heating subsystem, a degassing subsystem, a separation subsystem and a detection subsystem which are sequentially connected; the heating subsystem is a pulse electrode furnace; the degassing subsystem comprises an oxidation unit, an absorption unit and a dehydration unit which are arranged in sequence; the separation subsystem is a chromatographic separation column; the detection subsystem is a Thermal Conductivity Detector (TCD).
Furthermore, the pulse electrode furnace comprises an upper electrode, a lower electrode and a graphite crucible, wherein the graphite crucible is positioned between the upper electrode and the lower electrode and is heated by current; the upper electrode is provided with a vertical opening which is positioned right above the graphite crucible.
Furthermore, a feeding assembly is arranged above the upper electrode, the feeding assembly comprises a sample port sliding block and a fluxing agent port sliding block which can move horizontally, an upper cover is further arranged above the feeding assembly, the upper parts of the upper cover, the sample port sliding block and the fluxing agent port sliding block are sequentially arranged from top to bottom, and a quartz window is arranged on one side of the upper cover; a sample inlet is arranged on the sample port sliding block; a fluxing agent inlet is arranged on the fluxing agent inlet sliding block; the horizontal positions of the sample inlet and the flux inlet were observed through the quartz window.
During detection, the positions of the fluxing agent inlet and the sample inlet are observed by means of a quartz window, the position adjustment of the fluxing agent port sliding block and the sample port sliding block is assisted, the upper cover is opened, the fluxing agent and the sample are respectively put into the fluxing agent inlet and the sample inlet, after the graphite crucible is degassed at high temperature and decontaminated, the fluxing agent and the sample sequentially and respectively fall into the graphite crucible from the fluxing agent inlet and the sample inlet through the vertical opening in the upper electrode for high-temperature degassing.
The fluxing agent is nickel.
The oxidation unit is filled with a normal-temperature oxidant to oxidize CO into CO2(ii) a The absorption unit is filled with alkali asbestos to absorb CO2(ii) a Magnesium perchlorate is filled in the dehydration unit to absorb H2O。
The inlet of the heating subsystem is connected with an argon gas source, and argon can be input into the system to be used as carrier gas and protective gas of the pulse electrode furnace.
And a dust filtering unit and a purging bypass are sequentially arranged between the heating subsystem and the degassing subsystem.
And bypass mechanisms are also arranged at two ends of the separation subsystem.
And a flow controller is arranged between the separation subsystem and the detection subsystem.
And a flowmeter is arranged behind the detection subsystem.
When the system for detecting the carbon black surface functional groups is adopted for detection, the method mainly comprises the following steps:
firstly, melting and decomposing a sample in a heating subsystem under the assistance of a fluxing agent, and respectively converting three elements of oxygen, nitrogen and hydrogen in the sample into CO and N2And H2；
Second, the CO and N are reacted2And H2Feeding argon into a degassing subsystem to remove CO;
thirdly, adding N2And H2Separated by a separating subsystem, H2Entering a detection subsystem for detection;
and fourthly, converting the detection signal into a signal corresponding to the gas concentration, and carrying out compensation correction, linearization and integration on the blank value and the sample weight to obtain an analysis result so as to detect the hydrogen content on the surface of the carbon black.
Further, the second step of CO removal by the degassing subsystem comprises the following specific processes: oxidizing CO into CO by a normal-temperature oxidant in an oxidation unit2，CO2Is absorbed by the alkali asbestos in the absorption unit and is finally treated by the magnesium perchlorate in the dehydration unit to remove H generated in the process2O。
The third step is that the use method of the thermal conductivity detector is as follows: firstly, starting a thermal conductivity detector to be preheated to a working state, and determining that an instrument reaches a stable state (a TCD signal value is stabilized at 3000-4000) through a maintenance self-checking system of equipment; opening an argon switch of the thermal conductivity detector, and adjusting the pressure and flow rate of gas required by the test; setting a temperature program and an integration time of the thermal conductivity detector, wherein the temperature range is 0-3000 ℃, the heating rate is 3K/sec, and the integration time is 0-600 s.
The test method has the principle that
Compared with the prior art, the utility model has the advantages of it is following:
1. the accuracy is high, and the repeatability is good;
2. the hydrogen element in the sample is extracted by adopting an inert gas protection melting method, current is rapidly heated through a graphite crucible between an upper electrode and a lower electrode, the sample is heated and melted by a pulse furnace, the hydrogen element in the sample is extracted into hydrogen gas and introduced into a Thermal Conductivity Detector (TCD), and then the concentration of the hydrogen element is calculated according to the output of the detector.
3. The hydrogen element content is adopted to represent the surface activity of the carbon black, the representation effect is good, and the detection result has good correlation with the wear resistance of the tire.
Drawings
FIG. 1 is a diagram of a system configuration for detecting functional groups on the surface of carbon black;
FIG. 2 is a view showing a construction of a pulse electrode furnace;
in the figure: 1-heating subsystem, 2-degassing subsystem, 3-separation subsystem, 4-detection subsystem, 5-dust filtering unit, 6-purging bypass, 7-bypass mechanism, 8-flow controller, 9-flowmeter, 11-upper electrode, 12-lower electrode, 13-graphite crucible, 14-upper cover, 15-sample port slider, 16-flux port slider, 17-quartz window, 18-sample input port, 19-flux input port, 21-oxidation unit, 22-absorption unit, 23-dehydration unit, Y1-sample, Y2 flux.
FIG. 3 is a graph showing the degassing effect of the pulse electrode furnace.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments. The embodiments of the present invention are implemented on the premise of the technical solution of the present invention, and detailed implementation and specific operation processes are given, but the scope of the present invention is not limited to the following embodiments.
Example 1
As shown in figure 1, a measuring system for detecting the hydrogen content of functional groups on the surface of carbon black comprises a heating subsystem 1, a degassing subsystem 2, a separating subsystem 3 and a detecting subsystem 4 which are connected in sequence; the heating subsystem 1 is a pulse electrode furnace, and the degassing subsystem 2 comprises an oxidation unit 21, an absorption unit 22 and a dehydration unit 23 which are sequentially arranged; the oxidizing unit 21 is filled with a normal-temperature oxidizing agent; the absorption unit 22 is filled with alkali asbestos; the dehydration unit 23 is filled with magnesium perchlorate. The separation subsystem 3 is a chromatographic separation column; the detection subsystem 4 is a thermal conductivity detector.
As shown in fig. 2, the pulse electrode furnace includes an upper electrode 11, a lower electrode 12, and a graphite crucible 13, the graphite crucible 13 being located between the upper electrode 11 and the lower electrode 12; the upper electrode 11 is provided with a vertical opening, and the opening is positioned right above the graphite crucible 13. A feeding assembly is arranged above the upper electrode 11, the feeding assembly comprises a sample port slide 15 and a fluxing agent port slide 16 which can move horizontally, and an upper cover 14 is arranged above the feeding assembly. A quartz window 17 is arranged on one side of the upper cover 14; the sample port sliding block 15 is provided with a sample input port 18; the flux port slider 16 is provided with a flux inlet 19.
As shown in fig. 1, the inlet of the heating subsystem 1 is connected with an argon gas source, and the whole measuring system is sequentially connected with the heating subsystem 1, the dust filtering unit 5, the purging bypass 6, the oxidizing unit 21, the absorbing unit 22, the dehydrating unit 23, the separating subsystem 3, the flow controller 8, the detecting subsystem 4 and the flowmeter 9 through pipelines; wherein, as the chromatographic separation column both ends of separation subsystem 3 connect a bypass pipeline in parallel as bypass mechanism 7, use the bypass mechanism of separation column when carrying out the program control temperature, nitrogen gas and hydrogen enter TCD detector together this moment, and then the hydrogen is oxidized and is removed by coexisting gas compensating mechanism, therefore only nitrogen gas enters TCD detector, finally, through the differential operation processing two testing results of obtaining, and then determine the composition of hydrogen.
The components used in the measurement system are commercially available products, such as a Thermal Conductivity Detector (TCD) as the detection subsystem 4 (TCD has high sensitivity and wide range, and is manufactured by japan horiba).
The system is adopted to detect the hydrogen content of the functional group on the surface of the carbon black, and the steps are as follows:
firstly, a Thermal Conductivity Detector (TCD) is started to be preheated to a working state, and the instrument is determined to reach a stable state (the TCD signal value is stabilized within a range of 3500 +/-100) through a maintenance self-checking system of the equipment; opening an argon switch of the thermal conductivity detector, and adjusting the pressure and flow rate of gas required by the test; setting a temperature program and an integration time of the thermal conductivity detector, wherein the temperature range is 0-3000 ℃, the heating rate is 3K/sec, and the integration time is 0-600 s.
Weighing dried carbon black, wrapping the carbon black by using an ultra-pure nickel bag with a cover, extruding the residual air in the nickel bag by using a special sample press to obtain a sample Y1, observing and adjusting the horizontal positions of a fluxing agent port slide block 16 and a sample port slide block 15 by virtue of a quartz window 17, opening an upper cover 14, putting a sample Y1 into a sample input port 18 of a pulse electrode furnace, and putting a graphite crucible 13 into a lower electrode 12 platform; high purity nickel was used as a flux Y2, and placed in the flux inlet 19.
As shown in fig. 3, when a large current is passed through the graphite crucible 13 placed between the upper electrode 11 and the lower electrode 12 of the pulse electrode furnace, the crucible is rapidly raised to a high temperature due to joule heating effect, the pulse electrode furnace is heated to 3000 ℃ to perform degassing treatment under argon protection on the graphite crucible 13, and impurities adsorbed in the graphite crucible 13 are removed; after the graphite crucible 13 is degassed at a high temperature, the flux inlet 19 is automatically opened, the flux Y2 (nickel) falls into the graphite crucible 13 through the vertical opening in the upper electrode 11, the flux Y2 is similarly degassed at a high temperature, then the sample inlet 18 is automatically opened, the sample Y1 falls into the graphite crucible 13 through the vertical opening in the upper electrode 11, and hydrogen is decomposed by heating and melting.
The three elements of oxygen, nitrogen and hydrogen in the sample Y1 are converted into CO and N respectively in the heating subsystem 12And H2Argon gas is used as carrier gas and is conveyed to a dust filtering unit 5 to filter dust in the dust, then the dust is exhausted after passing through a purging bypass 6 (degassing of a crucible, a fluxing agent and the like), and then the dust is filteredArgon is fed into the degassing subsystem 2, and the normal temperature oxidant (Schutze Reagent in this example) in the oxidation unit 21 oxidizes CO into CO2，CO2Absorbed by the alkali asbestos in the absorption unit 22, and the residual gas is subjected to high-acid magnesium dehydrogenation in the dehydration unit 232Separating with chromatographic separation column of separation subsystem 3, (when program temperature control is carried out, separating bypass mechanism 7 is used, nitrogen and hydrogen are fed into TCD detector 4, then hydrogen is oxidized and removed by coexisting gas compensation mechanism, so that only nitrogen is fed into TCD detector, finally two detection results are obtained by means of differential operation treatment, and the hydrogen component is determined), and the residual gas is mainly H2The flow controller 8 controls the flow to enter the detection subsystem 4 for detection; a data acquisition controller and a data signal workstation (the data acquisition controller is self-contained, and the data signal workstation is an external computer system) of the TCD are adopted to convert detection signals into signals corresponding to the gas concentration, wherein the data acquisition device is connected with a detection subsystem 4TCD signal amplification and analog-to-digital conversion module, and an analysis result is obtained by performing compensation correction, linearization and integration on a blank value and the sample weight, so that the hydrogen content on the surface of the carbon black is detected.
The embodiments described above are intended to facilitate the understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention according to the disclosure of the present invention.
Claims (10)
1. A system for detecting functional groups on the surface of carbon black is characterized by comprising a heating subsystem (1), a degassing subsystem (2), a separating subsystem (3) and a detecting subsystem (4) which are sequentially connected; the heating subsystem (1) is a pulse electrode furnace; the degassing subsystem (2) comprises an oxidation unit (21), an absorption unit (22) and a dehydration unit (23) which are arranged in sequence; the separation subsystem (3) is a chromatographic separation column; the detection subsystem (4) is a thermal conductivity detector.
2. The system for detecting carbon black surface functional groups according to claim 1, wherein the pulse electrode furnace comprises an upper electrode (11), a lower electrode (12) and a graphite crucible (13), wherein the graphite crucible (13) is positioned between the upper electrode (11) and the lower electrode (12); the upper electrode (11) is provided with a vertical opening which is positioned right above the graphite crucible (13).
3. The system for detecting carbon black surface functional groups according to claim 2, wherein a feeding assembly is arranged above the upper electrode (11), the feeding assembly comprises a horizontally movable sample port slider (15) and a flux port slider (16), and an upper cover (14) is arranged above the feeding assembly.
4. The system for detecting carbon black surface functional groups according to claim 3, wherein a quartz window (17) is arranged on one side of the upper cover (14); the sample port sliding block (15) is provided with a sample input port (18); the flux port slider (16) is provided with a flux inlet (19).
5. The system for detecting carbon black surface functional groups according to claim 1, wherein the oxidation unit (21) is filled with a normal temperature oxidant; the absorption unit (22) is filled with alkali asbestos; and magnesium perchlorate is filled in the dehydration unit (23).
6. The system for detecting carbon black surface functional groups according to claim 1, wherein the inlet of the heating subsystem (1) is connected with an argon gas source.
7. The system for detecting the functional groups on the surface of the carbon black according to claim 1, wherein a dust filtering unit (5) and a purging bypass (6) are further arranged between the heating subsystem (1) and the degassing subsystem (2) in sequence.
8. The system for detecting carbon black surface functional groups according to claim 1, wherein a bypass mechanism (7) is further arranged at both ends of the separation subsystem (3).
9. The system for detecting carbon black surface functional groups according to claim 1, wherein a flow controller (8) is arranged between the separation subsystem (3) and the detection subsystem (4).
10. The system for detecting carbon black surface functional groups according to claim 1, wherein a flow meter (9) is arranged after the detection subsystem (4).
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