CN112920462B - Conductive composite master batch for rubber cable shielding material and preparation method thereof - Google Patents
Conductive composite master batch for rubber cable shielding material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a conductive composite master batch for a rubber cable shielding material and a preparation method thereof, wherein the composite master batch comprises the following components in parts by mass: 40-60 parts of colloidal graphene, 25-40 parts of superconducting carbon black combination and 10-20 parts of paraffin oil; wherein the effective content of the conductive substance is 30-45%. Firstly, preparing graphene and pretreatment liquid into dispersion liquid, blending and grafting the dispersion liquid with liquid ethylene propylene rubber and a catalyst at high temperature to obtain colloidal graphene, and then mixing and granulating the colloidal graphene with two conductive carbon blacks with different particle sizes and paraffin oil to prepare composite master batches. The master batch can greatly reduce the use of powder after being applied to a shielding material, the cleanliness is easy to control, the processability is effectively improved, the tear resistance and the electric stability are improved, the volume resistivity is greatly reduced, the problems of poor processability, easy tearing, low electric performance and difficult cleanliness control caused by the large application of conductive carbon black powder in the prior art are solved, the preparation process and the product do not need drying, the flow is short, the energy consumption is low, conventional equipment is used, the batch production is easy, and the application prospect is good.
Description
Technical Field
The invention relates to the field of modification and application of carbon nano composite materials, in particular to a conductive composite master batch for a rubber cable shielding material and a preparation method thereof.
Background
The medium and high voltage special rubber cable has wide application in the fields of urban power transmission and distribution, ships, rail traffic, aerospace, wind power generation, coal mines and the like, has high requirements on use safety, and has the advantages that in order to effectively prevent electric field concentration in the cable, ensure uniform distribution of the electric field and avoid insulation layer breakdown caused by electric treeing of the insulation layer, the related standard regulations require the use of a semi-conductive shielding material, along with the improvement of the voltage grade of the cable, the performance of the shielding layer material, particularly the electrical performance and the material cleanliness, are higher and higher, in addition, the rubber cable is frequently used in mobile and moving occasions, the fatigue fracture of the shielding layer is often caused in the application process, the service life and the power utilization safety of the cable are seriously influenced, the traditional material components are complex, a large amount of conductive carbon black powder is used, and the tear resistance, the processing performance, the electrical performance and the cleanliness of the material can not meet the application requirements often, it is urgently needed to find a conductive material with good tear resistance, low volume resistivity and controllable cleanliness to solve the problem.
Since andrelim and consuding norworth schloff succeeded in separating graphene from graphite in experiments by physicists of manchester university in england in 2004, the application of its excellent properties, particularly electrical and thermal conductivity, has caused a worldwide research surge. In graphene, electrons can be transferred very efficiently, so that the graphene has extremely high conductivity, and the electron mobility in graphene is over 15000cm at normal temperature 2 A resistivity of only about 10 -6 Omega cm, lower than copper or silver, is the material with the smallest resistivity in the world at present.
The graphene sheets have strong van der waals force, when the graphene sheets are excessively used, the graphene sheets are easily stacked and agglomerated to greatly reduce the electric conduction and heat conduction performance of the graphene sheets, and the graphene is difficult to disperse in rubber and elastomers, once the graphene sheets are excessively agglomerated and are difficult to disperse again, the physical and mechanical properties of the graphene sheets are greatly influenced, the stacking density of graphene powder is extremely low, dust is easily raised and excessively lost, and the graphene sheets cannot be directly used.
Chinese patent application No. 201710353718.2 discloses a preparation method of a graphene master batch special for automobile engineering plastics, which is characterized in that graphene is compounded with porous microspheres in advance in a slurry form, so that the porous microspheres carry the graphene, silane-terminated polyurethane prepolymer is added, the polyurethane prepolymer is subjected to high-pressure spray polymerization connection, and then the graphene master batch is obtained by dispersing the graphene master batch in carrier resin and granulating the graphene master batch.
Chinese patent application No. 201811511779.8 discloses a composite antistatic plastic concentrated master batch and a preparation method thereof, modified graphene, carbon nano-tubes, conductive carbon black and lubricant containing maleic anhydride grafted polypropylene are made into slurry and spray-dried into the concentrated master batch, the concentrated master batch obtained by the method can improve the compatibility with plastic and the performance of plastic strength and the like, but the melting point of the grafted polypropylene contained in the lubricant is usually 160-180 ℃, the processing temperature of a rubber shielding material is not more than 150 ℃, the master batch can not be used in the shielding material, in addition, hydrogen peroxide and solvent xylene are introduced into the master batch, which can greatly affect the strength and aging performance of the shielding material base material (such as ethylene propylene rubber, ethylene-octene copolymer and the like) and are not beneficial to environmental protection, the content of the graphene and the carbon nano-tubes in the master batch is too high and is difficult to agglomerate, and the carbon nano-tubes are easy to float fibers to cause apparent defects, in addition, the highest content of the conductive substance is 28.6%, and the excessive content of the lubricant can greatly affect the physical and mechanical properties of the material, and can only be added in a small amount to be used as an antistatic agent and cannot be used for producing products with high electrical properties.
The common problems of the invention are that the preparation process is longer, the performance control difficulty is higher, and the drying process with high energy consumption and low efficiency is required because water participates in the process.
Therefore, it is required to develop a conductive composite masterbatch for a rubber cable shielding material, which can be effectively dispersed in the shielding material, can effectively improve the tear resistance, electrical property and cleanliness of the shielding material, and has a short preparation flow and is easy to realize batch production.
Disclosure of Invention
Aiming at the problems, the invention provides a conductive composite master batch suitable for being applied to a rubber cable shielding material, which is characterized in that graphene and a coupling agent are dispersed in a pretreatment liquid to prepare a graphene dispersion liquid, the graphene dispersion liquid is mixed with liquid rubber and a catalyst at a high temperature to form graft modified colloidal graphene, then conductive carbon black with different particle sizes is matched and mixed, and finally the two materials and paraffin oil are mixed and granulated to prepare the conductive composite master batch. After the master batch is applied to the shielding material, the Mooney viscosity can be effectively reduced, the tear resistance is improved, the processability is improved, the volume resistivity of the shielding material is greatly reduced, the problems of poor processability, poor tear resistance, low electrical property and difficulty in control of cleanliness caused by the large amount of carbon black applied to the conventional shielding material are solved, and the preparation process and the product are free from drying, short in flow, low in energy consumption, easy to produce in batches and good in application prospect.
The invention also provides a preparation method of the conductive composite master batch for the rubber cable shielding material, which can improve the dispersibility of the graphene and the superconducting carbon black, reduce the consumption of high-cost graphene, achieve the effect that the high-performance shielding material with good tear resistance, high cleanliness, good electrical property and high stability can be obtained by only using a small amount of graphene and matching with a proper amount of carbon black, and has the advantages of no need of drying in the preparation process and products, short flow, low energy consumption, use of conventional equipment and easy realization of batch production.
In order to achieve the purpose, the invention adopts the following technical scheme:
a conductive composite master batch for a rubber cable shielding material comprises the following components in parts by weight: 40-60 parts of colloidal graphene, 25-40 parts of superconducting carbon black combination and 10-20 parts of paraffin oil. Wherein the effective content of the conductive substance accounts for 30-45% of the total mass.
The superconducting carbon black combination is composed of a specific surface area of less than 90m 2 A superconducting carbon black A with a particle size of more than 40 nm and a specific surface area of less than 100m 2 The superconducting carbon black B with the grain diameter less than 20 nanometers is prepared from the following components in a mass ratio of 2:1 are combined. The paraffin oil has kinematic viscosity (40 ℃) of more than 95mm 2 A petroleum-based liquid paraffin oil having a/s flash point greater than 230 ℃.
Fig. 1-2 shows the influence of three different graphene contents on the tensile strength and tear resistance of the shielding material after the graphene master batch is added into the shielding material, and it can be seen that the tear resistance of the shielding material can be improved only by adding 0.1% of graphene in the total mass of the shielding material after the master batch is used, the influence on the tensile strength is small, and the tensile strength and the tear strength are adversely affected by adding 5% of graphene. Fig. 3 to 4 show the changes of the mooney viscosity and the volume resistivity after the shielding material is prepared by using the composite masterbatch, and it can be seen that both the mooney viscosity and the volume resistivity are reduced, which indicates that the processability and the electrical property are improved, and meanwhile, the fluctuation rate of the volume resistivity is reduced, which indicates that the electrical property stability is improved.
Preferably, the colloidal graphene is composed of the following components: 0.05-3 parts of graphene, 0.05-0.5 part of coupling agent, 0.05-0.5 part of dicumyl peroxide, 10-20 parts of pretreatment liquid and 20-40 parts of liquid ethylene propylene rubber. Wherein the concentration of graphene in the colloidal graphene is 0.1-5%, the coupling agent is one or a combination of two of vinyldimethylsilane and vinyltriethoxysilane, and the pretreatment liquid is paraffin oil and diethylene glycol in a mass ratio of 2:1, and the molecular weight of the liquid ethylene propylene rubber is 1-4 ten thousand.
A preparation method of conductive composite master batches for rubber shielding materials is prepared by the following steps:
(1) putting the pretreatment liquid in the colloidal graphene component into a ball mill, putting graphene and a coupling agent into the ball mill for three times according to the proportion to mix for 30-60min, blanking and standing to obtain a graphene dispersion liquid, putting the graphene dispersion liquid and liquid ethylene propylene rubber into a vacuum kneader according to the proportion to mix for 8-12 min at 30-50 ℃, then putting dicumyl peroxide according to the proportion, quickly heating to 150-160 ℃ after mixing for 1-3 min, continuously stirring for 5-10 min, and cooling for later use after blanking to obtain colloidal graphene;
(2) putting the part of the superconducting carbon black A into a high-speed crushing stirrer with the rotating speed of more than 1000r/min, crushing to obtain conductive carbon black B, and uniformly mixing the other part of the superconducting carbon black A and the crushed conductive carbon black B according to the mass ratio of 2:1 for later use to obtain a superconducting carbon black combination;
(3) and (3) mixing the spare material obtained in the steps (1) and (2) and paraffin oil in a stirrer with the rotating speed of 500-1000r/min for 10-20 minutes according to the components and the proportion to obtain the conductive composite master batch.
The invention has the beneficial effects that:
1. the composite master batch modifies the graphene and makes the graphene into a colloid, so that the effect of mutually isolating the graphene and the conductive carbon black is realized, the adsorption covering effect of the graphene conductive carbon black is avoided, the effect of improving the performance of the shielding material only by using a small amount of graphene is achieved, the purposes of reducing the using amount of high-cost graphene and reducing the process loss are realized, and the application cost of the graphene is reduced.
2. The shielding material prepared by using the composite master batch has the advantages of reduced Mooney viscosity, improved processability, improved tear resistance, reduced volume resistivity, namely improved electrical property, greatly reduced carbon black powder consumption after the master batch mode is used, and easily controlled material cleanliness.
3. The preparation process of the composite master batch and the product do not need to be dried, the process flow is shortened, the production efficiency is improved, a large amount of water and electricity loss is reduced, and the batch production is easy to realize by using conventional industrial equipment.
Drawings
FIG. 1 shows the tensile strength test results of different contents of graphene;
FIG. 2 shows the tear strength test results for different contents of graphene;
FIG. 3 shows the Mooney viscosity of the shielding material;
fig. 4 shows the change of the volume resistivity of two types of shields.
Detailed Description
The technical solution of the present invention is further specifically described below by way of specific examples.
Example 1: a conductive composite master batch for a rubber cable shielding material is composed of the following components in parts by mass: 60 parts of colloidal graphene, 30 parts of superconducting carbon black combination and 10 parts of paraffin oil. The colloidal graphene consists of the following components: 0.1 part of graphene, 0.1 part of coupling agent, 0.3 part of dicumyl peroxide, 18.5 parts of pretreatment liquid (wherein 12.34 parts of paraffin oil and 6.16 parts of diethylene glycol) and 40 parts of liquid ethylene propylene rubber. Wherein the effective content of the conductive substance accounts for 30.1 percent of the total mass. The superconducting carbon black is prepared from carbon black with specific surface area less than 90m 2 A superconducting carbon black A with a particle size of more than 40 nm and a specific surface area of less than 100m 2 The superconducting carbon black B with the grain diameter less than 20 nanometers is prepared from the following components in a mass ratio of 2:1 are combined.
The preparation method comprises the following steps:
(1) putting the pretreatment liquid in parts by mass into a ball mill, putting graphene and a coupling agent into the ball mill for mixing for 30min in three times according to the proportion, blanking and standing to obtain graphene dispersion liquid, putting the graphene dispersion liquid and liquid ethylene propylene rubber into a vacuum kneader according to the proportion, mixing for 10 min at 30 ℃, then putting dicumyl peroxide according to the proportion, mixing for 2 min, rapidly heating to 155 ℃, continuing to stir for 5 min, blanking and cooling for later use to obtain colloidal graphene;
(2) putting part of the superconducting carbon black A into a high-speed crushing stirrer with the rotating speed of 1200r/min, crushing to obtain superconducting carbon black B, and uniformly mixing the other part of the superconducting carbon black A and the crushed conductive carbon black B according to the mass ratio of 2:1 for later use to obtain a superconducting carbon black combination;
(3) and (3) mixing the two materials obtained in the steps (1) and (2) and paraffin oil according to the components and the mixture ratio in a stirrer with the rotating speed of 800r/min for 12 minutes to obtain the conductive composite master batch.
Example 2: a conductive composite master batch for a rubber cable shielding material,the adhesive comprises the following components in parts by mass: 50 parts of colloidal graphene, 35 parts of superconducting carbon black combination and 15 parts of paraffin oil. The colloidal graphene consists of the following components: 0.8 part of graphene, 0.2 part of coupling agent, 0.22 part of dicumyl peroxide, 13.78 parts of pretreatment liquid (9.18 parts of paraffin oil and 4.6 parts of diethylene glycol) and 35 parts of liquid ethylene propylene rubber. Wherein the effective content of the conductive substance accounts for 35.8 percent of the total mass. The superconducting carbon black is prepared from carbon black with specific surface area less than 90m 2 A superconducting carbon black A with a particle size of more than 40 nm and a specific surface area of less than 100m 2 The superconducting carbon black B with the grain diameter less than 20 nanometers is prepared from the following components in a mass ratio of 2:1 are combined.
The preparation method comprises the following steps:
(1) putting the pretreatment liquid into a ball mill according to the mass part, putting graphene and a coupling agent into the ball mill for mixing for 40min in three times according to the proportion, blanking and standing to obtain a graphene dispersion liquid, putting the graphene dispersion liquid and liquid ethylene propylene rubber into a vacuum kneader according to the proportion, mixing for 10 min at 38 ℃, then putting dicumyl peroxide according to the proportion, mixing for 2 min, rapidly heating to 152 ℃, continuing stirring for 8 min, blanking and cooling for later use to obtain colloidal graphene;
(2) putting part of the superconducting carbon black A into a high-speed crushing stirrer with the rotating speed of 1200r/min, crushing to obtain superconducting carbon black B, and uniformly mixing the other part of the superconducting carbon black A and the crushed conductive carbon black B according to the mass ratio of 2:1 for later use to obtain a superconducting carbon black combination;
(3) and (3) mixing the two materials obtained in the steps (1) and (2) and paraffin oil for 10 minutes in a stirrer with the rotating speed of 1000r/min according to the components and the mixture ratio to obtain the conductive composite master batch.
Example 3: a conductive composite master batch for a rubber cable shielding material is composed of the following components in parts by mass: 40 parts of colloidal graphene, 40 parts of superconducting carbon black combination and 20 parts of paraffin oil. The colloidal graphene is composed of the following components: 2 parts of graphene, 0.4 part of coupling agent, 0.2 part of dicumyl peroxide, 8 parts of pretreatment liquid (5.3 parts of paraffin oil and 2.7 parts of diethylene glycol) and 29.4 parts of liquid ethylene propylene rubber. Wherein the effective content of the conductive substance accounts for the total mass42% of the amount. The superconducting carbon black is prepared from carbon black with specific surface area less than 90m 2 A superconducting carbon black A with a particle size of more than 40 nm and a specific surface area of less than 100m 2 The superconducting carbon black B with the grain diameter less than 20 nanometers is prepared from the following components in percentage by mass: 1 are combined.
The preparation method comprises the following steps:
(1) putting the pretreatment liquid in parts by mass into a ball mill, putting graphene and a coupling agent into the ball mill for mixing for 60min in three times according to the proportion, blanking and standing to obtain graphene dispersion liquid, putting the graphene dispersion liquid and liquid ethylene propylene rubber into a vacuum kneader according to the proportion, mixing for 10 min at 48 ℃, then putting dicumyl peroxide according to the proportion, mixing for 2 min, rapidly heating to 158 ℃, continuing stirring for 10 min, blanking and cooling for later use to obtain colloidal graphene;
(2) putting part of the superconducting carbon black A into a high-speed crushing stirrer with the rotation speed of 1200r/min, crushing to obtain superconducting carbon black B, and uniformly mixing the other part of the superconducting carbon black A and the crushed conductive carbon black B according to the mass ratio of 2:1 for later use to obtain a superconducting carbon black combination;
(3) and (3) mixing the two materials obtained in the steps (1) and (2) and paraffin oil for 15 minutes in a stirrer with the rotating speed of 900r/min according to the components and the proportion to obtain the conductive composite master batch.
The use method of the conductive composite master batch for the rubber cable shielding material comprises the following steps:
the conductive composite master batch prepared according to the embodiments 1 to 3 is added into the existing shielding material formula to replace partial carbon black, in order to reduce the influence of other factors, the conductive carbon black in the formula is replaced by the graphene and the conductive carbon black in the master batch in equal amount, the plasticizer in the formula is replaced by the rest components in equal amount, the total gel content is kept unchanged, the total amount of the conductive substances is kept unchanged, the cable shielding material is prepared according to the formula, the dumbbell type test sample with the thickness of 2mm is obtained by vulcanization sampling, the test sample is tested according to the national standard GB/T529 to obtain the tear strength, the Mooney viscosity is tested according to the GB/T1232, the volume resistivity is tested according to the GB/T3048, and the results are as follows:
table 1: test results
| Comparative example | Example 1 | Example 2 | Example 3 | |
| Mooney viscosity at 100 DEG C | 56.8 | 50.5 | 52.6 | 54.3 |
| Tear Strength N/mm | 48.3 | 56.5 | 54.8 | 53.1 |
| Volume resistivity mean |
55 | 37 | 35 | 41 |
As can be seen by combining fig. 1-4 and table 1, the reduced mooney viscosity of the cable shielding material prepared from the conductive composite master batch prepared by the invention means better processability, the improved tearing strength, and the problem that the cable shielding is easy to tear in application, and meanwhile, as can be seen from the volume resistivity data in the table above and the condition that the resistivity mean value is shifted down and the resistivity fluctuation condition in the repeatability verification result chart shown in fig. 4, the shielding material prepared from the conductive composite master batch has greatly improved electrical property and electrical property stability.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (6)
1. The utility model provides a compound master batch of electrically conductive for rubber cable shielding material which characterized in that: the composition comprises the following components in parts by mass:
40-60 parts of colloidal graphene, 25-40 parts of superconducting carbon black combination and 10-20 parts of paraffin oil;
wherein: the effective content of the conductive substance accounts for 30-45% of the total mass;
the superconducting carbon black combination is composed of a specific surface area of less than 90m 2 A superconducting carbon black A with a particle size of more than 40 nm and a specific surface area of less than 100m 2 The superconducting carbon black B with the grain diameter less than 20 nanometers is prepared from the following components in a mass ratio of 2:1, combining the components;
the colloidal graphene comprises the following components in parts by weight: 0.05-3 parts of graphene, 0.05-0.5 part of coupling agent, 0.05-0.5 part of dicumyl peroxide, 10-20 parts of pretreatment liquid and 20-40 parts of liquid ethylene propylene rubber;
the concentration of graphene in the colloidal graphene is 0.1-5%, and the graphene is one or a combination of a single layer or a few layers of graphene.
2. The conductive composite master batch for the rubber cable shielding material according to claim 1, wherein the conductive composite master batch comprises the following components in percentage by weight: the paraffin oil has a kinematic viscosity of more than 95mm at 40 deg.C 2 Petroleum based liquids/s and having a flash point greater than 230 ℃A paraffinic oil.
3. The conductive composite master batch for the rubber cable shielding material according to claim 1, wherein the conductive composite master batch comprises the following components in percentage by weight: the coupling agent is one or the combination of two of vinyldimethylsilane and vinyltriethoxysilane.
4. The conductive composite master batch for the rubber cable shielding material according to claim 1, wherein the conductive composite master batch comprises the following components in percentage by weight: the pretreatment liquid is paraffin oil and diethylene glycol according to a mass ratio of 2:1 are mixed.
5. The conductive composite masterbatch for the rubber cable shielding material according to claim 1, wherein: the molecular weight of the liquid ethylene propylene rubber is 1-4 ten thousand.
6. The preparation method of the conductive composite masterbatch according to any one of claims 1 to 5, characterized by comprising the following steps:
(1) putting the pretreatment liquid into a ball mill, putting the graphene and the coupling agent into the ball mill for mixing for 30-60min in three times according to the proportion, blanking and standing to obtain graphene dispersion liquid, putting the graphene dispersion liquid and the liquid ethylene propylene rubber into a vacuum kneader according to the proportion, mixing for 8-12 min at 30-50 ℃, then putting dicumyl peroxide according to the proportion, mixing for 1-3 min, rapidly heating to 150-160 ℃, continuously stirring for 5-10 min, and cooling for later use after blanking to obtain colloidal graphene;
(2) putting part of the superconducting carbon black A into a high-speed crushing stirrer with the rotating speed of more than 1000r/min, crushing to obtain conductive carbon black B, and uniformly mixing the other part of the superconducting carbon black A and the crushed conductive carbon black B according to the mass ratio of 2:1 for later use to obtain a superconducting carbon black combination;
mixing the spare material and paraffin oil obtained in the steps (1) and (2) according to the components and the proportion in the mixer with the rotating speed of 500-1000r/min for 10-20 minutes to obtain the conductive composite master batch.
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| CN112280231A (en) * | 2020-10-14 | 2021-01-29 | 南方电网科学研究院有限责任公司 | Shielding material for polypropylene-based thermoplastic cable and preparation method thereof |
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