CN115806716A - Thermoplastic recyclable insulating material and preparation method and application thereof - Google Patents
Thermoplastic recyclable insulating material and preparation method and application thereof Download PDFInfo
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- CN115806716A CN115806716A CN202211415241.3A CN202211415241A CN115806716A CN 115806716 A CN115806716 A CN 115806716A CN 202211415241 A CN202211415241 A CN 202211415241A CN 115806716 A CN115806716 A CN 115806716A
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Abstract
The invention provides a thermoplastic recyclable insulating material and a preparation method and application thereof. The invention provides a thermoplastic recyclable insulating material, which is obtained by melting, extruding and granulating a polypropylene grafted product and an auxiliary agent; the polypropylene graft product comprises first structural units derived from polypropylene and functional second structural units grafted on the first structural units; before and after aging, the change rates of the direct current resistivity, the breakdown field strength, the tensile strength and the elongation at break of the insulating material are all less than or equal to 10 percent. The insulating material provided by the invention has better aging resistance, and is beneficial to prolonging the service life and stabilizing the operation time of the polypropylene insulating material.
Description
Technical Field
The invention relates to a thermoplastic recyclable insulating material, a preparation method and application thereof, and relates to the technical field of insulating materials.
Background
The high molecular polymer material has excellent electrical insulation performance and lower manufacturing cost, so that the high molecular polymer material is widely applied to the field of electrical engineering and the power industry as an insulation material of power equipment. With the rapid development of the power industry, the power grid system moves towards higher voltage level and larger electric energy transmission capacity, and higher requirements are put forward on the performance of the insulating material. With this trend, the conventional polyethylene-based insulation materials have failed to meet the higher long-term operating temperature and the stronger electric field (the maximum long-term operating temperature of the insulation materials of the crosslinked polyethylene currently used is 70-90 ℃). There is therefore an urgent need to develop new insulating materials to accommodate higher long-term operating temperatures and stronger electric fields. In addition, since the crosslinked polyethylene material needs to be crosslinked during the production process to improve the thermal stability, the material is changed from original thermoplastic to thermosetting, on one hand, the crosslinking consumes a large amount of energy, and the degassing process generates waste gas; on the other hand, the thermosetting crosslinked polyethylene cannot be recycled after the service life of the cable insulation is over, and can only be treated by the traditional methods such as incineration, so that the environment is seriously polluted. In view of the above, the inherent properties of crosslinked polyethylene have not been able to meet the development requirements of environmental protection power systems and energy systems under the "dual carbon" strategy.
The polypropylene has the advantages of polyethylene as a high molecular polymer material, has better electrical insulation performance and higher melting point compared with polyethylene, is expected to adapt to more severe working environment as an insulation material, has the characteristic of thermoplastic recyclability, does not need a crosslinking degassing process and can realize recycling and reprocessing when the service life is over, thereby meeting the strategic development requirement of double carbon of an energy system. However, the attention of those skilled in the art is paid to how to improve the aging resistance, the service life and the stable operation time of polypropylene insulation materials.
Disclosure of Invention
The invention provides a thermoplastic recyclable insulating material, and a preparation method and application thereof, which are used for improving the aging resistance of a polypropylene insulating material, prolonging the service life of the polypropylene insulating material and stabilizing the operation time.
The invention provides a thermoplastic recyclable insulating material, which is obtained by melt extrusion and granulation of a polypropylene grafted product and an auxiliary agent;
the polypropylene graft product comprises first structural units derived from polypropylene and functional second structural units grafted onto the first structural units;
under the same test condition, the direct current resistivity of the insulating material before aging is rho 1 d.C. resistivity after aging is rho 2 ，(ρ 1 -ρ 2 )/ρ 1 ≤10％；
The breakdown field strength of the insulating material before aging is E g1 Breakdown field strength after aging is E g2 ，(E g1 -E g2 )/E g1 ≤10％；
The tensile strength of the insulating material before aging is M 1 Elongation at break of N 1 Tensile strength after aging of M 2 Elongation at break of N 2 ，(M 1 -M 2 )/M 1 ≤10％，(N 1 -N 2 )/N 1 ≤10％。
The structure of the polypropylene grafted product provided by the invention comprises a first structural unit and a second structural unit, wherein the first structural unit comprises a structure polymerized by propylene or a polymerized monomer containing a propylene group, and the second structural unit is a structural unit polymerized by a functional monomer and grafted on the first structural unit as a side chain.
The thermoplastic recyclable insulating material provided by the invention is obtained by melting, extruding and granulating a polypropylene graft product and an auxiliary agent, grafting and modifying polypropylene by using a functional monomer, wherein in the crystallization process of the graft product, graft chains formed by the functional monomer tend to be repelled by polypropylene molecular chains and intertwined with each other to form a spherical intertwining structure, so that the thermoplastic recyclable insulating material has a binding effect on the surrounding polypropylene molecular chains and enhances the bonding strength between the molecular chains. In the aging process, the amorphous region can firstly undergo a degradation reaction, so that the structure of the amorphous region is looser, the improvement of the solubility and the diffusion rate of oxygen is facilitated, the aging degradation reaction is accelerated, the entanglement structure among the graft chains is helpful for inhibiting the loosening of the structure of the amorphous region in the aging process, and the aging resistance is further improved, and particularly, the change rates of the direct current resistivity, the breakdown field strength, the tensile strength and the elongation at break of the insulating material before and after aging under a certain aging condition are not higher than 10%. Therefore, compared with a polypropylene material which is not grafted and modified, the insulating material provided by the invention has better aging resistance, and is beneficial to prolonging the service life of polypropylene insulation and stabilizing the operation time.
The direct current resistivity, the breakdown field strength, the tensile strength and the elongation at break provided by the invention can be tested by adopting the conventional technical means in the field, and the test conditions before and after aging are the same.
In a specific embodiment, the first structural unit is a homo-polypropylene structural unit or an ethylene-propylene random copolymer polypropylene structural unit, and the polymerization monomer in the second structural unit is methyl methacrylate or vinyltriethoxysilane, i.e., the homo-polypropylene or the ethylene-propylene random copolymer polypropylene and the methyl methacrylate or the vinyltriethoxysilane undergo a graft copolymerization reaction, so that the methacrylate or the vinyltriethoxysilane is polymerized and grafted on a molecular chain of the polypropylene to obtain a grafted product.
Specifically, the homo-polypropylene refers to polypropylene polymerized from a single propylene monomer, and the homo-polypropylene can be selected from isotactic polypropylene (methyl side groups in the homo-polypropylene are sequentially arranged), syndiotactic polypropylene (methyl side groups in the homo-polypropylene are sequentially arranged at intervals), and atactic polypropylene (methyl side groups in the homo-polypropylene are randomly arranged) according to the different connection sequence of the propylene monomers in the molecular structure of the homo-polypropylene from end to end; further, the homo-polypropylene is isotactic polypropylene.
The structural unit of the ethylene-propylene random copolymerization polypropylene is obtained by copolymerizing ethylene and propylene monomers serving as polymerization monomers, and a propylene chain segment and an ethylene chain segment are randomly distributed in a main chain.
According to researches, the aging resistance of the insulating material is improved to different degrees along with the increase of the grafting rate of the second structural units, but the aging resistance of the insulating material is greatly reduced when the grafting rate of the second structural units is improved to a certain degree, so that the content of the second structural units in a grafted state in the thermoplastic recyclable insulating material is 0.5-18wt%, namely the mass of the functional second structural units/the mass of the first structural units is 0.5-18wt%; further, the content of the functional second structural unit in a grafted state is 1 to 15wt%, for example, 1wt%, 2wt%, 3wt%, 5wt%, 8wt%, 10wt%, 12wt%, 15wt%, or a range consisting of any two thereof.
The breakdown field intensity Eg of the thermoplastic recyclable insulating material before aging is larger than 290kV/mm, and further, the breakdown field intensity E of the insulating material before aging g 310-1000kV/mm, and further, the breakdown field strength E of the insulating material before aging g 330-900kV/mm, for example 330kV/mm, 360kV/mm, 380kV/mm, 400kV/mm, 450kV/mm, 500kV/mm, 800kV/mm, 900kV/mm or a range consisting of any two thereof.
The DC resistivity of the insulating material before aging is more than 1.5 multiplied by 10 13 Omega. M, and further, the DC resistivity of the insulating material before aging was 2.5X 10 13 -1.0×10 22 Ω · m, e.g. 2.5X 10 13 Ω·m、5×10 13 Ω·m、10 14 Ω·m、10 15 Ω·m、10 20 Ω·m、10 22 Ω · m or any two thereof, and dc resistivity, as measured according to the method specified in GB/T1410-2006.
The tensile strength of the insulating material before aging is more than or equal to 20MPa, and the elongation at break is more than or equal to 400%.
The melt flow rate of the insulation material is 0.1-18g/10min, further the melt flow rate of the insulation material is 0.3-15g/10min, further the melt flow rate of the insulation material is 0.6-10g/10min, such as 0.6g/10min, 2g/10min, 3g/10min, 5g/10min, 10g/10min or a range consisting of any two of the above;
the melting temperature of the insulating material is 105-190 ℃, further the melting temperature is 110-170 ℃, such as 110 ℃, 140 ℃, 150 ℃, 160 ℃, 170 ℃ or any two of the ranges.
All the performance parameters related to the invention can be obtained by testing according to the conventional technical means in the field.
The second aspect of the present invention provides a method for preparing the above insulating material, wherein the method is obtained by melt-extruding and granulating a polypropylene graft product and an auxiliary agent, and the graft product is obtained by performing a grafting reaction between a polypropylene matrix and a functional monomer in an inert gas atmosphere, and specifically comprises the following steps:
step 1, mixing polypropylene and a functional monomer in the presence of inert gas, and carrying out grafting reaction to obtain a polypropylene grafting product;
in the grafting reaction process, grafting points can be formed on the polypropylene by treatment with a radical initiator, and then a functional monomer is grafted on the grafting points to complete the grafting reaction.
Further, the radical initiator is selected from peroxide-based radical initiators, specifically, the peroxide-based radical initiator is selected from one or more of dibenzoyl peroxide, dicumyl peroxide, di-tert-butyl peroxide, lauroyl peroxide, tert-butyl peroxybenzoate, diisopropyl oxide dicarbonate, tert-butyl peroxy (2-ethylhexanoate) peroxide and dicyclohexyl peroxydicarbonate.
The addition amount of the free radical initiator is 0.01-1% of the mass of the polypropylene, the temperature of the grafting reaction is 80-130 ℃, and the reaction time is 0.5-10h.
The grafting reaction provided by the invention can be added with an interfacial agent for swelling the polypropylene, and the interfacial agent can be specifically selected from one or more of an ether solvent, a ketone solvent, an aromatic hydrocarbon solvent and an alkane solvent; further, the interfacial agent is selected from one or more of chlorobenzene, polychlorinated benzene, alkane or cycloalkane with more than 6 carbon atoms, benzene, C1-C4 alkyl substituted benzene, C2-C6 fatty ether, C3-C6 fatty ketone and decalin; further, the interfacial agent is selected from one or more of benzene, toluene, xylene, chlorobenzene, tetrahydrofuran, diethyl ether, acetone, hexane, cyclohexane, decahydronaphthalene and heptane; the mass of the interface agent is 1-30% of the mass of the polypropylene.
A dispersing agent can be added in the grafting reaction provided by the invention, so that a relatively stable suspension can be formed, and the dispersing agent is water or an aqueous solution of sodium chloride; the mass of the dispersant is 30-300% of that of the polypropylene.
And 2, mixing the polypropylene grafted product with an auxiliary agent, and performing melt extrusion granulation to obtain the thermoplastic recyclable insulating material.
On the basis of preparing the grafted product, the grafted product and an auxiliary agent are mixed and then subjected to melt extrusion granulation to obtain the thermoplastic material, wherein the auxiliary agent comprises an antioxidant and optionally other auxiliary agents, the antioxidant is added into the polypropylene in an amount of more than 1500ppm, and the other auxiliary agents comprise any one or more of a voltage stabilizer, an anti-aging agent, a copper resisting agent and a processing auxiliary agent. The type and amount of other adjuvants used are conventional and known to those skilled in the art.
The melt extrusion granulation can be carried out in an extruder, the extrusion processing temperature is 180-250 ℃, further, the extrusion processing temperature is 190-220 ℃, and the temperature of each zone and the specific process can be carried out according to the conventional technical means in the field.
A third aspect of the invention provides the use of the above thermoplastic recyclable insulating material in an insulating material.
The insulating material provided by the invention has low charge injection accumulation amount and high charge dissipation rate, can be used as a main insulating material of a high-voltage direct-current cable, and is used in the field of insulating materials of direct-current cables.
The change rates of the direct current resistivity, the breakdown field strength, the tensile strength and the elongation at break of the insulating material before and after aging under a certain aging condition are not higher than 10%, and compared with a polypropylene material which is not grafted and modified, the insulating material provided by the invention has better aging resistance, and is beneficial to prolonging the service life and stabilizing the operation time of polypropylene insulation; meanwhile, the matrix material adopted by the method is a thermoplastic material, can be recycled, and is beneficial to environmental protection.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the following examples, the raw materials used and the purchasers are shown in table 1:
TABLE 1
| Name (R) | Description of the invention |
| T30s | Homopolymerized polypropylene, and ring tube production by long-distance refining. |
| GM250E | Atactic ethylene-propylene copolymerized polypropylene, shanghai stone production |
| Dibenzoyl peroxide | Bailingwei Tech Ltd (J)&K Chemicals) |
| Vinyl triethoxy silane | Bailingwei Tech Co Ltd (J)&K Chemicals) |
| Methacrylic acid methyl ester | Bailingwei Tech Co Ltd (J)&K Chemicals) |
| Vinyl pyridinePyrrolidinones | Bailingwei Tech Co Ltd (J)&K Chemicals) |
Example 1
The preparation method of the polypropylene insulating material provided by the embodiment comprises the following steps:
weighing 2.0kg of T30s powder, adding the powder into a 10L reaction kettle with mechanical stirring, sealing the reaction system, and removing oxygen by nitrogen replacement. 4.8g of dibenzoyl peroxide and 320g of methyl methacrylate are added, stirred and mixed for 30 minutes, dispersant water is added, swelling is carried out for 2 hours at 50 ℃, the temperature is raised to 90 ℃, and reaction is carried out for 4 hours. After the reaction is finished, cooling, filtering to remove the dispersant water, and vacuum drying at 70 ℃ for 10 hours to obtain the polypropylene-g-methyl methacrylate powder.
Weighing 1.0kg of polypropylene-g-methyl methacrylate powder, adding 3000ppm of antioxidant 1010/168 (in a mass ratio of 1:1) into a high-speed stirrer, and uniformly mixing. And granulating by a double-screw extruder to obtain the composite material C1.
Example 2
The preparation method of the polypropylene insulating material provided by the embodiment comprises the following steps:
weighing 2.0kg of GM250E powder, adding the powder into a 10L reaction kettle with mechanical stirring, sealing the reaction system, and removing oxygen by nitrogen replacement. 3.4g of dibenzoyl peroxide and 170g of methyl methacrylate are added, stirred and mixed for 30 minutes, dispersant water is added, swelling is carried out for 2 hours at 40 ℃, the temperature is raised to 100 ℃, and reaction is carried out for 3 hours. After the reaction is finished, cooling, and vacuum drying at 70 ℃ for 10 hours to obtain the polypropylene-g-methyl methacrylate powder.
Weighing 1.0kg of polypropylene-g-methyl methacrylate powder, adding 3000ppm of antioxidant 1010/168 (in a mass ratio of 1:1), adding into a high-speed stirrer, uniformly mixing, and granulating by using a double-screw extruder at the temperature of 190-220 ℃ to obtain the composite material C2.
Example 3
The preparation method of the polypropylene insulating material provided by the embodiment comprises the following steps:
weighing 2.0kg of T30s powder, adding the powder into a 10L reaction kettle with mechanical stirring, sealing the reaction system, and removing oxygen by nitrogen replacement. Adding 1.05g of dibenzoyl peroxide and 105g of vinyl triethoxysilane, stirring and mixing for 20 minutes, adding dispersant water, swelling for 2 hours at 40 ℃, heating to 90 ℃, and reacting for 3 hours. After the reaction is finished, cooling, and vacuum drying at 70 ℃ for 10 hours to obtain the polypropylene-g-vinyltriethoxysilane powder.
Weighing 1.0kg of polypropylene-g-vinyltriethoxysilane powder, adding 3000ppm of antioxidant 1010/168 (in a mass ratio of 1:1) into a high-speed stirrer, and uniformly mixing. And granulating by a double-screw extruder at the temperature of 190-220 ℃ to obtain the composite material C3.
Comparative example 1
The preparation method of the polypropylene insulating material provided by the comparative example comprises the following steps:
weighing 1.0kg of T30s, adding 3000ppm of antioxidant 1010/168 (in a mass ratio of 1:1), adding into a high-speed stirrer, uniformly mixing, and granulating by a double-screw extruder at the temperature of 190-220 ℃ to obtain a product D1.
Comparative example 2
The preparation method of the polypropylene insulating material provided by the comparative example comprises the following steps:
weighing 2.0kg of T30s powder, adding the powder into a 10L reaction kettle with mechanical stirring, sealing the reaction system, and removing oxygen by nitrogen replacement. Adding 15g of dibenzoyl peroxide and 1000g of methyl methacrylate, stirring and mixing for 30 minutes, adding dispersant water, swelling for 2 hours at 40 ℃, heating to 95 ℃, and reacting for 5 hours. After the reaction is finished, cooling, and vacuum drying at 70 ℃ for 10 hours to obtain the polypropylene-g-methyl methacrylate powder.
Weighing 1.0kg of polypropylene-g-methyl methacrylate powder, adding 3000ppm of antioxidant 1010/168 (in a mass ratio of 1:1) into a high-speed stirrer, and uniformly mixing. And granulating by a double-screw extruder at the temperature of 190-220 ℃ to obtain the composite material D2.
Comparative example 3
The preparation method of the polypropylene insulating material provided by the comparative example comprises the following steps:
weighing 2.0kg of GM250E powder, adding the powder into a 10L reaction kettle with mechanical stirring, sealing the reaction system, and removing oxygen by nitrogen replacement. Adding 3.5g of dibenzoyl peroxide and 170g of vinyl pyrrolidone, stirring and mixing for 30 minutes, adding dispersant water, swelling for 2 hours at 40 ℃, heating to 100 ℃, and reacting for 3 hours. After the reaction is finished, cooling, and vacuum drying at 70 ℃ for 10 hours to obtain the polypropylene-g-vinyl pyrrolidone powder.
Weighing 1.0kg of polypropylene-g-vinyl pyrrolidone powder, adding 3000ppm of antioxidant 1010/168 (in a mass ratio of 1:1), adding into a high-speed stirrer, uniformly mixing, and granulating by using a double-screw extruder, wherein the temperature of the extruder is 190-220 ℃, so as to obtain the composite material D3.
The graft products and the insulation materials according to examples 1 to 3 and comparative examples 1 to 3 were tested according to the following test items and methods, and the test results are shown in Table 2:
1. determination of the graft ratio GD:
placing 2-4g of the grafting product into a Soxhlet extractor, extracting with an organic solvent ethyl acetate for 24 hours, removing unreacted monomers and homopolymers thereof to obtain a pure grafting product, drying and weighing, and calculating the grafting rate GD of functional monomers, wherein the calculation formula is shown as formula 1:
in the formula 1, w 0 Is the mass of polypropylene, w 2 Is the mass of the grafted product after extraction.
2. Determination of the melt flow Rate MFR:
the melt flow rate MFR of the insulation material was determined at 230 ℃ under a load of 2.16kg using a melt index apparatus of type 7026 from CEAST, according to the method specified in GB/T3682-2018.
3. Determination of the melting temperature Tm:
the melting process and the crystallization process of the material were analyzed by differential scanning calorimetry. The specific operation is as follows: under the protection of nitrogen, 5-10mg of a sample is measured from 20 ℃ to 200 ℃ by a three-stage temperature rise and fall measuring method, and the melting and crystallization processes of the material are reflected by the change of heat flow, so that the melting temperature Tm is calculated.
4. Determination of breakdown field strength:
the measurement was carried out according to the method defined in GB/T1408-2006.
5. Measurement of direct current resistivity:
the measurement was carried out according to the method defined in GB/T1410-2006. The test conditions were 110 ℃ and 40Kv/mm.
6. Determination of tensile strength and elongation at break:
the measurement was carried out according to the method defined in GB/T1040.2-2006.
7. Method of aging test:
the aging is carried out by referring to the method specified in GB/T2951.2, and specifically at 135 ℃ for 7 days.
Table 2 test results of the insulating materials provided in examples 1 to 3 and comparative examples 1 to 3
As can be seen from Table 2, the base material without functional monomer graft modification has significantly reduced performance before and after aging, and poor aging resistance, and when the graft content of the functional monomer is too high and the grafted functional monomer is different, the aging resistance of the insulating material is also affected, and the service life and long-term stable operation of the polypropylene insulating material are also affected.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. The thermoplastic recyclable insulating material is characterized in that the thermoplastic recyclable insulating material is obtained by melt extrusion granulation of a polypropylene grafted product and an auxiliary agent;
the polypropylene graft product comprises first structural units derived from polypropylene and functional second structural units grafted onto the first structural units;
under the same test condition, the direct current resistivity of the insulating material before aging is rho 1 d.C. resistivity after aging is rho 2 ，(ρ 1 -ρ 2 )/ρ 1 ≤10％；
The breakdown field strength of the insulating material before aging is E g1 Breakdown field strength after aging is E g2 ，(E g1 -E g2 )/E g1 ≤10％；
The tensile strength of the insulating material before aging is M 1 Elongation at break of N 1 Tensile strength after aging of M 2 Elongation at break of N 2 ，(M 1 -M 2 )/M 1 ≤10％，(N 1 -N 2 )/N 1 ≤10％。
2. The thermoplastic recyclable insulation of claim 1 wherein the first structural units are homo polypropylene structural units or ethylene propylene random co-polypropylene structural units.
3. The thermoplastic recyclable insulation material of claim 1 or 2, wherein the polymerized monomer in the second structural unit is methyl methacrylate or vinyltriethoxysilane.
4. Thermoplastic recyclable insulation material according to any of the claims 1-3, characterized in that the mass of the functional second structural units in the grafted polypropylene product is 0.5-18wt% of the mass of the first structural units.
5. The thermoplastic recyclable insulation material as described in any of claims 1-4, wherein the aids include antioxidants and other aids including any one or more of voltage stabilizers, anti-aging agents, anti-copper agents, processing aids.
6. The thermoplastic recyclable insulation material of any of claims 1-5, wherein the breakdown field E of the insulation material before aging is E g More than 290kV/mm, and DC resistivity of more than 1.5 × 10 13 Ω·m。
7. Thermoplastic recyclable insulation according to any of the claims 1-5, characterized in that the insulation has a tensile strength before ageing of not less than 20MPa and an elongation at break of not less than 400%.
8. The thermoplastic recyclable insulation material as described in any of claims 1-5, wherein the insulation material has a melt flow rate of 0.1-18g/10min and a melting temperature of 105-190 ℃.
9. A method of making the thermoplastic recyclable insulation as described in any of claims 1 to 8, comprising the steps of:
in the presence of inert gas, polypropylene and functional monomer are mixed and subjected to grafting reaction to obtain a polypropylene grafting product;
and mixing the polypropylene grafted product with an auxiliary agent, and performing melt extrusion granulation to obtain the thermoplastic recyclable insulating material.
10. Use of the thermoplastic recyclable insulation according to any of the claims 1-8 in insulation.
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| CN202211415241.3A CN115806716A (en) | 2022-11-11 | 2022-11-11 | Thermoplastic recyclable insulating material and preparation method and application thereof |
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| CN202211415241.3A CN115806716A (en) | 2022-11-11 | 2022-11-11 | Thermoplastic recyclable insulating material and preparation method and application thereof |
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