Anti-bird packing material for cross arm and preparation method of anti-bird packing material

Abstract

The invention discloses a cross arm anti-bird packing material and a preparation method thereof, and belongs to the technical field of packing material preparation. The anti-bird packing material for the cross arm is prepared from the following components in parts by weight: 50-60 parts of ethylene propylene diene monomer, 1-2 parts of an anti-aging agent, 2-4 parts of an accelerant, 0.8-1.2 parts of a cross-linking agent, 3-6 parts of silicon filler, 5-8 parts of a modified antioxidant, 1-3 parts of an adhesive, 6-8 parts of pigment and 0.8-1.4 parts of a vulcanizing agent, the silicon filler is prepared from p-bromoethylbenzene, chloromethyl dimethyl chlorosilane, sodium azide, diethyl ether and lithium aluminum hydride, and the modified antioxidant is prepared from 2-chloro-4-nitrophenol, m-fluorobenzyl bromide, iron powder, abietic acid, oxalyl chloride and triethylamine. The packaging material prepared by the method has excellent durability, bird resistance and flame retardance.

Description

Technical Field

[0001] The invention belongs to the technical field of packaging material preparation, and in particular relates to a cross-arm bird-proof packaging material and a preparation method thereof. Background Art

[0002] As an angle iron structure fixed laterally on the top of a utility pole, the crossarm is used to support overhead wires and ensure the stability and safety of power transmission. However, in actual operation, crossarms often become the preferred location for birds to build nests. When birds build nests on crossarms, they not only use a variety of materials that are not necessarily insulators, but also the volume of the bird's nest or the arrangement of multiple bird nests may fill the space between two adjacent insulators, causing a short circuit accident between the lines, posing a serious safety hazard to the operation of the transmission line.

[0003] The impact of birds' nesting behavior on crossarms is not limited to physical contact. When choosing a nesting site, birds will frequently walk and peck on the surface of the crossarms, which will damage the anti-oxidation coating on the surface of the crossarms and affect the service life of the crossarms. In addition, when birds excrete feces near the crossarms, the bird droppings may form a conductive channel, causing the air gap of the pole to break down, causing the overhead transmission line to trip. The bodies of flying birds may also break down the air of the overhead transmission line, causing a trip accident, which in turn seriously threatens the stable operation of the power system.

[0004] Patent CN 111635633 B discloses a highly stable self-curing insulating protective packaging material and a preparation method thereof, which is composed of 50-80 parts by weight of methyl silicone rubber, 10-15 parts of polycarbomethylsilane, 5-10 parts of filler, 5-10 parts of cross-linking agent, 0.3-5 parts of end-capping agent, 0.5-3 parts of catalyst, 3-6 parts of fumed silica, 0.5-5 parts of light stabilizer and 10-20 parts of flame retardant. The filler is a mixture of silica powder and tourmaline powder. The prepared packaging material has the advantages of good weather resistance and durability in high humidity and high temperature environment. However, the bird-proof performance, durability and flame retardancy of the packaging material prepared by this method still have room for improvement. Summary of the invention

[0005] The object of the present invention is to provide a cross-arm bird-proof packaging material and a preparation method thereof, so as to solve the technical problems of poor bird-proof performance, durability and flame retardancy of packaging materials in the prior art.

[0006] In order to achieve the above object, the present invention adopts the following technical solutions:

[0007] The invention provides a cross-arm bird-proofing packaging material, which is composed of the following components in parts by weight: 50-60 parts of ethylene propylene rubber, 1-2 parts of an antioxidant, 2-4 parts of an accelerator, 0.8-1.2 parts of a crosslinking agent, 3-6 parts of a silicon filler, 5-8 parts of a modified antioxidant, 1-3 parts of an adhesive, 6-8 parts of a pigment, and 0.8-1.4 parts of a vulcanizing agent, wherein the silicon filler is prepared from 4-bromoethylbenzene, chloromethyldimethylchlorosilane, sodium azide, ether, lithium aluminum hydride and benzoic acid, and the modified antioxidant is prepared from 2-chloro-4-nitrophenol, m-fluorobenzyl bromide, iron powder, rosin acid, oxalyl chloride and triethylamine.

[0008] Preferably, the method for preparing the silicon filler comprises the following steps:

[0009] Q1: Add magnesium chips to a container filled with nitrogen, then add tetrahydrofuran, 4-bromoethylbenzene and iodine particles in sequence, heat for reaction, then heat for reflux reaction, and after the reaction is completed, obtain intermediate 1; slowly add chloromethyldimethylsilyl chloride to tetrahydrofuran under a nitrogen atmosphere and cool to obtain a silane solution, add the silane solution dropwise to the container containing intermediate 1 using a syringe, heat and stir for reaction, cool, quench the reaction, extract, dry, concentrate under reduced pressure, and purify to obtain intermediate 2;

[0010] Q2: Sodium azide is added to a container containing intermediate 2, and after stirring and mixing at room temperature, the mixture is poured into distilled water, extracted, washed, dried, and concentrated under reduced pressure to obtain intermediate 3; ether is added to a container containing intermediate 3, and then lithium aluminum hydride is added dropwise to the container, stirred in an ice bath, stirred at room temperature, the reaction is quenched, filtered, dried, evaporated under reduced pressure, and purified to obtain intermediate 4;

[0011] Q3: In an ice bath environment, benzoic acid is added to dichloromethane, and then 1-hydroxybenzotriazole and 1-ethyl-(3-dimethylaminopropyl)carbodiimide hydrochloride are added in sequence. After stirring for reaction, intermediate 4 is added, the temperature is raised and stirred, and after the reaction is completed, a silicon filler is obtained.

[0012] In the above process, the synthesis reaction formula of silicon filler is as follows:

[0013]

[0014] The results of mass spectrometry analysis of intermediate 1 were: m / z: 209.97 (100.0%), 207.97 (89.9%), 211.97 (12.2%), 210.97 (12.2%), 208.97 (11.4%), 208.98 (7.9%), 210.98 (7.7%), 211.98 (1.3%), 209.98 (1.3%), 212.97 (1.1%); the results of mass spectrometry analysis of intermediate 2 were: m / z: 212.08 (100.0%), 214.08 (35.9%), 213.08 (17.0%), 215.08 ( 5.9%), 216.07 (1.1%); the results of mass spectrometry analysis of intermediate 3 were: m / z: 219.12 (100.0%), 220.12 (18.1%), 221.12 (4.1%); the results of mass spectrometry analysis of intermediate 4 were: m / z: 193.13 (100.0%), 194.13 (17.6%), 195.13 (4.0%); the results of mass spectrometry analysis of silica filler were: m / z: 297.15 (100.0%), 298.16 (19.8%), 298.15 (5.4%), 299.15 (3.4%), 299.16 (3.1%).

[0015] Preferably, in Q1, the amount ratio of magnesium chips, tetrahydrofuran, p-bromoethylbenzene and iodine particles is (3.12-5.27) g: (8-12) mL: (8.34-9.23) mL: (0.12-0.18) g, the heating reaction temperature is 55-65°C, the reaction time is 30-45 min, the temperature of the reflux reaction is 70-75°C, and the reflux time is 3-4 h; the amount ratio of chloromethyldimethylsilyl chloride, tetrahydrofuran and intermediate 1 is (2.35-3.43) mL: (8-12) mL: (2-4) g, cooled to 0-2°C, heated and stirred reaction temperature is 28-32°C, stirring reaction time is 10-12 h, cooled to 0-1°C, distilled water is added to quench the reaction, extracted with petroleum ether, and dried with anhydrous sodium sulfate.

[0016] Preferably, in Q2, the amount ratio of sodium azide and intermediate 2 is (0.12-0.17) g: (0.85-0.92) g, the stirring time at room temperature is 5-8 h, extracted with petroleum ether, washed with saturated ammonium chloride, and dried with anhydrous sodium sulfate; the amount ratio of ether, intermediate 3 and lithium aluminum hydride is (2.33-4.12) mL: (1.2-1.8) g: (0.58-0.64) g, the ice bath stirring time is 10-15 min, the room temperature stirring time is 30-45 min, and 1vt% ammonia solution is added. The reaction was quenched with liquid, filtered through diatomaceous earth, and dried over anhydrous sodium sulfate; in Q3, the amount ratio of benzoic acid, dichloromethane, 1-hydroxybenzotriazole, 1-ethyl-(3-dimethylaminopropyl)carbodiimide hydrochloride and intermediate 4 was (0.06-0.08) g: (3-5) mL: (0.06-0.09) g: (0.11-0.14) g: (0.09-0.12) g, the stirring reaction temperature was 0-2°C, the reaction time was 30-45 min, the heating stirring time was 25-32°C, and the time was 2-4 h.

[0017] Preferably, the preparation method of the modified antioxidant comprises the following steps:

[0018] S1: 2-chloro-4-nitrophenol, potassium carbonate and m-fluorobenzyl bromide are sequentially added to a container containing N,N-dimethylformamide, and after heating and stirring, extraction, washing, drying and vacuum distillation are performed to obtain a light yellow solid; the light yellow solid, iron powder and anhydrous ethanol are mixed and stirred, and then calcium chloride solution is added, and after heating and stirring, filtering, vacuum distillation and purification are performed to obtain a yellow solid;

[0019] S2: Under ice bath conditions, oxalyl chloride and N,N-dimethylformamide are slowly added to a dichloromethane container containing rosin acid, and the reaction is carried out at room temperature. After the reaction is completed, vacuum rotary evaporation is performed to obtain a yellow oily substance; the yellow oily substance is added to a container containing dichloromethane to obtain a mixed solution 1, and a yellow solid and triethylamine are mixed and stirred, and then added dropwise to the mixed solution 1 to react. After the reaction is completed, extraction, washing, drying, vacuum rotary evaporation, and purification are performed to obtain a modified antioxidant.

[0020] In the above process, 2-chloro-4-nitrophenol and m-fluorobenzyl bromide are used as raw materials to prepare a yellow solid through alkylation reaction and reduction reaction, and then rosin acid is used as raw material and oxalyl chloride is used as acylating agent. A yellow oil is obtained by acylation reaction under the action of N,N-dimethylformamide, and then the yellow oil and the yellow solid are subjected to amide condensation to obtain a modified antioxidant, wherein the synthetic reaction formula of the modified antioxidant is as follows:

[0021]

[0022] The results of mass spectrometry analysis of the light yellow solid were: m / z: 281.03 (100.0%), 283.02 (32.0%), 282.03 (14.3%), 284.03 (4.7%), 283.03 (1.6%); the results of mass spectrometry analysis of the yellow solid were: m / z: 251.05 (100.0%), 253.05 (32.0%), 252.05 (14.4%), 254.05 (4.7%), 253.06 (1.1%); the results of mass spectrometry analysis of the yellow oil were: m / z: 251.05 (100.0%), 253.05 (32.0%), 252.05 (14.4%), 254.05 (4.7%), 253.06 (1.1%). The analysis results are: m / z: 320.19 (100.0%), 322.19 (32.2%), 321.19 (21.7%), 323.19 (7.0%), 322.20 (2.3%); the mass spectrometry analysis results of the modified antioxidant are: m / z: 535.27 (100.0%), 536.27 (36.2%), 537.26 (32.0%), 538.27 (11.7%), 537.27 (6.9%), 539.27 (2.2%).

[0023] Preferably, in S1, the amount ratio of 2-chloro-4-nitrophenol, potassium carbonate, m-fluorobenzyl bromide and N,N-dimethylformamide is (1-1.8) g: (0.8-1.44) g: (1.1-1.98) g: (20-36) mL, the heating and stirring temperature is 80-90°C, the stirring time is 3-5 h, the mixture is extracted with a mixed solution of ethyl acetate and water, washed with saturated sodium chloride, and dried with anhydrous sodium sulfate; the amount ratio of light yellow solid, iron powder, anhydrous ethanol and calcium chloride solution is (1-1.3) g: (0.6-4.8) g: (15-20) mL: (1.4-2.1) mL, the concentration of calcium chloride solution is 0.3 g / mL, the heating and stirring temperature is 85-90°C, and the time is 8-10 h.

[0024] Preferably, in S2, the dosage ratio of rosin acid, dichloromethane, oxalyl chloride and N,N-dimethylformamide is (1-2) g: (25-50) mL: (0.63-0.89) g: (0.01-0.02) mL, and the reaction time at room temperature is 4-6 h; the dosage ratio of yellow oil, dichloromethane, yellow solid and triethylamine is (1.2-1.5) g: (10-12) mL: (0.31-0.53) mg: (0.27-0.32) g, the reaction temperature is 28-33°C, the reaction time is 18-20 h, and the mixture is washed with saturated sodium chloride and dried with anhydrous sodium sulfate.

[0025] Preferably, the method for preparing the cross-arm bird-proof packaging material comprises the following steps:

[0026] Step 1: Add EPDM rubber to an open mill, add antioxidant, accelerator and cross-linking agent in sequence, and after reaction, continue to add silicon filler and modified antioxidant, adhesive and pigment, and finally add vulcanizing agent to obtain a mixture;

[0027] Step 2: After the mixture is allowed to stand, it is transferred to a mold and vulcanized using a flat vulcanizer to obtain a cross-arm bird-proofing packaging material.

[0028] Preferably, in the step 1, the distance between the front and rear rollers of the mixing mill is 0.7-0.9 mm, and the roller temperature is 40-50° C.; in the step 2, the standing time is 20-24 h.

[0029] In summary, due to the adoption of the above technical solution, the beneficial effects of the present invention are:

[0030] 1. The present invention firstly uses p-bromoethylbenzene, chloromethyldimethylsilyl chloride, sodium azide, ether, lithium aluminum hydride and benzoic acid to prepare a silicon filler, and then uses 2-chloro-4-nitrophenol, m-fluorobenzyl bromide, iron powder, rosin acid, oxalyl chloride and triethylamine to prepare a modified antioxidant, and the prepared silicon filler and the modified antioxidant are added to EPDM rubber to prepare a cross-arm bird-proofing packaging material, so that it has excellent durability, flame retardancy and bird-proofing properties.

[0031] 2. The present invention adds the prepared silicon filler to EPDM rubber and uses it as a cross-arm bird-proof packaging material, which can effectively improve the durability and mechanical properties of the packaging material. The silicon atoms and oxygen atoms in the silicon filler are connected by covalent bonds to form a stable three-dimensional network structure, which effectively resists chemical erosion and physical damage. At the same time, it also increases the cross-linking points between rubber molecular chains and enhances the interaction force, thereby improving the weather resistance and durability of the packaging material. In addition, as a high-strength and high-hardness filler, the silicon filler is filled between rubber molecular chains to play a supporting and reinforcing role, and through the interaction forces such as van der Waals forces and hydrogen bonds, the overall material is made more compact and stable, which significantly enhances the mechanical properties. At the same time, the silicon filler also has excellent electrical insulation properties. The silicon atoms and oxygen atoms in the molecular structure form stable covalent bonds to prevent the free movement of electrons, thereby improving the electrical insulation properties of the packaging material and reducing the risk of leakage.

[0032] 3. The present invention can effectively improve the durability, bird-proofing and flame-retardant properties of the packaging material by adding the prepared modified antioxidant to the cross-arm bird-proofing packaging material. The modified antioxidant has excellent antioxidant properties, can effectively resist the oxidation reaction, slow down the aging process of the cross-arm bird-proofing packaging material, and can also reduce the degradation of the packaging material caused by oxidation, significantly improving the durability and service life of the packaging material. At the same time, the terpene functional groups contained in the prepared modified antioxidant have a special smell, which can produce strong sensory stimulation to birds and other animals, thereby achieving the purpose of repelling birds; and the fluorine atoms contained in the modified antioxidant can effectively improve the flame-retardant properties of the packaging material. DETAILED DESCRIPTION

[0033] The following will be described clearly and completely in conjunction with the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0034] Embodiment 1: This embodiment discloses a method for preparing a silicon filler, comprising the following steps:

[0035] Q1: Add 3.64 g of magnesium chips to a nitrogen-filled container, then add 10 mL of tetrahydrofuran, 8.73 mL of p-bromoethylbenzene and 0.15 g of iodine particles in sequence, heat at 60°C for 45 min, then heat at 75°C for reflux for 4 h. After the reaction, obtain intermediate 1; under a nitrogen atmosphere, slowly add 2.93 mL of chloromethyldimethylsilyl chloride to 10 mL of tetrahydrofuran and cool to 0°C to obtain a silane solution, add the silane solution dropwise to a container containing 3 g of intermediate 1 using a syringe, heat to 32°C, stir for 12 h, cool to 0°C, add distilled water to quench the reaction, extract with petroleum ether, dry with anhydrous sodium sulfate, concentrate under reduced pressure, and purify to obtain intermediate 2;

[0036] Q2: 0.15 g of sodium azide was added to a container containing 0.88 g of intermediate 2, and the mixture was stirred at room temperature for 8 h, then poured into distilled water, extracted with petroleum ether, washed with saturated ammonium chloride, dried with anhydrous sodium sulfate, and concentrated under reduced pressure to obtain intermediate 3; 3.22 mL of ether was added to a container containing 1.5 g of intermediate 3, and then 0.61 g of lithium aluminum hydride was added dropwise to the container, stirred in an ice bath for 15 min, stirred at room temperature for 30 min, 1 vt% ammonia solution was added to quench the reaction, filtered through diatomaceous earth, dried with anhydrous sodium sulfate, evaporated under reduced pressure, and purified to obtain intermediate 4;

[0037] Q3: In an ice bath environment, 0.07 g of benzoic acid was added to 4 mL of dichloromethane, and then 0.075 g of 1-hydroxybenzotriazole and 0.12 g of 1-ethyl-(3-dimethylaminopropyl)carbodiimide hydrochloride were added in sequence. After stirring at 0°C for 30 min, 0.11 g of intermediate 4 was added, and the temperature was raised to 32°C and stirred for 2 h. After the reaction was completed, a silicon filler was obtained.

[0038] This embodiment discloses a method for preparing a modified antioxidant, comprising the following steps:

[0039] S1: 1.4 g of 2-chloro-4-nitrophenol, 1.12 g of potassium carbonate and 1.54 g of m-fluorobenzyl bromide were added to a container containing 28 mL of N,N-dimethylformamide in sequence, heated and stirred at 85°C for 4 h, extracted with a mixed solution of ethyl acetate and water, washed with saturated sodium chloride, dried with anhydrous sodium sulfate, and distilled under reduced pressure to obtain a light yellow solid; 1.15 g of the light yellow solid, 2.7 g of iron powder and 17.5 mL of anhydrous ethanol were mixed and stirred, and then 1.7 mL of a 0.3 g / mL calcium chloride solution was added, heated and stirred at 85°C for 10 h, filtered, distilled under reduced pressure, and purified to obtain a yellow solid;

[0040] S2: Under ice bath conditions, 0.72 g of oxalyl chloride and 0.015 mL of N,N-dimethylformamide were slowly added to a 35 mL container of dichloromethane containing 1.5 g of rosin acid, and the mixture was reacted at room temperature for 6 h. After the reaction, the mixture was evaporated under reduced pressure to obtain a yellow oil. 1.35 g of the yellow oil was added to a container containing 11 mL of dichloromethane to obtain a mixed solution 1. 0.42 mg of a yellow solid and 0.29 g of triethylamine were mixed and stirred, and then added dropwise to the mixed solution 1, and the mixture was reacted at 33 ° C for 18 h. After the reaction was completed, the mixture was extracted, washed with saturated sodium chloride, dried with anhydrous sodium sulfate, evaporated under reduced pressure, and purified to obtain a modified antioxidant.

[0041] The present embodiment discloses a cross-arm bird-proofing packaging material, which is composed of the following ingredients in parts by weight: 55 parts of EPDM rubber, 1.5 parts of antioxidant, 3 parts of accelerator, 1 part of cross-linking agent, 4.5 parts of silicon filler, 6.5 parts of modified antioxidant, 2 parts of adhesive, 7 parts of pigment, and 1.1 parts of vulcanizing agent.

[0042] This embodiment discloses a method for preparing a cross-arm bird-proof packaging material, comprising the following steps:

[0043] Step 1: Add EPDM rubber to an open mill, the distance between the front and rear rollers of the open mill is 0.8 mm, the roller temperature is 45°C, and antioxidant, accelerator and cross-linking agent are added in sequence. After the reaction, silicon filler and modified antioxidant, adhesive and pigment are added, and finally vulcanizing agent is added to obtain a mixture;

[0044] Step 2: After the mixture is allowed to stand for 24 hours, it is transferred to a mold and vulcanized using a flat vulcanizer to obtain the cross-arm bird-proofing packaging material.

[0045] Embodiment 2: This embodiment discloses a method for preparing a silicon filler, comprising the following steps:

[0046] Q1: Add 3.12g of magnesium chips to a nitrogen-filled container, then add 12mL of tetrahydrofuran, 8.34mL of p-bromoethylbenzene and 0.12g of iodine particles in sequence, heat at 60°C for 45min, then heat at 75°C for reflux for 4h. After the reaction, obtain intermediate 1; under a nitrogen atmosphere, slowly add 2.35mL of chloromethyldimethylsilyl chloride to 8mL of tetrahydrofuran and cool to 0°C to obtain a silane solution, add the silane solution dropwise to a container containing 4g of intermediate 1 using a syringe, heat to 32°C, stir for 12h, cool to 0°C, add distilled water to quench the reaction, extract with petroleum ether, dry with anhydrous sodium sulfate, concentrate under reduced pressure, and purify to obtain intermediate 2;

[0047] Q2: 0.12 g of sodium azide was added to a container containing 0.92 g of intermediate 2, and the mixture was stirred at room temperature for 8 h, then poured into distilled water, extracted with petroleum ether, washed with saturated ammonium chloride, dried with anhydrous sodium sulfate, and concentrated under reduced pressure to obtain intermediate 3; 2.33 mL of ether was added to a container containing 1.8 g of intermediate 3, and then 0.58 g of lithium aluminum hydride was added dropwise to the container, stirred in an ice bath for 15 min, stirred at room temperature for 30 min, 1 vt% ammonia solution was added to quench the reaction, filtered through diatomaceous earth, dried with anhydrous sodium sulfate, evaporated under reduced pressure, and purified to obtain intermediate 4;

[0048] Q3: In an ice bath environment, 0.06 g of benzoic acid was added to 3 mL of dichloromethane, and then 0.06 g of 1-hydroxybenzotriazole and 0.11 g of 1-ethyl-(3-dimethylaminopropyl)carbodiimide hydrochloride were added in sequence. After stirring at 0°C for 30 min, 0.09 g of intermediate 4 was added, and the temperature was raised to 32°C and stirred for 2 h. After the reaction was completed, a silicon filler was obtained.

[0049] This embodiment discloses a method for preparing a modified antioxidant, comprising the following steps:

[0050] S1: 1 g of 2-chloro-4-nitrophenol, 0.8 g of potassium carbonate and 1.98 g of m-fluorobenzyl bromide were added to a container containing 20 mL of N,N-dimethylformamide in sequence, heated and stirred at 85°C for 4 h, extracted with a mixed solution of ethyl acetate and water, washed with saturated sodium chloride, dried with anhydrous sodium sulfate, and distilled under reduced pressure to obtain a light yellow solid; 1.3 g of the light yellow solid, 0.6 g of iron powder and 15 mL of anhydrous ethanol were mixed and stirred, and then 1.4 mL of a 0.3 g / mL calcium chloride solution was added, heated and stirred at 85°C for 10 h, filtered, distilled under reduced pressure, and purified to obtain a yellow solid;

[0051] S2: Under ice bath conditions, 0.63 g of oxalyl chloride and 0.01 mL of N,N-dimethylformamide were slowly added to a 25 mL dichloromethane container containing 1 g of rosin acid, and the mixture was reacted at room temperature for 6 h. After the reaction, the mixture was evaporated under reduced pressure to obtain a yellow oil. 1.2 g of the yellow oil was added to a container containing 10 mL of dichloromethane to obtain a mixed solution 1. 0.31 mg of a yellow solid and 0.27 g of triethylamine were mixed and stirred, and then added dropwise to the mixed solution 1, and the mixture was reacted at 33 ° C for 18 h. After the reaction was completed, the mixture was extracted, washed with saturated sodium chloride, dried with anhydrous sodium sulfate, evaporated under reduced pressure, and purified to obtain a modified antioxidant.

[0052] The present embodiment discloses a cross-arm bird-proofing packaging material, which is composed of the following ingredients in parts by weight: 50 parts of EPDM rubber, 1 part of antioxidant, 2 parts of accelerator, 1.2 parts of cross-linking agent, 6 parts of silicon filler, 8 parts of modified antioxidant, 1 part of adhesive, 6 parts of pigment, and 0.8 parts of vulcanizer.

[0053] This embodiment discloses a method for preparing a cross-arm bird-proof packaging material, comprising the following steps:

[0054] Step 1: Add EPDM rubber to an open mill, the distance between the front and rear rollers of the open mill is 0.8 mm, the roller temperature is 45°C, and antioxidant, accelerator and cross-linking agent are added in sequence. After the reaction, silicon filler and modified antioxidant, adhesive and pigment are added, and finally vulcanizing agent is added to obtain a mixture;

[0055] Step 2: After the mixture is allowed to stand for 24 hours, it is transferred to a mold and vulcanized using a flat vulcanizer to obtain the cross-arm bird-proofing packaging material.

[0056] Embodiment 3: This embodiment discloses a method for preparing a silicon filler, comprising the following steps:

[0057] Q1: Add 5.27g of magnesium chips to a container filled with nitrogen, then add 8mL of tetrahydrofuran, 9.23mL of p-bromoethylbenzene and 0.18g of iodine particles in sequence, heat at 60°C for 45min, then heat at 75°C for reflux for 4h. After the reaction, intermediate 1 is obtained; under a nitrogen atmosphere, 3.43mL of chloromethyldimethylsilyl chloride is slowly added to 12mL of tetrahydrofuran and cooled to 0°C to obtain a silane solution, and the silane solution is added dropwise to a container containing 2g of intermediate 1 using a syringe, and the temperature is raised to 32°C and stirred for 12h, then cooled to 0°C, and distilled water is added to quench the reaction, extracted with petroleum ether, dried with anhydrous sodium sulfate, concentrated under reduced pressure, and purified to obtain intermediate 2;

[0058] Q2: 0.17 g of sodium azide was added to a container containing 0.85 g of intermediate 2, and the mixture was stirred at room temperature for 8 h, then poured into distilled water, extracted with petroleum ether, washed with saturated ammonium chloride, dried with anhydrous sodium sulfate, and concentrated under reduced pressure to obtain intermediate 3; 4.12 mL of ether was added to a container containing 1.2 g of intermediate 3, and then 0.64 g of lithium aluminum hydride was added dropwise to the container, stirred in an ice bath for 15 min, stirred at room temperature for 30 min, 1 vt% ammonia solution was added to quench the reaction, filtered through diatomaceous earth, dried with anhydrous sodium sulfate, evaporated under reduced pressure, and purified to obtain intermediate 4;

[0059] Q3: In an ice bath environment, 0.08 g of benzoic acid was added to 5 mL of dichloromethane, and then 0.09 g of 1-hydroxybenzotriazole and 0.14 g of 1-ethyl-(3-dimethylaminopropyl)carbodiimide hydrochloride were added in sequence. After stirring at 0°C for 30 min, 0.12 g of intermediate 4 was added, and the temperature was raised to 32°C and stirred for 2 h. After the reaction was completed, a silicon filler was obtained.

[0060] This embodiment discloses a method for preparing a modified antioxidant, comprising the following steps:

[0061] S1: 1.8 g of 2-chloro-4-nitrophenol, 1.44 g of potassium carbonate and 1.1 g of m-fluorobenzyl bromide were added to a container containing 36 mL of N,N-dimethylformamide in sequence, heated and stirred at 85°C for 4 h, extracted with a mixed solution of ethyl acetate and water, washed with saturated sodium chloride, dried with anhydrous sodium sulfate, and distilled under reduced pressure to obtain a light yellow solid; 1 g of the light yellow solid, 4.8 g of iron powder and 20 mL of anhydrous ethanol were mixed and stirred, and then 2.1 mL of a 0.3 g / mL calcium chloride solution was added, heated and stirred at 85°C for 10 h, filtered, distilled under reduced pressure, and purified to obtain a yellow solid;

[0062] S2: Under ice bath conditions, 0.89 g of oxalyl chloride and 0.02 mL of N,N-dimethylformamide were slowly added to a 50 mL dichloromethane container containing 2 g of rosin acid, and the mixture was reacted at room temperature for 6 h. After the reaction, the mixture was evaporated under reduced pressure to obtain a yellow oil. 1.5 g of the yellow oil was added to a container containing 12 mL of dichloromethane to obtain a mixed solution 1. 0.53 mg of a yellow solid and 0.32 g of triethylamine were mixed and stirred, and then added dropwise to the mixed solution 1, and the mixture was reacted at 33 ° C for 18 h. After the reaction was completed, the mixture was extracted, washed with saturated sodium chloride, dried with anhydrous sodium sulfate, evaporated under reduced pressure, and purified to obtain a modified antioxidant.

[0063] The present embodiment discloses a cross-arm bird-proofing packaging material, which is composed of the following ingredients in parts by weight: 60 parts of EPDM rubber, 2 parts of antioxidant, 4 parts of accelerator, 0.8 parts of cross-linking agent, 3 parts of silicon filler, 5 parts of modified antioxidant, 3 parts of adhesive, 8 parts of pigment, and 1.4 parts of vulcanizing agent.

[0064] This embodiment discloses a method for preparing a cross-arm bird-proof packaging material, comprising the following steps:

[0065] Step 1: Add EPDM rubber to an open mill, the distance between the front and rear rollers of the open mill is 0.8 mm, the roller temperature is 45°C, and antioxidant, accelerator and cross-linking agent are added in sequence. After the reaction, silicon filler and modified antioxidant, adhesive and pigment are added, and finally vulcanizing agent is added to obtain a mixture;

[0066] Step 2: After the mixture is allowed to stand for 24 hours, it is transferred to a mold and vulcanized using a flat vulcanizer to obtain the cross-arm bird-proofing packaging material.

[0067] Embodiment 4: This embodiment discloses a method for preparing a silicon filler, comprising the following steps:

[0068] Q1: Add 4.28g of magnesium chips to a nitrogen-filled container, then add 9mL of tetrahydrofuran, 8.53mL of p-bromoethylbenzene and 0.13g of iodine particles in sequence, heat at 60°C for 45min, then heat at 75°C for reflux for 4h. After the reaction, obtain intermediate 1; under a nitrogen atmosphere, slowly add 2.63mL of chloromethyldimethylsilyl chloride to 9mL of tetrahydrofuran and cool to 0°C to obtain a silane solution, add the silane solution dropwise to a container containing 2.5g of intermediate 1 using a syringe, heat to 32°C, stir for 12h, cool to 0°C, add distilled water to quench the reaction, extract with petroleum ether, dry with anhydrous sodium sulfate, concentrate under reduced pressure, and purify to obtain intermediate 2;

[0069] Q2: 0.13 g of sodium azide was added to a container containing 0.86 g of intermediate 2, and the mixture was stirred at room temperature for 8 h, then poured into distilled water, extracted with petroleum ether, washed with saturated ammonium chloride, dried with anhydrous sodium sulfate, and concentrated under reduced pressure to obtain intermediate 3; 2.78 mL of ether was added to a container containing 1.4 g of intermediate 3, and then 0.59 g of lithium aluminum hydride was added dropwise to the container, stirred in an ice bath for 15 min, stirred at room temperature for 30 min, 1 vt% ammonia solution was added to quench the reaction, filtered through diatomaceous earth, dried with anhydrous sodium sulfate, evaporated under reduced pressure, and purified to obtain intermediate 4;

[0070] Q3: In an ice bath environment, 0.065 g of benzoic acid was added to 3.5 mL of dichloromethane, and then 0.08 g of 1-hydroxybenzotriazole and 0.13 g of 1-ethyl-(3-dimethylaminopropyl)carbodiimide hydrochloride were added in sequence. After stirring at 0°C for 30 min, 0.1 g of intermediate 4 was added, and the temperature was raised to 32°C and stirred for 2 h. After the reaction was completed, a silicon filler was obtained.

[0071] This embodiment discloses a method for preparing a modified antioxidant, comprising the following steps:

[0072] S1: 1.2 g of 2-chloro-4-nitrophenol, 0.96 g of potassium carbonate and 1.32 g of m-fluorobenzyl bromide were added to a container containing 24 mL of N,N-dimethylformamide in sequence, heated and stirred at 85°C for 4 h, extracted with a mixed solution of ethyl acetate and water, washed with saturated sodium chloride, dried with anhydrous sodium sulfate, and distilled under reduced pressure to obtain a light yellow solid; 1.1 g of the light yellow solid, 3.2 g of iron powder and 16 mL of anhydrous ethanol were mixed and stirred, and then 1.6 mL of a 0.3 g / mL calcium chloride solution was added, heated and stirred at 85°C for 10 h, filtered, distilled under reduced pressure, and purified to obtain a yellow solid;

[0073] S2: Under ice bath conditions, 0.68 g of oxalyl chloride and 0.012 mL of N,N-dimethylformamide were slowly added to a 30 mL dichloromethane container containing 1.2 g of rosin acid, and the mixture was reacted at room temperature for 6 h. After the reaction, the mixture was evaporated under reduced pressure to obtain a yellow oil. 1.4 g of the yellow oil was added to a container containing 10.5 mL of dichloromethane to obtain a mixed solution 1. 0.35 mg of a yellow solid and 0.28 g of triethylamine were mixed and stirred, and then added dropwise to the mixed solution 1, and the mixture was reacted at 33 ° C for 18 h. After the reaction was completed, the mixture was extracted, washed with saturated sodium chloride, dried with anhydrous sodium sulfate, evaporated under reduced pressure, and purified to obtain a modified antioxidant.

[0074] The present embodiment discloses a cross-arm bird-proofing packaging material, which is composed of the following ingredients in parts by weight: 52 parts of EPDM rubber, 1.2 parts of antioxidant, 2.5 parts of accelerator, 0.9 parts of cross-linking agent, 4 parts of silicon filler, 5 parts of modified antioxidant, 1.5 parts of adhesive, 6.5 parts of pigment, and 1.2 parts of vulcanizing agent.

[0075] This embodiment discloses a method for preparing a cross-arm bird-proof packaging material, comprising the following steps:

[0076] Step 1: Add EPDM rubber to an open mill, the distance between the front and rear rollers of the open mill is 0.8 mm, the roller temperature is 45°C, and antioxidant, accelerator and cross-linking agent are added in sequence. After the reaction, silicon filler and modified antioxidant, adhesive and pigment are added, and finally vulcanizing agent is added to obtain a mixture;

[0077] Step 2: After the mixture is allowed to stand for 24 hours, it is transferred to a mold and vulcanized using a flat vulcanizer to obtain the cross-arm bird-proofing packaging material.

[0078] Comparative Example 1: Compared with Example 1, in the process of preparing the silicon filler in Comparative Example 1, no chloromethyldimethylsilyl chloride is added, and other conditions remain unchanged.

[0079] Comparative Example 2: Compared with Example 1, in the process of preparing the modified antioxidant in Comparative Example 2, no rosin acid was added, and other conditions remained unchanged.

[0080] Comparative Example 3: Compared with Example 1, in the process of preparing the cross-arm bird-proofing packaging material, no silicon filler is added in Comparative Example 3, and other conditions remain unchanged.

[0081] Comparative Example 4: Compared with Example 1, in Comparative Example 4, during the preparation of the cross-arm bird-proofing packaging material, no modified antioxidant is added, and other conditions remain unchanged.

[0082] Experimental example: The combustion performance of the sample was tested according to GB / T 2408-2021, the durability of the sample was tested according to GB / T3512-2014, and the tensile strength of the sample was tested according to HG / T 3849-2008. The test results are shown in the following table:

[0083] Table 1

[0084]

[0085]

[0086] From the test results in Table 1, it can be seen that the packaging materials prepared by Examples 1-4 of the present invention have excellent flame retardant properties and durability. From the comparison between Comparative Example 1 and Examples 1-4, it can be seen that the addition of chloromethyldimethylchlorosilane can effectively improve the durability of the packaging material; from the comparison between Comparative Example 2 and Examples 1-4, it can be seen that the addition of rosin acid can effectively improve the flame retardant properties and durability of the packaging material; from the comparison between Comparative Example 3 and Examples 1-4, it can be seen that the addition of silicon filler can effectively improve the durability of the packaging material; from the comparison between Comparative Example 4 and Examples 1-4, it can be seen that the addition of modified antioxidants can effectively improve the flame retardant properties and durability of the packaging material.

[0087] The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.

[0088] The preferred embodiments of the present invention disclosed above are only used to help explain the present invention. The preferred embodiments do not describe all the details in detail, nor do they limit the invention to only specific implementation methods. Obviously, many modifications and changes can be made according to the content of this specification. This specification selects and specifically describes these embodiments in order to better explain the principles and practical applications of the present invention, so that those skilled in the art can understand and use the present invention well. The present invention is limited only by the claims and their full scope and equivalents.

Claims

1. A cross arm bird-proof packaging material, characterized in that: The invention is composed of the following components in parts by weight: 50-60 parts of ethylene propylene rubber, 1-2 parts of antioxidant, 2-4 parts of accelerator, 0.8-1.2 parts of crosslinking agent, 3-6 parts of silicon filler, 5-8 parts of modified antioxidant, 1-3 parts of adhesive, 6-8 parts of pigment and 0.8-1.4 parts of vulcanizing agent, wherein the silicon filler is prepared from 4-bromoethylbenzene, chloromethyldimethylchlorosilane, sodium azide, ether, lithium aluminum hydride and benzoic acid, and the modified antioxidant is prepared from 2-chloro-4-nitrophenol, m-fluorobenzyl bromide, iron powder, rosin acid, oxalyl chloride and triethylamine.

2. The cross arm bird-proofing packaging material according to claim 1, characterized in that: The preparation method of the silicon filler comprises the following steps: Q1: Add magnesium chips to a container filled with nitrogen, then add tetrahydrofuran, 4-bromoethylbenzene and iodine particles in sequence, heat for reaction, then heat for reflux reaction, and after the reaction is completed, obtain intermediate 1; slowly add chloromethyldimethylsilyl chloride to tetrahydrofuran under a nitrogen atmosphere and cool to obtain a silane solution, add the silane solution dropwise to the container containing intermediate 1 using a syringe, heat and stir for reaction, cool, quench the reaction, extract, dry, concentrate under reduced pressure, and purify to obtain intermediate 2; Q2: Sodium azide is added to a container containing intermediate 2, and after stirring and mixing at room temperature, the mixture is poured into distilled water, extracted, washed, dried, and concentrated under reduced pressure to obtain intermediate 3; ether is added to a container containing intermediate 3, and then lithium aluminum hydride is added dropwise to the container, stirred in an ice bath, stirred at room temperature, the reaction is quenched, filtered, dried, evaporated under reduced pressure, and purified to obtain intermediate 4; Q3: In an ice bath environment, benzoic acid is added to dichloromethane, and then 1-hydroxybenzotriazole and 1-ethyl-(3-dimethylaminopropyl)carbodiimide hydrochloride are added in sequence. After stirring for reaction, intermediate 4 is added, the temperature is raised and stirred, and after the reaction is completed, a silicon filler is obtained.

3. The cross arm bird-proofing packaging material according to claim 2, characterized in that: In the Q1, the amount ratio of magnesium chips, tetrahydrofuran, p-bromoethylbenzene and iodine particles is (3.12-5.27) g: (8-12) mL: (8.34-9.23) mL: (0.12-0.18) g, the heating reaction temperature is 55-65°C, the reaction time is 30-45 min, the heating reflux reaction temperature is 70-75°C, and the reflux time is 3-4 h; the amount ratio of chloromethyldimethylsilyl chloride, tetrahydrofuran and intermediate 1 is (2.35-3.43) mL: (8-12) mL: (2-4) g, cooled to 0-2°C, heated and stirred reaction temperature is 28-32°C, stirring reaction time is 10-12 h, cooled to 0-1°C, distilled water is added to quench the reaction, extracted with petroleum ether, and dried with anhydrous sodium sulfate.

4. The cross arm bird-proofing packaging material according to claim 2, characterized in that: In the Q2, the dosage ratio of sodium azide and intermediate 2 is (0.12-0.17) g: (0.85-0.92) g, the stirring time at room temperature is 5-8 h, extracted with petroleum ether, washed with saturated ammonium chloride, and dried with anhydrous sodium sulfate; the dosage ratio of ether, intermediate 3 and lithium aluminum hydride is (2.33-4.12) mL: (1.2-1.8) g: (0.58-0.64) g, the ice bath stirring time is 10-15 min, the room temperature stirring time is 30-45 min, and 1vt% ammonia solution is added for The reaction was quenched, filtered through diatomaceous earth, and dried over anhydrous sodium sulfate; in Q3, the amount ratio of benzoic acid, dichloromethane, 1-hydroxybenzotriazole, 1-ethyl-(3-dimethylaminopropyl)carbodiimide hydrochloride and intermediate 4 was (0.06-0.08) g: (3-5) mL: (0.06-0.09) g: (0.11-0.14) g: (0.09-0.12) g, the stirring reaction temperature was 0-2°C, the reaction time was 30-45 min, the heating stirring time was 25-32°C, and the time was 2-4 h.

5. The cross arm bird-proofing packaging material according to claim 1, characterized in that: The preparation method of the modified antioxidant comprises the following steps: S1: 2-chloro-4-nitrophenol, potassium carbonate and m-fluorobenzyl bromide are sequentially added to a container containing N,N-dimethylformamide, and after heating and stirring, extraction, washing, drying and vacuum distillation are performed to obtain a light yellow solid; the light yellow solid, iron powder and anhydrous ethanol are mixed and stirred, and then calcium chloride solution is added, and after heating and stirring, filtering, vacuum distillation and purification are performed to obtain a yellow solid; S2: Under ice bath conditions, oxalyl chloride and N,N-dimethylformamide are slowly added to a dichloromethane container containing rosin acid, and the reaction is carried out at room temperature. After the reaction is completed, vacuum rotary evaporation is performed to obtain a yellow oily substance; the yellow oily substance is added to a container containing dichloromethane to obtain a mixed solution 1, and a yellow solid and triethylamine are mixed and stirred, and then added dropwise to the mixed solution 1 to react. After the reaction is completed, extraction, washing, drying, vacuum rotary evaporation, and purification are performed to obtain a modified antioxidant.

6. The cross arm bird-proofing packaging material according to claim 5, characterized in that: In the S1, the amount ratio of 2-chloro-4-nitrophenol, potassium carbonate, m-fluorobenzyl bromide and N,N-dimethylformamide is (1-1.8) g: (0.8-1.44) g: (1.1-1.98) g: (20-36) mL, the heating and stirring temperature is 80-90° C., the stirring time is 3-5 h, extraction is performed with a mixed solution of ethyl acetate and water, washing is performed with saturated sodium chloride, and drying is performed with anhydrous sodium sulfate; the amount ratio of light yellow solid, iron powder, anhydrous ethanol and calcium chloride solution is (1-1.3) g: (0.6-4.8) g: (15-20) mL: (1.4-2.1) mL, the concentration of calcium chloride solution is 0.3 g / mL, the heating and stirring temperature is 85-90° C., and the time is 8-10 h.

7. The cross arm bird-proofing packaging material according to claim 5, characterized in that: In S2, the dosage ratio of rosin acid, dichloromethane, oxalyl chloride and N,N-dimethylformamide is (1-2) g: (25-50) mL: (0.63-0.89) g: (0.01-0.02) mL, and the reaction time at room temperature is 4-6 h; the dosage ratio of yellow oil, dichloromethane, yellow solid and triethylamine is (1.2-1.5) g: (10-12) mL: (0.31-0.53) mg: (0.27-0.32) g, the reaction temperature is 28-33°C, the reaction time is 18-20 h, and the product is washed with saturated sodium chloride and dried with anhydrous sodium sulfate.

8. The method for preparing the cross arm bird-proof packaging material according to any one of claims 1 to 7, characterized in that: The following steps are involved: Step 1: Add EPDM rubber to an open mill, add antioxidant, accelerator and cross-linking agent in sequence, and after reaction, continue to add silicon filler and modified antioxidant, adhesive and pigment, and finally add vulcanizing agent to obtain a mixture; Step 2: After the mixture is allowed to stand, it is transferred to a mold and vulcanized using a flat vulcanizer to obtain a cross-arm bird-proofing packaging material.

9. The method for preparing the cross-arm bird-proof packaging material according to claim 8, characterized in that: In the step 1, the distance between the front and rear rollers of the mixing mill is 0.7-0.9 mm, and the roller temperature is 40-50° C.; in the step 2, the standing time is 20-24 hours.

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