CN111393572A - Recyclable antioxidant grafted polyolefin high-voltage direct-current cable insulating material and preparation method thereof - Google Patents
Recyclable antioxidant grafted polyolefin high-voltage direct-current cable insulating material and preparation method thereof Download PDFInfo
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- CN111393572A CN111393572A CN202010080822.0A CN202010080822A CN111393572A CN 111393572 A CN111393572 A CN 111393572A CN 202010080822 A CN202010080822 A CN 202010080822A CN 111393572 A CN111393572 A CN 111393572A
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- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
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Abstract
The invention discloses a recyclable antioxidant grafted polyolefin high-voltage direct-current cable insulating material and a preparation method thereof, and belongs to the technical field of high-voltage direct-current cable preparation. The invention solves the problems that the additive antioxidant in the existing polyolefin insulating material is gathered in an amorphous area in the polyolefin crystallization process to generate ionic space charge, and is easy to migrate and separate out and reduce the antioxidant effect in the production, storage and use processes of cables. The reactive antioxidant containing polar groups is added into thermoplastic polyolefin, is initiated by an initiator and is bonded to a polyolefin molecular chain through a melt grafting reaction, so that the micromolecular antioxidant is fixed on the polyolefin molecular chain, the space charge caused by the addition of the antioxidant is reduced, the trap energy level and the distribution characteristic in the material are regulated and controlled, and the accumulation of the space charge in the material is inhibited. Meanwhile, the thermoplastic polyolefin is used as a matrix material, and crosslinking is not needed, so that the thermoplastic polyolefin is a recyclable thermoplastic material.
Description
Technical Field
The invention relates to a recyclable antioxidant grafted polyolefin high-voltage direct-current cable insulating material and a preparation method thereof, and belongs to the technical field of high-voltage direct-current cable preparation.
Background
The polyolefin insulated direct current cable has a simple and firm structure, and is suitable for large-scale application to treatment of power transmission cable lines on the sea floor or road, however, under the action of a direct current electric field, the polyolefin insulating material can accumulate a large amount of space charges formed by injecting additives such as an antioxidant and the like into the polyolefin insulating material or ionizing impurities in the polyolefin insulating material, so that local electric field distortion in the insulating material is caused, particularly when the polarity of the direct current cable is reversed, the local field intensity is possibly 5-11 times higher than the average field intensity, and the electric conductivity, the breakdown performance, the aging performance and the like of the insulating material are obviously influenced, so that the long-term reliability and the service life of the direct current cable are influenced. A small amount of polar groups are introduced into the polyolefin insulating material, so that the trap density can be increased, the space charge distribution is uniform, and the direct current dielectric property is improved, however, a small molecular compound containing the polar groups is easy to migrate out, and a polar polymer has poor compatibility with polyolefin, so that the performance of the material is influenced.
The polyolefin cable insulation material is easy to age under the action of heat and oxygen in the production and use processes, the dielectric property, the mechanical property and the thermal stability of the polyolefin cable insulation material are influenced, and the service life of the cable is shortened. The antioxidant can delay the oxidative aging of the polymer and is an essential component of polyolefin cable insulation materials. The antioxidants used in the polyolefin cable insulation material mainly comprise antioxidants 300, 1076, 1035, 1010 and the like, however, the antioxidants belong to additive antioxidants, and the antioxidants containing polar groups are gathered in an amorphous area due to the action of polyolefin in the crystallization process, so that the antioxidants are important sources of ionic space charges in the material. And in the production, storage and use processes of the cable, the cable is easy to migrate, precipitate and lose, and meanwhile, the cable has poor compatibility with resin and low effective concentration, so that the antioxidant effect of the antioxidant is reduced. Therefore, it is necessary to provide an antioxidant grafted polyolefin high-voltage direct-current cable insulating material and a preparation method thereof.
Disclosure of Invention
The invention provides an antioxidant grafted polyolefin high-voltage direct-current cable insulating material and a preparation method thereof, aiming at solving the problems that an additive antioxidant in the existing polyolefin insulating material is gathered in an amorphous area in the polyolefin crystallization process, so that ionic space charges are generated in the material, the additive antioxidant is easy to migrate, precipitate and lose in the production, storage and use processes of a cable, and meanwhile, the additive is poor in compatibility with resin and low in effective concentration, so that the antioxidant effect of the antioxidant is reduced.
The technical scheme of the invention is as follows:
a recyclable antioxidant grafted polyolefin high-voltage direct-current cable insulating material is prepared from 100 parts by weight of thermoplastic polyolefin, 0.02-3 parts by weight of initiator and 0.01-10 parts by weight of reactive antioxidant; the reactive antioxidant has an ethylenically unsaturated substituent.
Further, the reactive antioxidant is N- (4-anilinophenyl) maleimide or N- (4-anilinophenyl) methacrylamide.
The insulating material is further limited to be prepared from 100 parts by weight of thermoplastic polyolefin, 0.02-3 parts by weight of initiator and 0.1-5 parts by weight of N- (4-anilinophenyl) maleimide.
The insulating material is further limited to be prepared from 100 parts by weight of thermoplastic polyolefin, 0.02-3 parts by weight of initiator and 0.1-7.5 parts by weight of N- (4-anilinophenyl) methacrylamide.
Further defined, the initiator is dicumyl peroxide, azobisisobutyronitrile, or benzoyl peroxide.
Further limiting, the insulating material is prepared from 100 parts by weight of thermoplastic polyolefin, 0.02-1.5 parts by weight of dicumyl peroxide and 0.01-10 parts by weight of reactive antioxidant;
the insulating material is prepared from 100 parts by weight of thermoplastic polyolefin, 0.15-2.5 parts by weight of azobisisobutyronitrile and 0.01-10 parts by weight of reactive antioxidant;
the insulating material is prepared from 100 parts by weight of thermoplastic polyolefin, 0.1-2 parts by weight of benzoyl peroxide and 0.01-10 parts by weight of reactive antioxidant.
Further defined, the thermoplastic polyolefin is polyethylene, polypropylene, or an ethylene propylene copolymer.
The preparation method of the insulating material comprises the following steps: melting thermoplastic polyolefin in an internal mixer, sequentially adding a reactive antioxidant and an initiator, and mixing for 10-30 min at the temperature of 100-200 ℃ and the rotating speed of 40-80 r/min to obtain the recyclable antioxidant grafted polyolefin high-voltage direct-current cable insulation material.
And further limiting, the mixing process comprises the specific steps of adding the reactive antioxidant, mixing for 2-8 min, adding the initiator, and continuously mixing for 1-15 min.
The invention has the following beneficial effects: the reactive antioxidant containing polar groups is added into thermoplastic polyolefin, is initiated by a free radical initiator and is bonded to a polyolefin molecular chain through a melt grafting reaction, so that the micromolecular antioxidant is fixed on the polyolefin molecular chain, and the space charge density caused by the addition of the additive antioxidant is reduced. In addition, the polar groups in the reactive antioxidant are uniformly distributed in the polyolefin, so that the trap energy level and distribution characteristics in the material can be regulated and controlled, and the aim of inhibiting the accumulation of space charges in the material under the action of a direct current electric field is fulfilled. Meanwhile, the antioxidant grafted on the polyolefin molecular chain is not easy to migrate, precipitate and lose, has better compatibility with resin, and can increase effective concentration, so that the insulating material has good thermal oxidation aging resistance. Therefore, the antioxidant grafted polyolefin high-voltage direct-current cable insulating material prepared by the method has better capacity of inhibiting space charge accumulation on the basis of good thermal oxygen aging resistance. In addition, the invention adopts thermoplastic polyolefin as a matrix material, and the antioxidant grafted polyolefin high-voltage direct-current cable insulation material does not need crosslinking in the preparation process, is a recyclable thermoplastic material, is an environment-friendly material, can be recycled, and is beneficial to environmental protection.
Drawings
FIG. 1 is a reaction scheme of the antioxidant-grafted polyolefin insulation prepared in example 1;
FIG. 2 is a space charge distribution plot of the neat polyolefin insulation made in comparative example 1;
FIG. 3 is a space charge distribution diagram of the antioxidant 300/polyolefin insulation prepared in comparative example 2;
FIG. 4 is a space charge distribution diagram of the antioxidant-grafted polyolefin insulation prepared in example 1;
FIG. 5 is a space charge distribution diagram of the antioxidant-grafted polyolefin insulation prepared in example 2;
FIG. 6 is a space charge distribution diagram of the antioxidant-grafted polyolefin insulation prepared in example 3.
Detailed Description
The experimental procedures used in the following examples are conventional unless otherwise specified. The materials, reagents, methods and apparatus used, unless otherwise specified, are conventional in the art and are commercially available to those skilled in the art.
Example 1:
adding 40g of polyethylene into an internal mixer, melting at 110 ℃, wherein the rotating speed is 50r/min, adding 0.12g N- (4-anilinophenyl) maleimide after melting, mixing for 5min at the same temperature and rotating speed, adding 0.08g of dicumyl peroxide, continuing mixing for 3min at the same temperature and rotating speed, and carrying out melt blending grafting to obtain the recyclable antioxidant grafted polyolefin high-voltage direct-current cable insulating material.
In the reaction process of the reactive antioxidant grafted polyolefin insulation material of the embodiment, as shown in fig. 1, dicumyl peroxide as an initiator is decomposed at a high temperature to generate a primary free radical, the primary free radical and a polyethylene molecular chain undergo a hydrogen elimination reaction to generate a polyethylene macromolecular chain free radical, then the macromolecular chain free radical and a reactive antioxidant N- (4-anilinophenyl) maleimide monomer undergo a grafting reaction to generate a graft free radical, the primary free radical can also react with the reactive antioxidant monomer to generate a monomer free radical, and finally the graft free radical can react with the monomer free radical and the primary free radical to generate a termination reaction to generate the antioxidant grafted polyolefin insulation material.
A DC field of-40 kV/mm was applied to a 300 μm thin film sample of the insulating material, the space charge density distribution of the sample was measured at intervals of 5s within 40min of pressurization as shown in a in FIG. 4, and then the short circuit was removed and the space charge density distribution of the sample was measured at intervals of 3s within 30min of short circuit as shown in b in FIG. 4. And the oxidation induction period of the insulation material was measured to be 90.4 min.
Example 2:
adding 40g of polyethylene into an internal mixer, melting at 120 ℃, wherein the rotating speed is 50r/min, adding 2g of N- (4-anilinophenyl) maleimide after melting, mixing for 5min at the same temperature and rotating speed, adding 1g of azodiisobutyronitrile, continuously mixing for 8min at the same temperature and rotating speed, and carrying out melt blending grafting to obtain the recyclable antioxidant grafted polyolefin high-voltage direct-current cable insulating material.
The reaction process of the reactive antioxidant grafted polyolefin insulating material of the embodiment is as follows: initiator azobisisobutyronitrile is decomposed at high temperature to generate primary free radical, the primary free radical and polyethylene molecular chain are subjected to hydrogen elimination reaction to generate polyethylene macromolecular chain free radical, and then the macromolecular chain free radical and reactive antioxidant N- (4-anilinophenyl) maleimide monomer are subjected to grafting reaction to generate graft free radical.
A DC field of-40 kV/mm was applied to a 300 μm thin film sample of the insulating material, the space charge density distribution of the sample was measured at intervals of 5s within 40min of pressurization as shown in a in FIG. 5, and then the short circuit was removed and the space charge density distribution of the sample was measured at intervals of 3s within 30min of short circuit as shown in b in FIG. 5. And the oxidation induction period of the insulation material was measured to be 80.7 min. As shown in FIG. 5, after the polyethylene is grafted with N- (4-anilinophenyl) maleimide, the space charge accumulation in the polyolefin is obviously inhibited, and the space charge accumulation in the sample is hardly obvious.
Example 3:
adding 40g of polypropylene into an internal mixer, melting at 180 ℃, wherein the rotating speed is 60r/min, adding 1.2g N- (4-anilinophenyl) methacrylamide after melting, mixing for 5min at the same temperature and rotating speed, adding 0.8g of benzoyl peroxide, continuing mixing for 10min at the same temperature and rotating speed, and carrying out melt blending grafting to obtain the recyclable antioxidant grafted polyolefin high-voltage direct-current cable insulating material.
The reaction process of the reactive antioxidant grafted polyolefin insulating material of the embodiment is as follows: the initiator benzoyl peroxide is decomposed at high temperature to generate primary free radicals, the primary free radicals and a polypropylene molecular chain are subjected to hydrogen elimination reaction to generate polypropylene macromolecular chain free radicals, and then the macromolecular chain free radicals and a reactive antioxidant N- (4-anilinophenyl) methacrylamide monomer are subjected to grafting reaction to generate graft free radicals.
A DC field of-40 kV/mm was applied to a 300 μm thin film sample of the insulating material, the space charge density distribution of the sample was measured at intervals of 5s within 40min of pressurization as shown in a in FIG. 6, and then the short circuit was removed and the space charge density distribution of the sample was measured at intervals of 3s within 30min of short circuit as shown in b in FIG. 6. And the oxidation induction period of the insulating material is measured to be greater than 180 min. As shown in FIG. 6, the polypropylene is grafted with N- (4-anilinophenyl) methacrylamide, so that the space charge accumulation in the polyolefin is obviously inhibited, and almost no space charge accumulation is obvious in the sample.
Example 4:
adding 40g of polyethylene into an internal mixer, melting at 100 ℃, wherein the rotating speed is 60r/min, adding 0.04g N- (4-anilinophenyl) maleimide after melting, mixing for 5min at the same temperature and rotating speed, adding 0.008g of dicumyl peroxide, continuously mixing for 10min at the same temperature and rotating speed, and carrying out melt blending grafting to obtain the recyclable antioxidant grafted polyolefin high-voltage direct-current cable insulating material. The oxidation induction period of the insulation material was measured for 87.2 min.
Example 5:
adding 40g of polyethylene into an internal mixer, melting at 110 ℃, wherein the rotating speed is 60r/min, adding 0.6g N- (4-anilinophenyl) methacrylamide after melting, mixing for 5min at the same temperature and rotating speed, adding 0.04g of benzoyl peroxide, continuously mixing for 12min at the same temperature and rotating speed, and carrying out melt blending grafting to obtain the recyclable antioxidant grafted polyolefin high-voltage direct-current cable insulating material. The oxidation induction period of the insulating material is measured to be more than 180 min.
Example 6:
adding 40g of polypropylene into an internal mixer, melting at 200 ℃, wherein the rotating speed is 70r/min, adding 0.8g N- (4-anilinophenyl) maleimide after melting, mixing for 5min at the same temperature and rotating speed, adding 0.4g of azodiisobutyronitrile, continuously mixing for 10min at the same temperature and rotating speed, and carrying out melt blending grafting to obtain the recyclable antioxidant grafted polyolefin high-voltage direct-current cable insulating material. The oxidation induction period of the insulation material was measured for 81.7 min.
Example 7:
adding 40g of ethylene propylene copolymer into an internal mixer, melting at 180 ℃, wherein the rotating speed is 60r/min, adding 0.04g N- (4-anilinophenyl) methacrylamide after melting, mixing for 5min at the same temperature and rotating speed, adding 0.06g of azodiisobutyronitrile, continuously mixing for 8min at the same temperature and rotating speed, and carrying out melt blending grafting to obtain the recyclable antioxidant grafted polyolefin high-voltage direct-current cable insulating material. The oxidation induction period of the insulation material was measured for 40.3 min.
Example 8:
adding 40g of ethylene propylene copolymer into an internal mixer, melting at 190 ℃, wherein the rotating speed is 50r/min, adding 3g of N- (4-anilinophenyl) methacrylamide after melting, mixing for 5min at the same temperature and rotating speed, adding 0.6g of dicumyl peroxide, continuing mixing for 3min at the same temperature and rotating speed, and carrying out melt blending grafting to obtain the recyclable antioxidant grafted polyolefin high-voltage direct-current cable insulating material. The oxidation induction period of the insulating material is measured to be more than 180 min.
Comparative example 1:
adding 40g of polyethylene into an internal mixer, melting at 110 ℃, wherein the rotating speed is 50r/min, adding 0.08g of dicumyl peroxide after melting, and mixing for 3min at the same temperature and rotating speed to obtain the pure polyolefin insulating material. A DC field of-40 kV/mm is applied to a film sample of 300 μm of the pure polyolefin insulation material, the space charge density distribution of the sample is measured at an interval of 5s within 40min of pressurization, as shown in a diagram in figure 2, then the short circuit is relieved, and the space charge density distribution of the sample is measured at an interval of 3s within 30min of short circuit, as shown in b diagram in figure 2. The oxidation induction period of the insulation material was measured for 3.07 min.
Comparative example 2:
adding 40g of polyethylene into an internal mixer, melting at 110 ℃, wherein the rotating speed is 50r/min, adding 0.12g of antioxidant 300 after melting, and mixing for 5min at the same temperature and rotating speed to obtain the antioxidant 300/polyolefin insulating material. A DC field of-40 kV/mm is applied to a film sample of 300 mu m of the antioxidant 300/polyolefin insulating material, the space charge density distribution of the sample is measured at intervals of 5s within 40min of pressurization, as shown in a diagram in figure 3, then the short circuit is relieved, and the space charge density distribution of the sample is measured at intervals of 3s within 30min of short circuit, as shown in b diagram in figure 3. The oxidation induction period of the insulation material was measured for 91.64 min.
The data are analyzed:
comparing the oxidation induction periods of the insulation materials prepared in examples 1 to 8 and comparative examples 1 and 2, it can be seen that the oxidation induction period of comparative example 1 is very small, and the oxidation induction periods of the insulation materials prepared in examples 1 and 2 are 90.4min and 91.64min, respectively, with a very small difference, which indicates that the oxidation induction period of the antioxidant grafted polyolefin high voltage direct current cable insulation material prepared in example 1 is significantly improved compared with that of pure polyolefin, and is equivalent to that of antioxidant 300/polyolefin insulation material, and indicates that the antioxidant grafted polyolefin high voltage direct current cable insulation material can maintain good thermal aging resistance and has recyclability without adding additional additives.
As shown in fig. 2, that is, the space charge distribution diagram of the pure polyolefin insulating material prepared in comparative example 1 shows, with the increase of the voltage application time, there are heteropolar space charges near the cathode and homopolar space charges injected near the anode, and there are a large number of positive and negative space charge packets in the sample, which causes serious space charge accumulation and seriously affects the dc dielectric performance of the insulating material. As shown in fig. 3, in comparative example 2, after the antioxidant 300 commonly used for polyolefin insulation materials of cables is added, a large amount of space charges with different polarities are accumulated near the cathode along with the increase of voltage application time, space charges with the same polarity are injected near the anode, and space charges also exist in the sample. As shown in fig. 4, namely the space charge distribution diagram of the antioxidant grafted polyolefin high voltage direct current cable insulation material prepared in example 1, it can be seen that the space charge accumulation in the polyolefin is obviously inhibited after the antioxidant is grafted. With the increase of the voltage application time, almost no obvious space charge accumulation exists in the sample, and the direct current insulation performance of the material is greatly improved. It can be seen that the antioxidant grafted polyolefin high voltage direct current cable insulation material obtained in the above embodiment of the present invention has very little space charge accumulation, and shows better space charge inhibition capability than the pure polyolefin insulation material in fig. 2, and it can be seen from fig. 3 that a large amount of space charge is accumulated in the antioxidant 300/polyolefin added with the antioxidant 300 commonly used for cable polyolefin insulation materials.
From the comprehensive performance, the antioxidant grafted polyolefin high-voltage direct-current cable insulating material meets the requirements of wire and cable insulating materials, has good space charge inhibition capability, and meanwhile, the antioxidant grafted on a polyolefin molecular chain is not easy to migrate and separate out, so that the insulating material has good thermal oxidation aging resistance.
Claims (9)
1. A recyclable antioxidant grafted polyolefin high-voltage direct-current cable insulating material is characterized by being prepared from 100 parts by weight of thermoplastic polyolefin, 0.02-3 parts by weight of initiator and 0.01-10 parts by weight of reactive antioxidant; the reactive antioxidant has an ethylenically unsaturated substituent.
2. The recyclable antioxidant grafted polyolefin high-voltage direct current cable insulation material as claimed in claim 1, wherein the reactive antioxidant is N- (4-anilinophenyl) maleimide or N- (4-anilinophenyl) methacrylamide.
3. The recyclable antioxidant grafted polyolefin high-voltage direct current cable insulation material as claimed in claim 2, characterized in that the insulation material is prepared from 100 parts by weight of thermoplastic polyolefin, 0.02-3 parts by weight of initiator and 0.1-5 parts by weight of N- (4-anilinophenyl) maleimide.
4. The recyclable antioxidant grafted polyolefin high-voltage direct current cable insulation material as claimed in claim 2, characterized in that the insulation material is prepared from 100 parts by weight of thermoplastic polyolefin, 0.02-3 parts by weight of initiator and 0.1-7.5 parts by weight of N- (4-anilinophenyl) methacrylamide.
5. The recyclable antioxidant grafted polyolefin high-voltage direct current cable insulation material as claimed in claim 1, wherein the initiator is dicumyl peroxide, azobisisobutyronitrile or benzoyl peroxide.
6. The recyclable antioxidant grafted polyolefin high-voltage direct current cable insulation material as claimed in claim 5, characterized in that the insulation material is prepared from 100 parts by weight of thermoplastic polyolefin, 0.02-1.5 parts by weight of dicumyl peroxide and 0.01-10 parts by weight of reactive antioxidant;
the insulating material is prepared from 100 parts by weight of thermoplastic polyolefin, 0.15-2.5 parts by weight of azobisisobutyronitrile and 0.01-10 parts by weight of reactive antioxidant;
the insulating material is prepared from 100 parts by weight of thermoplastic polyolefin, 0.1-2 parts by weight of benzoyl peroxide and 0.01-10 parts by weight of reactive antioxidant.
7. The recyclable antioxidant grafted polyolefin high voltage direct current cable insulation material as claimed in claim 1, wherein the thermoplastic polyolefin is polyethylene, polypropylene or ethylene propylene copolymer.
8. A method for preparing the recyclable antioxidant grafted polyolefin high voltage direct current cable insulation material as described in claim 1, characterized in that the method is performed by the following steps: melting thermoplastic polyolefin in an internal mixer, sequentially adding a reactive antioxidant and an initiator, and mixing for 10-30 min at the temperature of 100-200 ℃ and the rotating speed of 40-80 r/min to obtain the recyclable antioxidant grafted polyolefin high-voltage direct-current cable insulation material.
9. The preparation method of the recyclable antioxidant grafted polyolefin high-voltage direct current cable insulation material according to claim 8, characterized in that the mixing process comprises the steps of adding a reactive antioxidant, mixing for 2-8 min, adding an initiator, and continuously mixing for 1-15 min.
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