CN114736444B - Polymer-based conductive composite material for heat tracing belt and preparation method thereof - Google Patents
Polymer-based conductive composite material for heat tracing belt and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of electric heating composite materials, and particularly relates to a polymer-based electric heating composite material for a high-temperature heat tracing belt and a preparation method thereof. The invention provides a polymer-based conductive composite material for heat tracing bands, wherein the raw materials of the composite material comprise polyethylene and multi-wall carbon nanotubes; wherein the polyethylene is high-density polyethylene with the weight-average molecular weight of 20-60 ten thousand g/mol; the average length of the multiwall carbon nanotubes is less than 10 μm. Under the condition that multiple conductive fillers are compounded without combining multiple matrixes, only one matrix and one filler are used, the rapid (less than or equal to 2.5 minutes) temperature rise to 120 ℃ under the ultra-low safety voltage of 18V is realized, the temperature is maintained at 120+/-10 ℃ for a long time, the phenomenon of burning tape does not occur, and the excellent high-temperature electrothermal stability is shown.
Description
Technical Field
The invention belongs to the field of electric heating composite materials, and particularly relates to a polymer-based electric heating composite material for a high-temperature heat tracing belt and a preparation method thereof.
Background
The polymer-based electrothermal composite material is a composite material formed by taking an organic polymer as a matrix and adding some inorganic conductive fillers into the matrix, and the composite material combines the good flexibility of the polymer material, the good conductivity and the good Joule heating performance of the inorganic fillers and has good comprehensive performance.
Compared with the ceramic-based electrothermal composite material, the polymer-based electrothermal composite material has the advantages of good processability, low cost and low cost, so that the polymer-based electrothermal composite material is widely applied to various aspects such as heat tracing bands, aerospace deicing and snow melting, water heating, sanitation and medical treatment and the like. The polymer-based electrothermal composite material is mostly used as a heating element to be applied to core materials of heat tracing bands. In China, the polymer-based electrothermal composite material for heat tracing bands is widely applied in the low and medium temperature fields at present, and is still in a research and development state in the high temperature field, and mainly has the following problems: 1. the inorganic filler used in commercial heat tracing bands is mainly carbon black, the Joule thermal performance of the carbon black is poor, a large amount of filler is needed to reach high temperature, the mechanical property of the heat tracing bands is obviously reduced by using a large amount of filler, and the application range of the heat tracing bands is limited; 2. the volume resistivity of the commercial heat tracing belt at room temperature is large, high voltage is usually required to reach high temperature, and the use cost is increased; 3. carbon black is used as a filler, so that the conductive network formed in the matrix has poor stability at high temperature, and the condition of burning tape is easy to occur.
Disclosure of Invention
Aiming at the defects, the invention provides a polymer-based conductive composite material for a heat tracing band, which solves the problems of large filling capacity, high use voltage and poor high-temperature electrothermal stability of the conventional high-temperature heat tracing band.
The technical scheme of the invention is as follows:
the first technical problem to be solved by the invention is to provide a polymer-based conductive composite material for heat tracing bands, wherein the raw materials of the composite material comprise polyethylene and multi-wall carbon nanotubes; wherein the polyethylene is high-density polyethylene with the weight-average molecular weight of 20-60 ten thousand g/mol; the average length of the multiwall carbon nanotubes is less than 10 μm.
Further, the ratio of polyethylene to multiwall carbon nanotubes is: 100 parts of polyethylene and 3-7 parts of multi-wall carbon nano tubes.
Further, the polymer-based conductive composite material for the heat tracing band has high-temperature electrothermal stability, and can be heated to 120 ℃ within 2.5 minutes under the safety voltage of 18V and maintained at 120+/-10 ℃ for a long time.
The second technical problem to be solved by the present invention is to provide a preparation method of the polymer-based conductive composite material for heat tracing bands, the preparation method comprising: and (3) melt blending the dried polyethylene and the multi-wall carbon nano tube to obtain the composite material.
Further, the melt blending is performed at a temperature equal to or lower than the decomposition temperature of the polyethylene at a temperature equal to or higher than the melting point.
The invention has the beneficial effects that:
compared with the electric heating composite material disclosed by the prior art and used in the commercial heat tracing belt at present, under the condition that multiple conductive fillers are not compounded by combining multiple matrixes, only one matrix and one filler are used, the rapid (less than or equal to 2.5 minutes) temperature rise to 120 ℃ and long-term maintenance at 120+/-10 ℃ under the ultra-low safety voltage of 18V are realized, and the phenomenon of burning is avoided, namely the excellent high-temperature electric heating stability is shown. In addition, the preparation process is simple, and is beneficial to rapid and large-scale production; the conductive filler has low loading, better mechanical property and more application scenes.
Description of the drawings:
FIG. 1 is (a) an IR thermal imaging graph and (b) a temperature/current versus time graph of the high density polyethylene (5960G 1) conductive composite obtained in example 1 at 18V.
Fig. 2 is (a) an infrared thermogram and (b) a temperature/current versus time plot for the high density polyethylene (5960G 1) conductive composite of example 2 at 18V.
Fig. 3 is (a) an infrared thermogram and (b) a temperature/current versus time plot at 18V for the high density polyethylene (5000S) conductive composite obtained in comparative example 1.
Fig. 4 is (a) an infrared thermogram and (b) a temperature/current versus time plot of the linear low density polyethylene (FB 2230) conductive composite of comparative example 2 at 18V.
Fig. 5 is (a) an infrared thermogram and (b) a plot of current and temperature versus time for the medium density polyethylene (FB 2310) conductive composite obtained in comparative example 3 at 96V.
FIG. 6 is a plot of DeltaT over time for the different polymer systems obtained in the examples of the present invention (example 1) and the comparative example (comparative example 1).
Fig. 7 (a) (b) (c) are graphs of volume resistivity of two multi-walled carbon nanotubes using different average lengths for high density polyethylene (5960G 1), medium density polyethylene (FB 2310), and linear low density polyethylene (FB 2230), respectively; as can be seen from fig. 7: on the premise of using the same matrix, the average length of the conductive filler can influence the dispersion of the conductive filler in the matrix so as to influence the conductive network of the conductive composite material, the volume resistivity and the high-temperature electrothermal stability; the more perfect the conductive network obtained by using NC7000, the less the conductive network is damaged in the heating and temperature raising process of the composite material, and the better the high-temperature electrothermal stability of the composite material, compared with the conductive filler (multi-wall carbon nanotube XF 13) with the average length of more than 10 mu m, the conductive filler (multi-wall carbon nanotube NC 7000) with the average length of less than 10 mu m is selected.
Detailed Description
The polymer-based conductive composite material is prepared by using specific polyethylene and specific filler, can be quickly (in 2.5 minutes or less) heated to 120 ℃ under the ultra-low safety voltage of 18V and maintained at 120+/-10 ℃ for a long time, and does not generate the phenomenon of burning, namely, the polymer-based conductive composite material has excellent high-temperature electrothermal stability; it can be used as a high temperature heat trace belt. In addition, the electric tracing is used as a heating component, and can be divided into a self-limiting temperature tracing band and a constant power tracing band according to the action mode; the self-limiting temperature heat tracing band is an electric heat tracing band made of conductive polymers with very high positive temperature coefficients, and the polymer-based conductive composite material prepared by the method is suitable for preparing constant-power heat tracing bands.
In the present invention, a matrix having a high relative molecular mass, i.e., a high-density polyethylene having a weight-to-average molecular mass of more than 20 ten thousand G/mol, is selected, wherein a high-density polyethylene (5960G 1) having a weight-to-average molecular mass of about 29 ten thousand G/mol is used as the matrix; the multi-walled carbon nanotubes having a short average length are selected as the conductive filler, i.e., the average length of the multi-walled carbon nanotubes is less than 10 μm, and the multi-walled carbon nanotubes (NC 7000) having an average length of 1.5 μm are used as the conductive filler.
Example 1
Placing high density polyethylene (5960G 1) and multi-wall carbon nanotubes (NC 7000) in an oven at 80deg.C for 24 hours, and oven drying the water; mixing the dried high-density polyethylene and the multiwall carbon nano tube according to the weight ratio of 100:4, sequentially adding the materials into a torque rheometer (the temperature is 180 ℃, the rotating speed is 60r/min, and the time is 10 min) for melt blending; and taking out the materials after full melt blending, granulating and naturally cooling to obtain the polyethylene-based electric heating composite material.
And (3) placing the obtained granules into a specific mold, embedding copper wires, performing hot press molding by a flat vulcanizing machine (the temperature is 180 ℃ and the time is 5min for prepressing, 5min for hot pressing and 5min for cold pressing), and then taking out the mold to obtain polymer-based conductive composite material sample bars for testing the electrothermal performance. The electrical and thermal properties of the test bars were recorded by paperless thermography and infrared imager using a dc voltage regulator source to apply 18V across the bars as shown in fig. 1; as can be seen from fig. 1: the conductive composite material prepared from the high-density polyethylene (5960G 1) with the weight-average molecular weight higher than 20 ten thousand G/mol can be heated to 120 ℃ in less than or equal to 2.5 minutes under the direct-current voltage of 18V, can be stably maintained for 30 minutes at 120 ℃, does not generate the burning phenomenon, and shows good high-temperature electrothermal stability.
Example 2
Placing a high-density polyethylene (5960G 1) and a multi-wall carbon nano (NC 7000) tube in an oven at 80 ℃ for 24 hours, and drying the water; mixing the dried high-density polyethylene and the multiwall carbon nano tube according to the weight ratio of 100:4, sequentially adding the materials into a torque rheometer (the temperature is 180 ℃, the rotating speed is 60r/min, and the time is 10 min) for melt blending; and taking out the materials after full melt blending, granulating and naturally cooling to obtain the polyethylene-based electric heating composite material.
And (3) placing the obtained granules into a specific mold, embedding copper wires, performing hot press molding by a flat vulcanizing machine (the temperature is 180 ℃ and the time is 5min for prepressing, 5min for hot pressing and 5min for cold pressing), and then taking out the mold to obtain polymer-based conductive composite material sample bars for testing the electrothermal performance. The high temperature electrothermal stability of the test bars operated for a long period of time (10 hours) was recorded by paperless thermography and infrared imager by applying 18V across the bars using a dc voltage stabilizing source as shown in figure 2. As can be seen from fig. 2: the conductive composite material prepared from the high-density polyethylene (5960G 1) with the weight-average molecular weight higher than 20 ten thousand G/mol can be heated to 120 ℃ in less than or equal to 2.5 minutes under the direct-current voltage of 18V, can be stably maintained at 120 ℃ for 10 hours, does not generate burning phenomenon, and shows excellent high-temperature electrothermal stability.
Comparative example 1
High density polyethylene (5000S, its weight-average molecular weight is 12.5 ten thousand g/mol) and multi-wall carbon nanotubes (NC 7000) are placed in an oven at 80 ℃ for 24 hours, and the moisture is dried; mixing the dried high-density polyethylene and the multiwall carbon nano tube according to the weight ratio of 100:4, sequentially adding the materials into a torque rheometer (the temperature is 180 ℃, the rotating speed is 60r/min, and the time is 10 min) for melt blending; and taking out the materials after full melt blending, granulating and naturally cooling to obtain the polyethylene-based electric heating composite material.
Placing the obtained granules into a specific mold, embedding copper wires, performing hot press molding by a flat vulcanizing machine (the temperature is 180 ℃ and the time is 5min for prepressing, 5min for hot pressing and 5min for cold pressing), and then taking out the mold to obtain polymer-based conductive composite material sample bars for testing the electric heating performance; the electrical and thermal properties of the test bars were recorded by paperless thermography and infrared imaging by applying 18V voltage across the bars using a dc voltage stabilizing source as shown in fig. 3; as can be seen from fig. 3: the conductive composite material prepared from high-density polyethylene (5000S) with the weight-average molecular weight lower than 20 ten thousand g/mol has the advantages that the surface temperature of the material is continuously increased under the direct-current voltage of 18V, the internal current is continuously increased, the surface temperature of the material cannot be kept stable, the burning phenomenon occurs, the poor high-temperature electrothermal stability is shown, and the weight-average molecular weight of the matrix is necessary to be higher than 20 ten thousand g/mol.
Comparative example 2
Placing linear low density polyethylene (FB 2230, weight average molecular weight of which is 50 ten thousand g/mol) and multi-wall carbon nanotubes (NC 7000) in an oven at 80 ℃ for 24 hours, and drying the water; the dried linear low density polyethylene and the multiwall carbon nanotube are mixed according to the weight ratio of 100:7, sequentially adding the mixture into a torque rheometer (the temperature is 180 ℃, the rotating speed is 60r/min, and the time is 10 min) for melt blending; and taking out the materials after full melt blending, granulating and naturally cooling to obtain the polymer-based conductive composite material.
Placing the obtained granules into a specific mould, embedding copper wires, performing hot press molding by a flat vulcanizing machine (the temperature is 180 ℃ and the time is 5min for prepressing, 5min for hot pressing and 5min for cold pressing), and then taking out the mould to obtain a polyethylene-based electrothermal composite material spline for testing electrothermal performance; the electrical and thermal properties of the test bars were recorded by paperless thermography and infrared imager using a dc voltage regulator source to apply 18V across the bars as shown in fig. 4; as can be seen from fig. 4: the conductive composite material prepared from the linear low density polyethylene (FB 2230) with the weight-average molecular weight higher than 20 ten thousand has the advantages that the surface temperature of the material is continuously increased under the direct current of 18V, the internal current is continuously increased, the surface temperature of the material cannot be kept stable, the burning zone phenomenon occurs, the particularly poor high-temperature electrothermal stability is shown, and the conductive composite material not only needs to have the weight-average molecular weight of the matrix higher than 20 ten thousand g/mol, but also needs to have the molecular chain linear (namely, as far as possible without short branched chains).
Comparative example 3
Placing medium density polyethylene (FB 2310 with a weight-average molecular weight of 46 ten thousand g/mol) and multi-wall carbon nanotubes (NC 7000) in an oven at 80 ℃ for 24 hours, and drying the water; mixing the dried medium density polyethylene and the multiwall carbon nanotube according to a ratio of 100:7, sequentially adding the materials into a torque rheometer (the temperature is 180 ℃, the rotating speed is 60r/min, and the time is 10 min) for melt blending; and taking out the materials after full melt blending, granulating and naturally cooling to obtain the polymer-based conductive composite material.
Putting the obtained granules into a mould, performing hot press forming (the temperature is 180 ℃ for 5min, the time is 5min, the hot press is 5min, the cold press is 5 min), then taking out the sample strip in the mould, bonding copper meshes at two ends of the sample strip, and finally obtaining a polyethylene electrothermal composite material sample strip for testing electrothermal performance; the current and temperature changes over time in the test spline work were recorded by paperless thermography and infrared imager by applying 96V voltage across the spline using a dc voltage stabilizing source as shown in fig. 5; as can be seen from fig. 5: the conductive composite material prepared from medium density polyethylene (FB 2310) with the weight-average molecular weight higher than 20 ten thousand g/mol has the advantages that the surface temperature of the material is continuously increased under the direct-current voltage of 96V, the internal current is continuously increased, the surface temperature of the material cannot be kept stable, the burning phenomenon occurs, particularly poor high-temperature electrothermal stability is shown, and the fact that the weight-average molecular weight of a matrix is higher than 20 ten thousand g/mol and a molecular chain is linear is needed is indicated.
The polyethylene-based electrothermal composites of examples 1, 2 and comparative examples 1 to 3 were subjected to electrothermal testing, and the results are shown in table 1.
Table 1 results of electrothermal testing of the materials obtained in examples and comparative examples
The polyethylene electrothermal composite material obtained in the embodiment is subjected to electrothermal test at the highest surface temperature T 1 With temperature T at the onset of melting of the material 2 The difference, defined as DeltaT; the change of delta T with time can reflect the high-temperature electrothermal stability of the polymer conductive composite material, and the smaller the delta T change, the better the stability, and the result is shown in figure 6; as can be seen from fig. 6: the conductive composite material prepared from the high-density polyethylene (5960G 1) with the weight-average molecular weight higher than 20 ten thousand G/mol has better high-temperature electrothermal stability than the conductive composite material prepared from the high-density polyethylene (5000S) with the weight-average molecular weight lower than 20 ten thousand G/mol.
Comparative example 4
Placing high density polyethylene (5960G 1) and multi-wall carbon nanotubes (XF 13, average length of which is 20-30 μm) in an oven at 80deg.C for 24 hours, and oven drying the water; and (3) mixing the dried polyethylene and the multiwall carbon nanotubes according to a ratio of 100:4, after weighing the mass ratio, adding the mixture into a torque rheometer (the temperature is 180 ℃, the rotating speed is 60r/min, and the time is 10 min), and carrying out melt blending; and taking out the materials after full melt blending, granulating and naturally cooling to obtain the polymer-based conductive composite material.
And (3) putting the obtained granules into a mould, performing hot press forming (the temperature is 180 ℃ for 5min, the time is 5min, the hot press is 5min, the cold press is 5 min) by a plate vulcanizing machine, then taking out the sample strip in the mould, bonding copper meshes at two ends of the sample strip, and finally obtaining the polyethylene-based electrothermal composite material sample strip, wherein the sample strip is used for testing the volume resistivity, and the test result is shown in figure 7 c.
Comparative example 5
Placing medium density polyethylene (FB 2310) and multi-wall carbon nanotubes (XF 13) in an oven at 80 ℃ for 24 hours, and drying the water; and (3) mixing the dried polyethylene and the multiwall carbon nanotubes according to a ratio of 100:7, after weighing the mass ratio, adding the mixture into a torque rheometer (the temperature is 180 ℃, the rotating speed is 60r/min, and the time is 10 min), and carrying out melt blending; and taking out the materials after full melt blending, granulating and naturally cooling to obtain the polymer-based conductive composite material.
And (3) putting the obtained granules into a mould, performing hot press forming (the temperature is 180 ℃ for 5min, the time is 5min, the hot press is 5min, the cold press is 5 min) by a plate vulcanizing machine, then taking out the sample strip in the mould, bonding copper meshes at two ends of the sample strip, and finally obtaining the polyethylene-based electrothermal composite material sample strip for testing the volume resistivity, wherein the test result is shown in figure 7 b.
Comparative example 6
Placing linear low density polyethylene (FB 2230) and multi-wall carbon nanotubes (XF 13) in an oven at 80 ℃ for 24 hours, and drying the moisture; and (3) mixing the dried polyethylene and the multiwall carbon nanotubes according to a ratio of 100:7, after weighing the mass ratio, adding the mixture into a torque rheometer (the temperature is 180 ℃, the rotating speed is 60r/min, and the time is 10 min), and carrying out melt blending; and taking out the materials after full melt blending, granulating and naturally cooling to obtain the polymer-based conductive composite material.
And (3) putting the obtained granules into a mould, performing hot press forming (the temperature is 180 ℃ for 5min, the time is 5min, the hot press is 5min, the cold press is 5 min) by a plate vulcanizing machine, then taking out the sample strip in the mould, bonding copper meshes at two ends of the sample strip, and finally obtaining the polyethylene-based electrothermal composite material sample strip, wherein the sample strip is used for testing the volume resistivity, and the test result is shown in figure 7 a.
Claims (3)
1. The polymer-based conductive composite material is used for a heat tracing belt and is characterized in that the raw materials of the composite material comprise polyethylene and multi-wall carbon nano tubes; wherein the ratio of the polyethylene to the multiwall carbon nanotubes is: 100 parts of polyethylene and 3-7 parts of multi-wall carbon nano tubes; the polyethylene is high-density polyethylene with the weight-average molecular weight of 20-60 ten thousand g/mol; the average length of the multi-wall carbon nanotubes is less than 10 μm; and, when the composite material is used for heat tracing belt, the temperature can be raised to 120 ℃ within 2.5 minutes under the safety voltage of 18V and maintained at 120+/-10 ℃ for a long time.
2. The polymer-based conductive composite for heat tracing bands of claim 1, wherein said composite is prepared by the following method: and (3) melt blending the dried polyethylene and the multi-wall carbon nano tube to obtain the composite material.
3. A polymer-based conductive composite for use in heat tracing bands according to claim 2, wherein said melt blending is performed at a temperature below the decomposition temperature of the polyethylene above the melting point.
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| KR101799573B1 (en) * | 2016-02-19 | 2017-11-20 | 금호석유화학 주식회사 | Conductive resin composition and plastic article using the same |
| KR101830957B1 (en) * | 2016-02-19 | 2018-02-22 | 금호석유화학 주식회사 | Method for manufacturing conductive resin composition |
| KR101824105B1 (en) * | 2016-12-29 | 2018-01-31 | 금호석유화학 주식회사 | A semi-conductive composition for ultra-high voltage power cables and a method for manufacturing the same |
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