CN116003893B - Soft antifreezing anti-cracking polyolefin insulating material for cable and preparation method thereof - Google Patents
Soft antifreezing anti-cracking polyolefin insulating material for cable and preparation method thereof Download PDFInfo
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- CN116003893B CN116003893B CN202211716176.8A CN202211716176A CN116003893B CN 116003893 B CN116003893 B CN 116003893B CN 202211716176 A CN202211716176 A CN 202211716176A CN 116003893 B CN116003893 B CN 116003893B
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- 238000005336 cracking Methods 0.000 title claims abstract description 56
- 229920000098 polyolefin Polymers 0.000 title claims abstract description 34
- 239000011810 insulating material Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000007710 freezing Methods 0.000 claims abstract description 29
- 238000003756 stirring Methods 0.000 claims description 68
- 238000006243 chemical reaction Methods 0.000 claims description 55
- 239000007795 chemical reaction product Substances 0.000 claims description 36
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 32
- 238000001035 drying Methods 0.000 claims description 27
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 26
- 239000003795 chemical substances by application Substances 0.000 claims description 26
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 20
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 16
- NIHNNTQXNPWCJQ-UHFFFAOYSA-N fluorene Chemical compound C1=CC=C2CC3=CC=CC=C3C2=C1 NIHNNTQXNPWCJQ-UHFFFAOYSA-N 0.000 claims description 16
- 239000004611 light stabiliser Substances 0.000 claims description 16
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 238000001914 filtration Methods 0.000 claims description 15
- 238000001291 vacuum drying Methods 0.000 claims description 15
- RGHHSNMVTDWUBI-UHFFFAOYSA-N 4-hydroxybenzaldehyde Chemical compound OC1=CC=C(C=O)C=C1 RGHHSNMVTDWUBI-UHFFFAOYSA-N 0.000 claims description 14
- PCLIMKBDDGJMGD-UHFFFAOYSA-N N-bromosuccinimide Chemical compound BrN1C(=O)CCC1=O PCLIMKBDDGJMGD-UHFFFAOYSA-N 0.000 claims description 14
- OTBHHUPVCYLGQO-UHFFFAOYSA-N bis(3-aminopropyl)amine Chemical compound NCCCNCCCN OTBHHUPVCYLGQO-UHFFFAOYSA-N 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 13
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 12
- MZRVEZGGRBJDDB-UHFFFAOYSA-N N-Butyllithium Chemical compound [Li]CCCC MZRVEZGGRBJDDB-UHFFFAOYSA-N 0.000 claims description 12
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 12
- 239000012065 filter cake Substances 0.000 claims description 12
- 239000000706 filtrate Substances 0.000 claims description 12
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 12
- LPNYRYFBWFDTMA-UHFFFAOYSA-N potassium tert-butoxide Chemical compound [K+].CC(C)(C)[O-] LPNYRYFBWFDTMA-UHFFFAOYSA-N 0.000 claims description 12
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 12
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 12
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 11
- 238000001704 evaporation Methods 0.000 claims description 11
- 230000001376 precipitating effect Effects 0.000 claims description 11
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 10
- 239000003963 antioxidant agent Substances 0.000 claims description 10
- 230000003078 antioxidant effect Effects 0.000 claims description 10
- 239000004917 carbon fiber Substances 0.000 claims description 10
- 239000012153 distilled water Substances 0.000 claims description 10
- 229920001903 high density polyethylene Polymers 0.000 claims description 10
- 239000004700 high-density polyethylene Substances 0.000 claims description 10
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 10
- NFHFRUOZVGFOOS-UHFFFAOYSA-N palladium;triphenylphosphane Chemical compound [Pd].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 NFHFRUOZVGFOOS-UHFFFAOYSA-N 0.000 claims description 10
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 8
- 239000002270 dispersing agent Substances 0.000 claims description 8
- 239000000284 extract Substances 0.000 claims description 8
- 239000000377 silicon dioxide Substances 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- MNDIARAMWBIKFW-UHFFFAOYSA-N 1-bromohexane Chemical compound CCCCCCBr MNDIARAMWBIKFW-UHFFFAOYSA-N 0.000 claims description 7
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 7
- NHDIQVFFNDKAQU-UHFFFAOYSA-N tripropan-2-yl borate Chemical compound CC(C)OB(OC(C)C)OC(C)C NHDIQVFFNDKAQU-UHFFFAOYSA-N 0.000 claims description 7
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 6
- 239000008187 granular material Substances 0.000 claims description 6
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 6
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 6
- 238000003828 vacuum filtration Methods 0.000 claims description 6
- 239000011592 zinc chloride Substances 0.000 claims description 6
- 235000005074 zinc chloride Nutrition 0.000 claims description 6
- BCKVHOUUJMYIAN-UHFFFAOYSA-N 5-bromo-2-benzofuran-1,3-dione Chemical compound BrC1=CC=C2C(=O)OC(=O)C2=C1 BCKVHOUUJMYIAN-UHFFFAOYSA-N 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000001125 extrusion Methods 0.000 claims description 5
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 4
- 239000005457 ice water Substances 0.000 claims description 4
- 239000012074 organic phase Substances 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 239000008096 xylene Substances 0.000 claims description 4
- HCILJBJJZALOAL-UHFFFAOYSA-N 3-(3,5-ditert-butyl-4-hydroxyphenyl)-n'-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyl]propanehydrazide Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)NNC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 HCILJBJJZALOAL-UHFFFAOYSA-N 0.000 claims description 3
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 claims description 3
- 229940113115 polyethylene glycol 200 Drugs 0.000 claims description 3
- 229940068918 polyethylene glycol 400 Drugs 0.000 claims description 3
- 238000000967 suction filtration Methods 0.000 claims description 3
- 150000008064 anhydrides Chemical class 0.000 claims description 2
- 239000012774 insulation material Substances 0.000 claims 3
- 239000002244 precipitate Substances 0.000 claims 3
- 239000007788 liquid Substances 0.000 claims 1
- 230000008014 freezing Effects 0.000 abstract description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 18
- 238000010992 reflux Methods 0.000 description 15
- 239000002904 solvent Substances 0.000 description 12
- 229910052757 nitrogen Inorganic materials 0.000 description 9
- 230000005540 biological transmission Effects 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 5
- 238000002390 rotary evaporation Methods 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 230000002528 anti-freeze Effects 0.000 description 3
- 125000001246 bromo group Chemical group Br* 0.000 description 3
- 238000010534 nucleophilic substitution reaction Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 125000005619 boric acid group Chemical group 0.000 description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-L phthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC=C1C([O-])=O XNGIFLGASWRNHJ-UHFFFAOYSA-L 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 238000007792 addition Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A30/00—Adapting or protecting infrastructure or their operation
- Y02A30/14—Extreme weather resilient electric power supply systems, e.g. strengthening power lines or underground power cables
Landscapes
- Organic Insulating Materials (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to the field of power cables, in particular to a soft antifreezing anti-cracking polyolefin insulating material for a cable and a preparation method thereof, which are used for solving the problems that the existing power cable is poor in freezing resistance, the cable is likely to crack or even break, and large-area power failure and other disastrous accidents are caused; according to the preparation method, the anti-freezing and anti-cracking agent is added into the soft anti-freezing and anti-cracking polyolefin insulating material for the cable, so that the flexibility of the soft anti-freezing and anti-cracking polyolefin insulating material for the cable can be effectively improved, the toughness of the soft anti-freezing and anti-cracking polyolefin insulating material for the cable is greatly improved, the mechanical property is still kept good at low temperature, the low-temperature embrittlement temperature of the soft anti-freezing and anti-cracking polyolefin insulating material is reduced, the freezing resistance is good, and the occurrence rate of even breakage due to freezing cracking is reduced.
Description
Technical Field
The invention relates to the field of power cables, in particular to a soft antifreezing anti-cracking polyolefin insulating material for a cable and a preparation method thereof.
Background
The power cable is a cable for transmitting and distributing electric energy, and is commonly used for urban underground power grids, power station outgoing lines, power supply in industrial and mining enterprises and power transmission lines under sea water passing through the river. In the electric power line, the proportion of the cable is gradually increasing. Along with the rapid development of the economy in China, the energy demand is also continuously increased, and the requirements on the power transmission and distribution industry in China are higher. Power transmission, especially long distance transmission, cables remain the dominant mode of transmission, and thus the stability of the cable system will directly affect the transmission capacity and transmission efficiency.
Especially in high latitude areas with severe natural conditions, the weather resistance of the cable is important. In cold winter, icing is a widely distributed natural phenomenon, for example, rime is a beautiful natural landscape. However, for the power transmission line, severe ice coating can cause cable cracking and even breaking, and large-area power failure and other disastrous accidents can be caused.
How to improve the prior power cable has poor freezing resistance, possibly causes cracking and even breaking of the cable, and causes catastrophic accidents such as large-area power failure and the like is the key of the invention, so that a need exists to solve the problems of the soft anti-freezing and anti-cracking polyolefin insulating material for the cable and the preparation method thereof.
Disclosure of Invention
In order to overcome the technical problems, the invention aims to provide a soft antifreezing anti-cracking polyolefin insulating material for cables and a preparation method thereof: the soft anti-freezing and anti-cracking polyolefin insulating material for the cable is prepared by adding high-density polyethylene, an anti-freezing and anti-cracking agent, carbon fiber, silica micropowder, an antioxidant, a light stabilizer and a dispersing agent into a mixer, mixing to obtain a mixture, adding the mixture into an extruder, carrying out melt extrusion, granulating, and placing granules into a vacuum drying oven for drying, and solves the problems that the conventional power cable is poor in freezing resistance, the cable is cracked or even broken, and large-area power failure and other disastrous accidents are caused.
The aim of the invention can be achieved by the following technical scheme:
a preparation method of a soft antifreezing anti-cracking polyolefin insulating material for cables comprises the following steps:
step one: weighing 80-100 parts of high-density polyethylene, 12-36 parts of anti-freezing and anti-cracking agent, 8-16 parts of carbon fiber, 5-15 parts of silica micropowder, 1-3 parts of antioxidant, 1.5-3.5 parts of light stabilizer and 2-6 parts of dispersing agent according to parts by weight for standby;
step two: adding high-density polyethylene, an antifreezing and anticracking agent, carbon fiber, silica micropowder, an antioxidant, a light stabilizer and a dispersing agent into a mixer, and uniformly mixing to obtain a mixture;
step three: adding the mixture into a mixing mill, mixing 10-15min at 50-60 ℃, and then heating to 110-125 ℃ to continue mixing 25-35min to obtain a mixed material;
step four: adding the mixed material into an extruder, carrying out melt extrusion, granulating, placing the granules into a vacuum drying oven, and drying for 8-10h at the temperature of 70-75 ℃ to obtain the soft antifreezing anti-cracking polyolefin insulating material for the cable.
As a further scheme of the invention: the antioxidant is one of an antioxidant 168 and an antioxidant 1024, the light stabilizer is one of a light stabilizer TH-944 and a light stabilizer 770, and the dispersing agent is one of polyethylene glycol 200 and polyethylene glycol 400.
As a further scheme of the invention: the antifreezing and anticracking agent is prepared by the following steps:
step s1: adding 3,3' -diaminodipropylamine, 4-bromophthalic anhydride and dimethylbenzene into a three-neck flask provided with a stirrer, a thermometer, an air duct and a reflux condenser, introducing nitrogen for protection, stirring and reacting for 10-15h under the conditions of 130-135 ℃ and stirring speed of 400-500 r/min, cooling the reaction product to room temperature after the reaction is finished, and removing the solvent by rotary evaporation to obtain an intermediate 1;
the reaction principle is as follows:
step s2: adding p-hydroxybenzaldehyde, phenol and N, N-dimethylacetamide into a three-neck flask provided with a stirrer, a thermometer and a reflux condenser, stirring and reacting for 15-25 min under the conditions that the temperature is 45-50 ℃ and the stirring speed is 400-500 r/min, then adding anhydrous zinc chloride and p-toluenesulfonic acid, continuing stirring and reacting for 20-25h, adding a reaction product into dichloromethane after the reaction is finished, precipitating, vacuum filtering, washing a filter cake with distilled water for 2-3 times, and then placing in a vacuum drying box, and drying for 2-3h under the conditions that the temperature is 60-65 ℃ to obtain an intermediate 2;
the reaction principle is as follows:
step s3: adding the intermediate 1, the intermediate 2, anhydrous potassium carbonate, toluene and N-methyl pyrrolidone into a three-neck flask provided with a stirrer, a thermometer, an air duct and a reflux condenser, introducing nitrogen for protection, stirring and reacting for 1.5-2.5 hours under the conditions of 140-145 ℃ and stirring speed of 400-500 r/min, heating to 175-180 ℃ and continuously stirring and reacting for 5-7 hours, cooling the reaction product to room temperature after the reaction is finished, adding the reaction product into hydrochloric acid solution, precipitating, vacuum filtering, washing a filter cake with distilled water and absolute ethyl alcohol for 2-3 times in sequence, and then placing in a vacuum drying box, and drying for 3-4 hours under the conditions of 90-95 ℃ to obtain the intermediate 3;
the reaction principle is as follows:
step s4: adding fluorene and 1-bromohexane into a four-neck flask provided with a stirrer, a thermometer, an air duct, a reflux condenser and a constant pressure dropping funnel, introducing nitrogen for protection, dropwise adding a potassium tert-butoxide solution while stirring under the condition that the temperature is-5-0 ℃ and the stirring rate is 400-500 r/min, controlling the dropping rate to be 1-2 drops/s, continuing to stir for reaction for 10-15h after the dropping is finished, adding a reaction product into ice water after the reaction is finished, precipitating, performing vacuum suction filtration, placing a filter cake into a vacuum drying box, and drying for 5-6h under the condition that the temperature is 70-75 ℃ to obtain an intermediate 4;
the reaction principle is as follows:
step s5: adding the intermediate 4, chloroform and N-bromosuccinimide into a three-neck flask with a stirrer and a thermometer, stirring at 60-65 ℃ and stirring speed of 400-500 r/min for 3-4h, adding the reaction product into distilled water after the reaction is finished, standing for layering, drying an organic phase with anhydrous magnesium sulfate, vacuum filtering, and rotationally evaporating the filtrate to remove the solvent to obtain an intermediate 5;
the reaction principle is as follows:
step s6: adding the intermediate 5, tetrahydrofuran and n-butyllithium into a three-neck flask with a stirrer and a thermometer, stirring at the temperature of-70 ℃ and the stirring speed of 400-500 r/min for reacting for 1-2h, adding triisopropyl borate for continuously stirring for reacting for 5-10 min, heating to 25-30 ℃ for continuously stirring for reacting for 10-15h, cooling to 0-3 ℃ for continuously stirring for reacting for 1-2h, adding deionized water for continuously stirring for reacting for 10-15min, extracting the reaction product with anhydrous diethyl ether for 2-3 times after the reaction is finished, combining the extracts, drying with anhydrous magnesium sulfate, vacuum suction filtering, and rotationally evaporating the filtrate to remove the solvent to obtain the intermediate 6;
the reaction principle is as follows:
step s7: adding the intermediate 3, the intermediate 6, the tetra (triphenylphosphine) palladium, the sodium carbonate and the tetrahydrofuran into a three-neck flask provided with a stirrer, a thermometer and a reflux condenser, stirring and reacting for 2-3 hours under the condition that the temperature is 75-80 ℃ and the stirring speed is 400-500 r/min, cooling the reaction product to room temperature after the reaction is finished, extracting the reaction product with methylene dichloride for 2-3 times, combining the extracting solutions, drying with anhydrous magnesium sulfate, vacuum filtering, and rotationally evaporating the filtrate to remove the solvent to obtain the antifreezing and anticracking agent.
The reaction principle is as follows:
as a further scheme of the invention: the 3,3' -diaminodipropylamine, 4-bromophenic anhydride and xylene in step s1 were used in a ratio of 0.1mol:0.2mol:100-120 mL.
As a further scheme of the invention: the dosage ratio of the p-hydroxybenzaldehyde, phenol, anhydrous zinc chloride, p-toluenesulfonic acid and N, N-dimethylacetamide in step s2 was 0.1mol:0.35-0.4mol:1.3-1.5g:1.6-2.0g:120-150 mL.
As a further scheme of the invention: the ratio of the amounts of intermediate 1, intermediate 2, anhydrous potassium carbonate, toluene and N-methylpyrrolidone used in step s3 was 0.3mol:0.1mol:0.33-0.35mol:100-120mL:120-150mL, wherein the mass fraction of the hydrochloric acid solution is 12-15%.
As a further scheme of the invention: the fluorene, 1-bromohexane and potassium t-butoxide solution in step s4 were used in an amount ratio of 0.1mol:0.22-0.25mol:20-30mL of the potassium tert-butoxide solution is prepared from 1g of potassium tert-butoxide: 10-15mL of the solution formed by dissolving in tetrahydrofuran.
As a further scheme of the invention: the ratio of the amount of intermediate 4, chloroform and N-bromosuccinimide in step s5 was 0.1mol:80-100mL:0.1 mol.
As a further scheme of the invention: the dosage ratio of the intermediate 5, tetrahydrofuran, n-butyllithium, triisopropyl borate, hydrochloric acid solution and deionized water in the step s6 is 0.1mol:120-150mL:0.11-0.13mol:0.13-0.15mol:180-200mL:200-300mL, wherein the molar concentration of the hydrochloric acid solution is 2.0-2.5 mol/L.
As a further scheme of the invention: the ratio of the amounts of intermediate 3, intermediate 6, tetrakis (triphenylphosphine) palladium, sodium carbonate and tetrahydrofuran used in step s7 was 10mmol:33-36mmol:0.15-0.25g:30-33mol:60-80mL.
As a further scheme of the invention: the soft anti-freezing and anti-cracking polyolefin insulating material for the cable is prepared according to the preparation method of the soft anti-freezing and anti-cracking polyolefin insulating material for the cable.
The invention has the beneficial effects that:
the invention relates to a soft anti-freezing and anti-cracking polyolefin insulating material for a cable and a preparation method thereof, wherein high-density polyethylene, an anti-freezing and anti-cracking agent, carbon fiber, silicon micropowder, an antioxidant, a light stabilizer and a dispersing agent are added into a mixer to be uniformly mixed to obtain a mixture, the mixture is added into a mixer to be mixed to obtain a mixed material, the mixed material is added into an extruder to be melt extruded, and the mixture is granulated, and the granules are placed into a vacuum drying oven to be dried to obtain the soft anti-freezing and anti-cracking polyolefin insulating material for the cable; according to the preparation method, the anti-freezing and anti-cracking agent is added into the soft anti-freezing and anti-cracking polyolefin insulating material for the cable, so that the flexibility of the soft anti-freezing and anti-cracking polyolefin insulating material for the cable can be effectively improved, the toughness of the soft anti-freezing and anti-cracking polyolefin insulating material for the cable is greatly improved, the mechanical property is still kept good at low temperature, the low-temperature embrittlement temperature of the material is reduced, the freezing resistance is good, and the occurrence rate of frozen cracking and even fracture is reduced;
firstly, utilizing amino on 3,3' -diaminodipropylamine and bromine atoms on 4-bromophthalic anhydride to generate nucleophilic substitution reaction to obtain an intermediate 1, then reacting p-hydroxybenzaldehyde and phenol to generate an intermediate 2, then reacting hydroxyl on the intermediate 2 and bromine atoms on the intermediate 1 to generate nucleophilic substitution reaction to obtain an intermediate 3, utilizing fluorene and 1-bromohexane to react, introducing long carbon chains into fluorene to obtain an intermediate 4, utilizing N-bromosuccinimide to brominate the intermediate 4 to obtain an intermediate 5, then reacting the intermediate 5 with triisopropyl borate to introduce boric acid groups to obtain an intermediate 6, and then reacting bromine atoms on the intermediate 3 and boric acid groups on the intermediate 6 to generate nucleophilic substitution reaction to obtain the anti-cracking agent; the antifreezing and anti-cracking agent takes three benzene rings as a framework to form a hyperbranched structure, the hyperbranched structure is difficult to crystallize, no winding exists among chains, and the free volume of molecules is large, so that the antifreezing and anti-cracking agent still has good movement capability in an ultralow temperature environment, and a large number of introduced long carbon chains have good flexibility, so that the toughness of the antifreezing and anti-cracking agent is improved, and the toughness of the soft antifreezing and anti-cracking polyolefin insulating material of the cable is further improved, so that the prepared soft antifreezing and anti-cracking polyolefin insulating material of the cable has good low temperature resistance, freezing resistance and anti-cracking, and can effectively protect the cable.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1:
the embodiment is a preparation method of an antifreezing and anti-cracking agent, which comprises the following steps:
step s1: adding 0.1 mL of 3,3' -diaminodipropylamine, 0.2 mL of 4-bromophthalic anhydride and 100mL of xylene into a three-neck flask provided with a stirrer, a thermometer, an air duct and a reflux condenser, introducing nitrogen for protection, stirring and reacting for 10 hours under the condition that the temperature is 130 ℃ and the stirring rate is 400 r/min, cooling the reaction product to room temperature after the reaction is finished, and removing the solvent by rotary evaporation to obtain an intermediate 1;
step s2: adding 0.1mol of p-hydroxybenzaldehyde, 0.35mol of phenol and 120mLN, N-dimethylacetamide into a three-neck flask provided with a stirrer, a thermometer and a reflux condenser, stirring at a temperature of 45 ℃ and a stirring rate of 400 r/min for reaction for 15min, adding 1.3g of anhydrous zinc chloride and 1.6g of p-toluenesulfonic acid, continuing stirring for reaction for 20h, adding the reaction product into dichloromethane after the reaction is finished, precipitating, vacuum filtering, washing a filter cake with distilled water for 2 times, and then placing in a vacuum drying oven, and drying at a temperature of 60 ℃ for 2h to obtain an intermediate 2;
step s3: adding 0.3mol of intermediate 1, 0.1mol of intermediate 2, 0.33 mol of anhydrous potassium carbonate, 100mL of toluene and 120 mLN-methylpyrrolidone into a three-neck flask provided with a stirrer, a thermometer, an air duct and a reflux condenser, introducing nitrogen for protection, stirring at the temperature of 140 ℃ and the stirring rate of 400 r/min for reaction for 1.5 hours, heating to 175 ℃ for continuous stirring for reaction for 5 hours, cooling the reaction product to room temperature after the reaction is finished, adding the reaction product into a hydrochloric acid solution with the mass fraction of 12%, precipitating and precipitating, vacuum-filtering, washing a filter cake with distilled water and absolute ethyl alcohol for 2 times in sequence, and then placing in a vacuum drying box for drying for 3 hours at the temperature of 90 ℃ to obtain an intermediate 3;
step s4: 0.1mol of fluorene and 0.22 mol of 1-bromohexane are added into a four-neck flask provided with a stirrer, a thermometer, an air duct, a reflux condenser and a constant pressure dropping funnel, nitrogen is introduced for protection, and 20mL of potassium tert-butoxide is added dropwise while stirring under the conditions that the temperature is minus 5 ℃ and the stirring rate is 400 r/min according to 1g:10mL of potassium tert-butoxide solution formed by dissolving tetrahydrofuran is controlled to have the dropping speed of 1 drop/s, stirring is continued to react for 10h after the dropping is finished, a reaction product is added into ice water after the reaction is finished, precipitation is separated out, vacuum filtration is carried out, a filter cake is placed in a vacuum drying box, and drying is carried out for 5-6h under the condition that the temperature is 70 ℃ to obtain an intermediate 4;
step s5: adding 0.1mol of intermediate 4, 80mL of chloroform and 0.1mol of N-bromosuccinimide into a three-neck flask with a stirrer and a thermometer, stirring at a temperature of 60 ℃ and a stirring rate of 400 r/min for 3 hours, adding a reaction product into distilled water after the reaction is finished, standing for layering, drying an organic phase with anhydrous magnesium sulfate, vacuum filtering, and rotationally evaporating a filtrate to remove a solvent to obtain an intermediate 5;
step s6: adding 0.1mol of intermediate 5, 120mL of tetrahydrofuran and 0.11 mol of n-butyllithium into a three-neck flask provided with a stirrer and a thermometer, stirring and reacting for 1h under the condition that the temperature is-70 ℃ and the stirring rate is 400 r/min, adding 0.13mol of triisopropyl borate, continuing to stir and react for 5min, heating to 25 ℃ and continuing to stir and react for 10h, cooling to 0 ℃, adding 180-200mL of hydrochloric acid solution with the molar concentration of 2.0 mol/L and continuing to stir and react for 1h, adding 200mL of deionized water, continuing to stir and react for 10 min, extracting a reaction product with dehydrated diethyl ether for 2 times after the reaction is finished, combining the extracts, drying with anhydrous magnesium sulfate, vacuum filtering, and rotationally evaporating the filtrate to remove the solvent to obtain an intermediate 6;
step s7: 10mmol of intermediate 3, 33 mmol of intermediate 6, 0.15g of tetrakis (triphenylphosphine) palladium, 30 mole of sodium carbonate and 60mL of tetrahydrofuran are added to a three-necked flask equipped with a stirrer, a thermometer and a reflux condenser, and the reaction is stirred at a temperature of 75 ℃ and a stirring rate of 400 r/min for 2 hours, the reaction product is cooled to room temperature after the completion of the reaction, the reaction product is extracted with methylene chloride for 2 times, the extracts are combined and dried with anhydrous magnesium sulfate, and then vacuum filtration is performed, and the filtrate is subjected to rotary evaporation to remove the solvent, thereby obtaining the antifreeze cracking inhibitor.
Example 2:
the embodiment is a preparation method of an antifreezing and anti-cracking agent, which comprises the following steps:
step s1: adding 0.1 mL of 3,3' -diaminodipropylamine, 0.2 mL of 4-bromophthalic anhydride and 120mL of xylene into a three-neck flask provided with a stirrer, a thermometer, an air duct and a reflux condenser, introducing nitrogen for protection, stirring and reacting for 15h under the condition that the temperature is 135 ℃ and the stirring speed is 500 r/min, cooling the reaction product to room temperature after the reaction is finished, and removing the solvent by rotary evaporation to obtain an intermediate 1;
step s2: adding 0.1mol of p-hydroxybenzaldehyde, 0.4mol of phenol and 150mLN, N-dimethylacetamide into a three-neck flask provided with a stirrer, a thermometer and a reflux condenser, stirring at a temperature of 50 ℃ and a stirring rate of 500 r/min for reaction for 25 min, adding 1.5g of anhydrous zinc chloride and 2.0g of p-toluenesulfonic acid, continuing stirring for reaction for 25h, adding the reaction product into dichloromethane after the reaction is finished, precipitating, vacuum filtering, washing a filter cake with distilled water for 3 times, and then placing in a vacuum drying oven, and drying for 3h at a temperature of 65 ℃ to obtain an intermediate 2;
step s3: adding 0.3mol of intermediate 1, 0.1mol of intermediate 2, 0.35mol of anhydrous potassium carbonate, 120mL of toluene and 150 mLN-methylpyrrolidone into a three-neck flask provided with a stirrer, a thermometer, an air duct and a reflux condenser, introducing nitrogen for protection, stirring at 145 ℃ and a stirring rate of 500 r/min for 2.5h, heating to 180 ℃ for reaction for 7h, cooling the reaction product to room temperature after the reaction, adding the reaction product into 15% hydrochloric acid solution by mass fraction, precipitating and filtering in vacuum, washing a filter cake with distilled water and absolute ethyl alcohol for 3 times in sequence, and then placing in a vacuum drying box for drying at 95 ℃ for 4h to obtain an intermediate 3;
step s4: 0.1mol of fluorene and 0.25mol of 1-bromohexane are added into a four-neck flask provided with a stirrer, a thermometer, an air duct, a reflux condenser and a constant pressure dropping funnel, nitrogen is introduced for protection, 30mL of potassium tert-butoxide is added dropwise while stirring under the condition that the temperature is 0 ℃ and the stirring rate is 500 r/min according to 1g:15mL of potassium tert-butoxide solution formed by dissolving tetrahydrofuran is controlled to have the dropping speed of 2 drops/s, stirring is continued for reaction for 15h after the dropping is finished, a reaction product is added into ice water after the reaction is finished, precipitation is separated out, vacuum filtration is carried out, a filter cake is placed in a vacuum drying box, and drying is carried out for 6h under the condition that the temperature is 75 ℃ to obtain an intermediate 4;
step s5: adding 0.1mol of intermediate 4, 100mL of chloroform and 0.1mol of N-bromosuccinimide into a three-neck flask with a stirrer and a thermometer, stirring and reacting for 4 hours under the condition that the temperature is 65 ℃ and the stirring rate is 500 r/min, adding a reaction product into distilled water after the reaction is finished, standing for layering, drying an organic phase with anhydrous magnesium sulfate, vacuum filtering, and rotationally evaporating a filtrate to remove a solvent to obtain an intermediate 5;
step s6: adding 0.1mol of intermediate 5, 150mL of tetrahydrofuran and 0.13mol of n-butyllithium into a three-neck flask with a stirrer and a thermometer, stirring at the temperature of-70 ℃ and the stirring rate of 500 r/min for 2h, adding 0.15mol of triisopropyl borate, continuing stirring for 10 min, heating to 30 ℃ for 15h, cooling to 3 ℃ for 2h, adding 200mL of hydrochloric acid solution with the molar concentration of 2.5mol/L, continuing stirring for 15min, extracting the reaction product with dehydrated diethyl ether for 3 times after the reaction, combining the extracts, drying with anhydrous magnesium sulfate, vacuum filtering, and rotationally evaporating the filtrate to remove the solvent to obtain intermediate 6;
step s7: 10mmol of intermediate 3, 36mmol of intermediate 6, 0.25g of tetrakis (triphenylphosphine) palladium, 33 mole of sodium carbonate and 80mL of tetrahydrofuran are added to a three-necked flask equipped with a stirrer, a thermometer and a reflux condenser, and the reaction is stirred at 80℃for 3 hours at a stirring rate of 500 r/min, the reaction product is cooled to room temperature after the completion of the reaction, the reaction product is extracted 3 times with methylene chloride, the extracts are combined and dried over anhydrous magnesium sulfate, followed by vacuum filtration, and the solvent is removed by rotary evaporation of the filtrate to obtain an antifreezing anti-cracking agent.
Example 3:
the embodiment is a preparation method of a soft antifreezing and anti-cracking polyolefin insulating material for cables, which comprises the following steps:
step one: weighing 80 parts of high-density polyethylene, 12 parts of an antifreezing and cracking agent from example 1, 8 parts of carbon fiber, 5 parts of silica powder, 168 1 parts of an antioxidant, 1.5 parts of a light stabilizer TH-944 and 200 parts of polyethylene glycol according to parts by weight for later use;
step two: adding high-density polyethylene, an antifreezing and anticracking agent, carbon fiber, silica micropowder, an antioxidant 168, a light stabilizer TH-944 and polyethylene glycol 200 into a mixer, and uniformly mixing to obtain a mixture;
step three: adding the mixture into a mixing mill, mixing for 10 min at 50 ℃, and then continuously mixing for 25 min at 110 ℃ to obtain a mixed material;
step four: adding the mixed material into an extruder, carrying out melt extrusion, granulating, placing the granules into a vacuum drying oven, and drying for 8 hours at the temperature of 70 ℃ to obtain the soft antifreezing anti-cracking polyolefin insulating material for the cable.
Example 4:
the embodiment is a preparation method of a soft antifreezing and anti-cracking polyolefin insulating material for cables, which comprises the following steps:
step one: weighing 100 parts of high-density polyethylene, 36 parts of an antifreezing and cracking agent from example 2, 16 parts of carbon fiber, 15 parts of silica micropowder, 1024 3 parts of antioxidant, 3.5 parts of light stabilizer 770 and 400 parts of polyethylene glycol according to parts by weight for later use;
step two: adding high-density polyethylene, an antifreezing and anticracking agent, carbon fiber, silicon micropowder, an antioxidant 1024, a light stabilizer 770 and polyethylene glycol 400 into a mixer, and uniformly mixing to obtain a mixture;
step three: adding the mixture into a mixing mill, mixing 15min under the condition of 60 ℃, and then continuously mixing 35min under the condition of heating to 125 ℃ to obtain a mixed material;
step four: adding the mixed material into an extruder, carrying out melt extrusion, granulating, placing the granules into a vacuum drying oven, and drying for 10 hours at the temperature of 75 ℃ to obtain the soft antifreezing anti-cracking polyolefin insulating material for the cable.
Comparative example 1:
comparative example 1 is different from example 4 in that no antifreeze cracking agent is added.
Comparative example 2:
comparative example 2 is different from example 4 in that phthalate is added instead of the antifreeze cracking agent.
The properties of the soft freeze-proof and crack-resistant polyolefin insulating materials for cables of examples 3 to 4 and comparative examples 1 to 2 were examined, and the results are shown in the following table:
referring to the data in the table, according to the comparison between the examples 3-4 and the comparative examples 1-2, it can be known that the mechanical property and the low-temperature embrittlement resistance of the soft anti-freezing and anti-cracking polyolefin insulating material for cables can be improved by adding the anti-freezing and anti-cracking agent and the phthalate, and the anti-freezing and anti-cracking agent has better effect.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is merely illustrative and explanatory of the invention, as various modifications and additions may be made to the particular embodiments described, or in a similar manner, by those skilled in the art, without departing from the scope of the invention or exceeding the scope of the invention as defined in the claims.
Claims (3)
1. The preparation method of the soft antifreezing anti-cracking polyolefin insulating material for the cable is characterized by comprising the following steps of:
step one: weighing 80-100 parts of high-density polyethylene, 12-36 parts of anti-freezing and anti-cracking agent, 8-16 parts of carbon fiber, 5-15 parts of silica micropowder, 1-3 parts of antioxidant, 1.5-3.5 parts of light stabilizer and 2-6 parts of dispersing agent according to parts by weight for standby;
step two: adding high-density polyethylene, an antifreezing and anticracking agent, carbon fiber, silica micropowder, an antioxidant, a light stabilizer and a dispersing agent into a mixer, and uniformly mixing to obtain a mixture;
step three: adding the mixture into a mixing mill, mixing for 10-15min at 50-60 ℃, and then continuously mixing for 25-35min at the temperature of 110-125 ℃ to obtain a mixed material;
step four: adding the mixed material into an extruder, carrying out melt extrusion, granulating, placing the granules into a vacuum drying oven, and drying for 8-10h at the temperature of 70-75 ℃ to obtain the soft antifreezing anti-cracking polyolefin insulating material for the cable;
the antifreezing and anticracking agent is prepared by the following steps:
step s1: adding 3,3' -diaminodipropylamine, 4-bromophthalic anhydride and dimethylbenzene into a three-neck flask, stirring for reaction, cooling a reaction product to room temperature after the reaction is finished, and then rotationally evaporating to obtain an intermediate 1;
the 3,3' -diaminodipropylamine, 4-bromophenic anhydride and xylene in step s1 were used in an amount ratio of 0.1mol:0.2mol:100-120mL;
step s2: adding p-hydroxybenzaldehyde, phenol and N, N-dimethylacetamide into a three-neck flask for stirring reaction, then adding anhydrous zinc chloride and p-toluenesulfonic acid for continuous stirring reaction, adding a reaction product into dichloromethane after the reaction is finished, precipitating a precipitate, then carrying out vacuum suction filtration, washing and drying a filter cake to obtain an intermediate 2; the dosage ratio of the p-hydroxybenzaldehyde, phenol, anhydrous zinc chloride, p-toluenesulfonic acid and N, N-dimethylacetamide in the step s2 is 0.1mol:0.35-0.4mol:1.3-1.5g:1.6-2.0g:120-150mL;
step s3: adding the intermediate 1, the intermediate 2, anhydrous potassium carbonate, toluene and N-methyl pyrrolidone into a three-neck flask, stirring for reaction, cooling a reaction product to room temperature after the reaction is finished, adding the reaction product into a hydrochloric acid solution, precipitating a precipitate, performing vacuum filtration, washing a filter cake, and drying to obtain an intermediate 3; the dosage ratio of the intermediate 1, the intermediate 2, the anhydrous potassium carbonate, toluene and the N-methylpyrrolidone in the step s3 is 0.3mol:0.1mol:0.33 to 0.35mol:100-120mL:120-150mL, wherein the mass fraction of the hydrochloric acid solution is 12-15%;
step s4: adding fluorene and 1-bromohexane into a four-neck flask, dropwise adding a potassium tert-butoxide solution while stirring, continuing stirring for reaction after the dropwise adding is finished, adding a reaction product into ice water after the reaction is finished, precipitating a precipitate, then carrying out vacuum suction filtration, and drying a filter cake to obtain an intermediate 4; the dosage ratio of fluorene, 1-bromohexane and potassium tert-butoxide solution in step s4 was 0.1mol:0.22 to 0.25mol:20-30mL of the potassium tert-butoxide solution is prepared from 1g of potassium tert-butoxide: 10-15mL of the solution formed by dissolving the solution in tetrahydrofuran;
step s5: adding the intermediate 4, chloroform and N-bromosuccinimide into a three-neck flask, stirring for reaction, adding a reaction product into distilled water after the reaction is finished, standing for layering, drying an organic phase, vacuum filtering, and rotationally evaporating filtrate to obtain an intermediate 5; the ratio of the amount of the intermediate 4, chloroform and N-bromosuccinimide in step s5 was 0.1mol:80-100mL:0.1mol;
step s6: adding the intermediate 5, tetrahydrofuran and n-butyllithium into a three-neck flask, stirring for reaction, sequentially adding triisopropyl borate, hydrochloric acid solution and deionized water, continuously stirring for reaction, extracting a reaction product after the reaction is finished, combining extract liquid, drying with anhydrous magnesium sulfate, vacuum filtering, and rotationally evaporating filtrate to obtain an intermediate 6; the dosage ratio of the intermediate 5, tetrahydrofuran, n-butyllithium, triisopropyl borate, hydrochloric acid solution and deionized water in the step s6 is 0.1mol:120-150mL:0.11-0.13mol:0.13 to 0.15mol:180-200mL:200-300mL, wherein the molar concentration of the hydrochloric acid solution is 2.0-2.5mol/L;
step s7: adding the intermediate 3, the intermediate 6, the tetra (triphenylphosphine) palladium, sodium carbonate and tetrahydrofuran into a three-neck flask, stirring for reaction, cooling a reaction product to room temperature after the reaction is finished, extracting the reaction product, combining the extracts, drying the extracts with anhydrous magnesium sulfate, performing vacuum filtration, and rotationally evaporating filtrate to obtain the antifreezing anti-cracking agent; the ratio of the amounts of intermediate 3, intermediate 6, tetrakis (triphenylphosphine) palladium, sodium carbonate and tetrahydrofuran in step s7 was 10mmol:33-36mmol:0.15-0.25g:30-33mol:60-80mL.
2. The preparation method of the soft antifreezing and anti-cracking polyolefin insulating material for the cable according to claim 1, wherein the antioxidant is one of an antioxidant 168 and an antioxidant 1024, the light stabilizer is one of a light stabilizer TH-944 and a light stabilizer 770, and the dispersing agent is one of polyethylene glycol 200 and polyethylene glycol 400.
3. A soft freeze-proof and crack-resistant polyolefin insulation material for cables, characterized in that the soft freeze-proof and crack-resistant polyolefin insulation material for cables is prepared according to the preparation method of the soft freeze-proof and crack-resistant polyolefin insulation material for cables according to any one of claims 1-2.
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| CN111978617A (en) * | 2020-08-31 | 2020-11-24 | 方伟 | Cross-linked polyethylene insulated cold-resistant power cable |
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