CN115806645B - High-voltage-resistant insulating material and preparation method thereof - Google Patents
High-voltage-resistant insulating material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a high-voltage resistant insulating material and a preparation method thereof, belonging to the technical field of polyethylene resin. Solves the problems that the polyethylene insulating material in the prior art has low breakdown strength, and the voltage-resistant monomer is easy to migrate and separate out, so that the breakdown strength is difficult to keep long-acting. The high-voltage resistant insulating material consists of 99-99.8wt% of pre-irradiated polyethylene resin and 0.2wt% -1.0wt% of voltage resistant monomer, wherein the structural formula of the voltage resistant monomer is shown as formula (I). The high-voltage resistant insulating material disclosed by the invention bonds the voltage resistant monomer to a polyethylene resin molecular chain, so that migration and precipitation of the voltage resistant monomer are limited, the high-breakdown strength performance can be kept for a long time, and the high-voltage direct-current breakdown strength of the high-voltage resistant insulating material is 405.2-481.2kV/mm through a high-voltage direct-current breakdown experiment.
Description
Technical Field
The invention belongs to the technical field of polyethylene resin, and particularly relates to a high-voltage-resistant insulating material and a preparation method thereof.
Background
In recent years, due to rapid development of new energy sources, factors such as long-distance power transmission and regional internet and the like, the high-voltage direct current power transmission technology is increasingly favored by the industry. The insulating material for the high-voltage direct-current transmission cable is an important component of a high-voltage transmission system, and the low breakdown strength of the insulating material is a key factor for limiting the development of the high-voltage direct-current transmission system. Scientists strive to improve the breakdown strength of the insulating material, on one hand, the thickness of the insulating layer can be reduced, the heat in the cable can be transmitted to the outside in time, the probability of thermal breakdown of the insulating material is reduced, and meanwhile, the cost of the insulating cable is also reduced; on the other hand, higher power transmission voltage can be ensured, the power transmission efficiency is greatly improved, and the calculation shows that if the power transmission voltage is increased to be twice as high as the original power transmission voltage, the electric energy loss on the power transmission line can be reduced to be one fourth as high as the original power transmission line. Therefore, in the construction, use and development of the high-voltage direct current power transmission system, the problem of low breakdown strength of the insulating material needs to be solved.
In order to solve the problem of low breakdown strength inherent to the insulating material itself, many methods for improving the electrical properties of the insulating material have been proposed and developed, wherein copolymerization, blending modification, inorganic nanoparticle filling modification and grafting modification are the most dominant modification methods. The grafting modification technology is an efficient modification method of the polymer insulating material, and has the advantages of simple production process and low cost, and the polymer matrix breakdown strength can be remarkably improved by only grafting high-efficiency functional monomers from the standpoint of designing the macromolecular chain structure of the polymer.
The voltage-resistant monomer is an organic micromolecular compound, can obviously improve the breakdown strength of the polymer, and is widely used for improving the voltage-resistant breakdown performance of the polymer insulating material. For example, a cable insulation material and a preparation method thereof (CN 114621512A) in China disclose that 4-isopropoxybenzoic acid, 2, 5-dimethoxy phenylboronic acid and o-methoxy phenylboronic acid are used as voltage stabilizers to improve the breakdown strength of a polymer. However, the voltage-resistant monomer has a phase difference with a nonpolar polymer, and is easy to migrate and precipitate from the inside of the polymer to the surface of the polymer, so that the breakdown strength of the modified polymer is difficult to keep long-acting.
Disclosure of Invention
In view of the above, the invention provides a high-voltage resistant insulating material and a preparation method thereof, which are used for solving the problems that the polyethylene insulating material in the prior art has inherent low breakdown strength, and a voltage resistant monomer is easy to migrate and separate out, so that the breakdown strength is difficult to maintain long-term.
The technical scheme adopted by the invention for solving the technical problems is as follows.
The invention provides a high-voltage resistant insulating material which consists of 99-99.8 wt% of pre-irradiation polyethylene resin and 0.2-1.0 wt% of voltage resistant monomer, wherein the structural formula of the voltage resistant monomer is shown as a formula (I).
Preferably, the high voltage resistant insulating material is composed of 99.2wt% to 99.6wt% of pre-irradiated polyethylene resin and 0.4wt% to 0.8wt% of voltage resistant monomer.
More preferably, the high voltage resistant insulating material is composed of 99.4wt% of the pre-irradiated polyethylene resin and 0.6wt% of the voltage resistant monomer.
Preferably, the pre-irradiated polyethylene resin is prepared by the following method: an electron accelerator is adopted as an irradiation source, and beta-rays are used for pre-irradiating the polyethylene resin in an air atmosphere, wherein the pre-irradiation dosage range is 15-30kGy.
Preferably, the polyethylene resin is a linear low density polyethylene;
more preferably, the polyethylene resin is a lucky DFDA 7042.
Preferably, the preparation method of the voltage-resistant monomer with the structure of formula (I) comprises the following steps:
uniformly mixing 3, 6-di-tert-butylcarbazole, 3, 5-dibromostyrene, dimethylformamide, potassium carbonate, 1, 10-phenanthroline and copper iodide, reacting for 20-24 hours at 110-130 ℃ under the protection of inert atmosphere, adding ice water for quenching, filtering, washing the obtained grey green crude product with water, drying, and purifying to obtain the voltage-resistant monomer.
More preferably, the ratio of the 3, 6-di-tert-butylcarbazole, 3, 5-dibromostyrene, dimethylformamide, potassium carbonate, 1, 10-phenanthroline and copper iodide is 11.5mmol:5.1mmol:20.0ml:20.9mmol:1.2mmol:10.6mmol.
More preferably, the purification adopts silica gel column chromatography, and the volume ratio of petroleum ether to dichloromethane is 5:1.
More preferably, the inert atmosphere is nitrogen.
The invention also provides a preparation method of the high-voltage resistant insulating material, which comprises the steps of weighing the components according to the composition and the proportion, and then encrypting and refining the pre-irradiation polyethylene resin and the voltage resistant monomer to obtain the high-voltage resistant insulating material.
Preferably, the banburying temperature is 180-190 ℃, the banburying time is 6-9min, and the banburying rotating speed is 50-70rpm.
Preferably, internal mixing is performed by an internal mixer.
The preparation method of the high-voltage resistant insulating material comprises the following steps: the voltage-resistant monomer is grafted with the pre-irradiation polyethylene resin, and the voltage-resistant monomer is grafted onto a polyethylene molecular chain, so that the voltage-resistant monomer is linked with the polyethylene resin through covalent bonds, and therefore, the loss cannot occur, and the voltage-resistant time is long.
Compared with the prior art, the invention has the beneficial effects that:
(1) According to the high-voltage resistant insulating material, the multi-benzene ring compound is introduced into the polyethylene monomer through a grafting reaction, the voltage resistant monomer has low ionization energy, and can effectively dissipate energy of high-energy electrons, so that impact of the high-energy electrons on polyethylene molecular chains is avoided, the breakdown resistance of the polyethylene with a benzene ring structure is improved, the breakdown strength of the polymer insulating material is obviously improved, and through a high-voltage direct-current breakdown experiment, the direct-current breakdown strength of the high-voltage resistant insulating material is 405.2-481.2kV/mm, and the direct-current breakdown strength of polyethylene resin is 282.2-292.6kV/mm under the same conditions.
(2) According to the preparation method of the high-voltage resistant insulating material, the voltage resistant monomer is grafted onto the molecular chain of the polyethylene resin through chemical bonding by the pre-irradiation fusion grafting technology, an initiator is not used in the grafting process, adverse effects of initiator residues on dielectric strength of the polyethylene resin are avoided, the problem that polar small molecules are incompatible with the polyethylene is solved, meanwhile, homopolymerization of the voltage resistant monomer is greatly reduced, self-crosslinking of the polyethylene resin is avoided, grafting rate is improved, migration and precipitation of the voltage resistant monomer are inhibited, and as grafting can effectively inhibit migration of the voltage resistant monomer which is not grafted in the polyethylene resin, the voltage resistant group is contained in the voltage resistant monomer, the breakdown resistance of the polyethylene with a benzene ring structure is improved, and long-acting voltage resistant performance can be maintained.
Detailed Description
For a further understanding of the present invention, preferred embodiments of the invention are described below in conjunction with the detailed description, but it is to be understood that these descriptions are merely intended to illustrate further features and advantages of the invention and are not limiting of the patent claims of the invention.
The high-voltage resistant insulating material consists of 99-99.8wt% of pre-irradiated polyethylene resin and 0.2wt% -1.0wt% of voltage resistant monomer, wherein the structural formula of the voltage resistant monomer is shown as formula (I).
In the technical scheme, the high-voltage resistant insulating material can be prepared only by the pre-irradiation polyethylene resin being 99-99.8 wt% and the voltage resistant monomer being 0.2-1.0 wt%, and has high breakdown resistance and long-acting voltage resistance. The present embodiment provides several preferable ratios, but is not limited thereto, such as being composed of 99.8wt% of the pre-irradiated polyethylene resin and 0.2wt% of the voltage-resistant monomer, or being composed of 99.6wt% of the pre-irradiated polyethylene resin and 0.4wt% of the voltage-resistant monomer, or being composed of 99.4wt% of the pre-irradiated polyethylene resin and 0.6wt% of the voltage-resistant monomer, or being composed of 99.2wt% of the pre-irradiated polyethylene resin and 0.8wt% of the voltage-resistant monomer, or being composed of 99.0wt% of the pre-irradiated polyethylene resin and 1.0wt% of the voltage-resistant monomer.
In the technical scheme, the pre-irradiation polyethylene resin is preferably prepared by the following method: an electron accelerator is adopted as an irradiation source, and beta-rays are used for pre-irradiating the polyethylene resin in an air atmosphere, wherein the pre-irradiation dosage range is 15-30kGy. It should be noted that the present invention is not limited thereto, and other methods capable of realizing pre-irradiation of polyethylene are also applicable to the present invention, and the pre-irradiation is usually performed at normal temperature and normal pressure.
In the above embodiments, the polyethylene resin is preferably a linear polyethylene resin, such as DFDA 7042, which is a gigantic product. It should be noted that other polyethylenes known to those skilled in the art are also suitable for use in the present invention.
In the above technical solution, according to the structure of formula (i), a person skilled in the art can prepare the voltage-resistant monomer in this embodiment, and this embodiment provides a preparation method of the voltage-resistant monomer, but is not limited thereto: under the protection of inert atmosphere, 3, 6-di-tert-butylcarbazole, 3, 5-dibromostyrene, dimethylformamide, potassium carbonate, 1, 10-phenanthroline and copper iodide are reacted for 20-24 hours at 110-130 ℃, preferably at 120 ℃ for 24 hours, ice water is added for quenching, filtration is carried out, the obtained gray green crude product is washed with water and dried, silica gel column chromatography is carried out for purification (the volume ratio of petroleum ether to dichloromethane is 5:1), and the voltage-resistant monomer is obtained, wherein the proportion of 3, 6-di-tert-butylcarbazole, 3, 5-dibromostyrene, dimethylformamide, potassium carbonate, 1, 10-phenanthroline and copper iodide is 11.5mmol:5.1mmol:20.0ml:20.9mmol:1.2mmol:10.6mmol. The inert atmosphere is preferably nitrogen, but other inert atmospheres are also possible. The amount of ice water is added according to the actual need, and is usually 11.5mmol of 3, 6-di-tert-butylcarbazole and 50mL.
The invention also provides a preparation method of the high-voltage resistant insulating material, which comprises the following steps: firstly weighing the components according to the composition and the proportion, then adding the pre-irradiation polyethylene resin and the voltage-resistant monomer into an internal mixer, and banburying for 6-9min at 180-190 ℃ to obtain the high-voltage-resistant insulating material, wherein the rotating speed of a rotor of the internal mixer is 50-70rpm, preferably 60rpm.
The terms used in the present invention generally have meanings commonly understood by those of ordinary skill in the art unless otherwise indicated. In the invention, the normal temperature is 20-25 ℃, and the normal pressure is atmospheric pressure. High voltage refers to an ac voltage above 1000V or a dc voltage above 1500V at the distribution line.
In order to enable those skilled in the art to better understand the technical solutions of the present invention, the present invention will be described in further detail with reference to examples.
In the following examples, various processes and methods, which are not described in detail, are conventional methods well known in the art. Materials, reagents, devices, instruments, equipment and the like used in the examples described below are commercially available unless otherwise specified.
Example 1
Step one, pre-irradiating polyethylene (Ji-chemical DFDA 7042) with beta-rays of an electron accelerator at normal temperature and normal pressure under the air atmosphere, wherein the pre-irradiation dose is 15kGy, so as to obtain the pre-irradiated polyethylene resin.
Step two, 3, 6-di-tert-butylcarbazole (3.22 g, 11.5 mmol), 3, 5-dibromostyrene (1.34 g,5.1 mmol), DMF (20.0 mL), potassium carbonate (2.88 g,20.9 mmol), 1, 10-phenanthroline (0.23 g,1.2 mmol) and copper iodide (2.02 g,10.6 mmol) were added to a two-neck flask, stirred at room temperature under nitrogen atmosphere for 10 minutes, then reacted at 120 ℃ for 24 hours, poured into ice water (50 mL) to quench the reaction, filtered to obtain a grey green crude product, washed with water and dried, and further purified by silica gel column chromatography (petroleum ether/dichloromethane=5:1) to obtain 1.51g of the withstand voltage monomer represented by the structural formula (i).
And thirdly, adding 99.8 parts by weight of pre-irradiated polyethylene and 0.2 part by weight of voltage-resistant monomer with a structural formula shown as formula (I) into an internal mixer for grafting reaction, wherein the rotating speed of a rotor is 60rpm, the reaction temperature is 190 ℃, and the reaction is carried out for 6min to obtain the high-voltage-resistant insulating material.
The high voltage resistant insulation material prepared in example 1 was subjected to a high voltage direct current breakdown strength test as follows: the high voltage resistant insulating material is prepared into a round film with the diameter of 75cm and the thickness of 65+/-10 mm, the round film is tested on a GJW-50kV computer control voltage breakdown tester, a direct current breakdown mode is adopted, the boosting rate is set to be 1.0kV/mm, and the value of the high voltage direct current breakdown strength number is taken as the average value of 5 tests.
The test results are: the direct current breakdown strength of the pure polyethylene (Ji chemical DFDA 7042) is 283.1kV/mm, 282.2kV/mm, 281.5kV/mm, 280.1kV/mm, 283.2kV/mm, and the average value of 5 times of testing is 282.2kV/mm; the direct current breakdown strength of the high voltage resistant insulating material is 402.5kV/mm, 405.3kV/mm, 409.6kV/mm, 403.1kV/mm and 405.5kV/mm, and the average value of 5 tests is 405.2kV/mm.
Example 2
Step one and step two are the same as in example 1.
And thirdly, adding 99.6 parts by weight of pre-irradiated polyethylene and 0.4 part by weight of voltage-resistant monomer with a structural formula shown as formula (I) into an internal mixer for grafting reaction, wherein the rotating speed of a rotor is 60rpm, the reaction temperature is 190 ℃, and the reaction is carried out for 6 minutes to obtain the high-voltage-resistant insulating material.
The high voltage resistant insulation material prepared in example 2 was subjected to a high voltage direct current breakdown strength test, which was the same as the test method in example 1. Through tests, the direct current breakdown strength of the polyethylene is 285.3kV/mm, 281.5kV/mm, 282.1kV/mm, 283.5kV/mm and 285.1kV/mm, the average value of 5 tests is 283.5kV/mm, the direct current breakdown strength of the high voltage resistant insulating material is 432.4kV/mm, 431.2kV/mm, 427.6kV/mm, 428.3kV/mm and 426.5kV/mm, and the average value of 5 tests is 429.2kV/mm.
Example 3
Step one and step two are the same as in example 1.
And thirdly, adding 99.4 parts by weight of pre-irradiated polyethylene and 0.6 part by weight of voltage-resistant monomer with a structural formula shown as formula (I) into an internal mixer for grafting reaction, wherein the rotating speed of a rotor is 60rpm, the reaction temperature is 190 ℃, and the reaction is carried out for 6min to obtain the high-voltage-resistant insulating material.
The high voltage resistant insulating material prepared in example 3 was subjected to a high voltage direct current breakdown strength test, which was the same as the test method in example 1. Through tests, the direct current breakdown strength of the polyethylene is 292.3kV/mm, 293.5kV/mm, 294.8kV/mm, 291.6kV/mm and 290.8kV/mm, the average value of 5 tests is 292.6kV/mm, the direct current breakdown strength of the high voltage resistant insulating material is 479.4kV/mm, 478.2kV/mm, 477.6kV/mm, 478.6kV/mm and 479.2kV/mm, and the average value of 5 tests is 478.6kV/mm.
Example 4
Step one and step two are the same as in example 1.
And thirdly, adding 99.2 parts by weight of pre-irradiated polyethylene and 0.8 part by weight of voltage-resistant monomer with a structural formula shown as formula (I) into an internal mixer for grafting reaction, wherein the rotating speed of a rotor is 60rpm, the reaction temperature is 190 ℃, and the high-voltage-resistant insulating material is obtained after reaction for 6 min.
The high voltage resistant insulating material prepared in example 4 was subjected to a high voltage direct current breakdown strength test, which was the same as in example 1. Through tests, the DC breakdown strength of the polyethylene is 284.2kV/mm, 286.9kV/mm, 287.9kV/mm, 285.8kV/mm and 283.7kV/mm, the average value of 5 tests is 285.7kV/mm, the DC breakdown strength of the high-voltage resistant insulating material is 473.5kV/mm, 472.3kV/mm, 471.8kV/mm, 473.7kV/mm and 471.7kV/mm, and the average value of 5 tests is 472.6kV/mm.
Example 5
Step one and step two are the same as in example 1.
And thirdly, adding 99.0 parts by weight of pre-irradiated polyethylene and 1.0 part by weight of voltage-resistant monomer with a structural formula shown as formula (I) into an internal mixer for grafting reaction, wherein the rotating speed of a rotor is 60rpm, the reaction temperature is 190 ℃, and the high-voltage-resistant insulating material is obtained after reaction for 6 min.
The high voltage resistant insulating material prepared in example 5 was subjected to a high voltage direct current breakdown strength test, which was the same as in example 1. The DC breakdown strength of the polyethylene is 288.6kV/mm, 289.9kV/mm, 291.5kV/mm, 292.8kV/mm and 283.7kV/mm, the average value of 5 tests is 289.3kV/mm, the DC breakdown strength of the high voltage resistant insulating material is 481.3kV/mm, 480.7kV/mm, 480.2kV/mm, 481.2kV/mm and 482.6kV/mm, and the average value of 5 tests is 481.2kV/mm.
The test results of the examples 1-5 show that the high-voltage-resistant insulating material has the direct-current breakdown strength of 405.2-481.2kV/mm through a high-voltage direct-current breakdown experiment, and the direct-current breakdown strength of the polyethylene resin is 282.2-292.6kV/mm under the same conditions.
It is apparent that the above embodiments are merely examples for clarity of illustration and are not limiting examples. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. And obvious variations or modifications thereof are contemplated as falling within the scope of the present invention.
Claims (10)
1. The high-voltage resistant insulating material is characterized by comprising 99-99.8wt% of pre-irradiation polyethylene resin and 0.2wt% -1.0wt% of voltage resistant monomer, wherein the structural formula of the voltage resistant monomer is shown as formula (I).
The direct-current breakdown strength of the high-voltage resistant insulating material is 405.2-481.2kV/mm.
2. The high voltage resistant insulation material according to claim 1, characterized by consisting of 99.2wt% to 99.6wt% of the pre-irradiated polyethylene resin and 0.4wt% to 0.8wt% of the voltage resistant monomer.
3. The high voltage resistant insulation material according to claim 2, characterized in that it consists of 99.4wt% of pre-irradiated polyethylene resin and 0.6wt% of voltage resistant monomer.
4. The high voltage resistant insulation material according to claim 1, wherein the pre-irradiated polyethylene resin is prepared by the following method: an electron accelerator is adopted as an irradiation source, and beta-rays are used for pre-irradiating the polyethylene resin in an air atmosphere, wherein the pre-irradiation dosage range is 15-30kGy.
5. The high voltage resistant insulation material of claim 1, wherein the polyethylene resin is a linear low density polyethylene.
6. The high voltage resistant insulating material according to claim 1, wherein the preparation method of the voltage resistant monomer of the structure of formula (i) is as follows:
uniformly mixing 3, 6-di-tert-butylcarbazole, 3, 5-dibromostyrene, dimethylformamide, potassium carbonate, 1, 10-phenanthroline and copper iodide, reacting for 20-24 hours at 110-130 ℃ under the protection of inert atmosphere, adding ice water for quenching, filtering, washing the obtained grey green crude product with water, drying, and purifying to obtain the voltage-resistant monomer.
7. The high voltage resistant insulation material according to claim 6, wherein,
the ratio of the 3, 6-di-tert-butylcarbazole, 3, 5-dibromostyrene, dimethylformamide, potassium carbonate, 1, 10-phenanthroline and copper iodide is 11.5mmol:5.1mmol:20.0ml:20.9mmol:1.2mmol:10.6mmol;
the purification adopts silica gel column chromatography, and the volume ratio of petroleum ether to dichloromethane is (3-5) 1;
the inert atmosphere is nitrogen.
8. The method for preparing a high voltage resistant insulating material according to any one of claims 1 to 7, wherein the components are weighed according to the composition and the proportion, and then the pre-irradiated polyethylene resin and the voltage resistant monomer are encrypted to obtain the high voltage resistant insulating material.
9. The method for preparing a high voltage resistant insulation material according to claim 8, wherein the banburying temperature is 180-190 ℃, the banburying time is 6-9min, and the banburying rotating speed is 50-70rpm.
10. The method for producing a high voltage resistant insulating material according to claim 8, wherein internal mixing is performed by an internal mixer.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106893186A (en) * | 2017-04-19 | 2017-06-27 | 哈尔滨理工大学 | High dielectric property N ethyl carbazoles/composite polyethylene material and preparation method thereof |
| AU2020102276A4 (en) * | 2020-09-15 | 2020-10-29 | Tsinghua University | Preparation method of cable insulating layer material having polyolefin grafting polar group |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106893186A (en) * | 2017-04-19 | 2017-06-27 | 哈尔滨理工大学 | High dielectric property N ethyl carbazoles/composite polyethylene material and preparation method thereof |
| AU2020102276A4 (en) * | 2020-09-15 | 2020-10-29 | Tsinghua University | Preparation method of cable insulating layer material having polyolefin grafting polar group |
Non-Patent Citations (1)
| Title |
|---|
| Synthesis and Efficiency of Voltage Stabilizers for XLPE Cable Insulation;V. Englund;IEEE Transactions on Dielectrics and Electrical Insulation;第16卷(第5期);1455-1461 * |
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