A sealing ring material and a method for producing the same
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-05
- Publication Date
- 2026-08-11
AI Technical Summary
[0003]目前,市面上常见的密封圈多以橡胶为基材,其具有良好的弹性,在受力环境下可发生形变填充到间隙中形成密封,可适应不同形状和尺寸的配合面,其中,丁腈橡胶/氯丁橡胶复合密封材料兼具耐油性和耐候性,被广泛应用在各种密封环境下;但是,橡胶材料的强度不足,特别在一些高压管路中,橡胶密封圈强度不足,金属密封圈的密封性不稳定,导致密封材料逐渐难以满足高压低损耗的发展需求;现有技术中,通过在橡胶材料中引入高性能填料,如石墨烯(Gr)、碳纳米管(CNT)等,这些填料在一定程度上可以提升橡胶密封材料的强度,但是,这些填料多为硬质材料,在外力作用下,两者极易产生不可逆的滑移形变,使得密封结构变形,导致密封性下降,甚至密封失效
本发明公开一种适用于橡胶体系的CNT复合强化剂,其由烷基硫醇与二烯丙基胺加成反应,得到具有双支烷基链的中间体1,再由烯丙基碘与中间体1中的仲胺取代,形成叔胺化合物,即中间体2,之后由3-氯丙基三甲氧基硅烷与中间体2进行季铵化反应,制得改性剂,最后将改性剂水解偶联负载到碳纳米管表面;碳纳米管自身具有极高的强度和模量,改性剂引入烷基链修饰,提高碳纳米管的分散性,利于形成均匀地强化效果;与现有偶联碳纳米管材料相比,其季铵结构和硫醚结构促进其分子中的不饱和双键与橡胶基体硫化强化,有效提升碳纳米管与橡胶基体的结合强度,进一步提升碳纳米管的强化作用,而其双支烷基链穿插在碳纳米管和橡胶的交联界面间形成增韧作用,改善碳纳米管与橡胶的结合韧性,在受到外力作用时,碳纳米管与橡胶大分子可发生更大的弹性形变,一方面使得材料强韧性得以协同提升,另一方面,该弹性形变赋予材料优异的抗永久压缩变形和抗蠕变性能,应用于密封圈中具有更稳定的密封效果。
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Abstract
Description
Technical Field
[0001] This invention belongs to the field of polymer materials, specifically, it relates to a sealing ring material and its preparation method. Background Technology
[0002] The primary function of sealing rings is to prevent the leakage of liquids or gases. Based on their function, sealing rings can be mainly classified into oil-resistant sealing rings, waterproof sealing rings, corrosion-resistant sealing rings, and gas sealing rings. Based on their form, there are also many varieties of products, including lip seals, O-rings, and seals with complex cross-sectional shapes. They are widely used in various industrial machinery, hydraulic pipelines, valves, and other fields.
[0003] Currently, most common sealing rings on the market are made of rubber, which has good elasticity and can deform under stress to fill gaps and form a seal. It can adapt to mating surfaces of different shapes and sizes. Among them, nitrile rubber / chloroprene rubber composite sealing materials have both oil resistance and weather resistance and are widely used in various sealing environments. However, the strength of rubber materials is insufficient, especially in some high-pressure pipelines. The strength of rubber sealing rings is insufficient, and the sealing performance of metal sealing rings is unstable, making it increasingly difficult for sealing materials to meet the development requirements of high pressure and low loss. In existing technologies, high-performance fillers such as graphene (Gr) and carbon nanotubes (CNT) are introduced into rubber materials. These fillers can improve the strength of rubber sealing materials to a certain extent. However, these fillers are mostly hard materials. Under external force, they are prone to irreversible slip deformation, which causes deformation of the sealing structure, resulting in decreased sealing performance or even sealing failure. Summary of the Invention
[0004] In order to solve the technical problems mentioned in the background art, the purpose of this invention is to provide a sealing ring material and a method for preparing the same.
[0005] The objective of this invention can be achieved through the following technical solutions: A sealing ring material, by weight, comprises: 100 parts of nitrile rubber, 15-20 parts of chloroprene rubber, 10-15 parts of CNT composite reinforcing agent, 12-17 parts of reinforcing filler, 1.9-2.3 parts of vulcanizing agent, 1-1.4 parts of accelerator, 2-3 parts of antioxidant, and 2.2-2.8 parts of anti-sticking agent.
[0006] The CNT composite reinforcing agent is prepared by the following method: Step A1: Premix diallylamine, benzoyl peroxide and acetone, purge with nitrogen, heat to 30-55℃, stir at 60-90 rpm, irradiate with 120-200 W / m2 UV, slowly add alkyl thiols and react for 2.5-4 h, add sodium sulfite to quench the reaction, remove acetone by rotary evaporation, wash the substrate with water and dry to obtain intermediate 1; Furthermore, the feed ratio of diallylamine, alkyl thiol, benzoyl peroxide, and acetone is 0.1 mol: 0.2 mol: 0.07-0.11 g: 60-120 mL. The alkyl thiol undergoes an addition reaction with diallylamine to introduce a terminal alkyl chain. The specific reaction process is shown below:
[0007] Preferably, the alkyl thiol is selected from one of n-octyl thiol, n-tetradecyl thiol, and n-octadecyl thiol.
[0008] Step A2: Premix intermediate 1, potassium carbonate, 15-crown ether-5 and tetrahydrofuran, preheat to 30-40℃, stir at 120-180 rpm, add allyl iodine intermittently and react for 2.5-4 h, then continue to heat to 55-65℃ and react for 1-1.5 h. After the reaction is completed, remove tetrahydrofuran by rotary evaporation, wash the substrate with water and dry to obtain intermediate 2; Furthermore, the feed ratio of intermediate 1, allyl iodine, potassium carbonate, 15-crown ether-5, and tetrahydrofuran is 0.1 mol: 0.1 mol: 0.5-0.8 g: 6-10 mL: 100-170 mL. Allyl iodine substitutes with the secondary amine in intermediate 1 to form a tertiary amine compound. The specific reaction process is shown below:
[0009] Step A3: Mix intermediate 2,3-chloropropyltrimethoxysilane, potassium iodide, hydroquinone and dioxane, heat to 90-100℃, stir at 30-50 rpm, reflux for 20-30 h, and remove dioxane by rotary evaporation under reduced pressure after the reaction is completed to obtain the modifier. Furthermore, the feed ratio of intermediate 2, 3-chloropropyltrimethoxysilane, potassium iodide, hydroquinone, and dioxane is 0.1 mol: 0.105-0.11 mol: 0.9-1.4 g: 40-60 mg: 150-240 mL. 3-chloropropyltrimethoxysilane undergoes a quaternization reaction with intermediate 2, the specific reaction process of which is shown below:
[0010] Step A4: Mix the modifier, dimethylacetamide, ethanol and deionized water, adjust the pH to 2-3 with hydrochloric acid, add carbon nanotubes and disperse ultrasonically, stir for 3-4 hours, then neutralize with ammonia water, let stand for 24 hours, take the precipitate, wash with water and dry to obtain CNT composite reinforcing agent; Furthermore, the feeding ratio of carbon nanotubes, modifier, dimethylacetamide, ethanol and deionized water is 10g:0.6-0.8g:10-15mL:10-20mL:15-25mL. The modifier is hydrolyzed under acidic conditions and coupled and loaded onto the surface of carbon nanotubes for composite.
[0011] Preferably, the vulcanizing agent is selected from sulfur, and the accelerator is a compound of zinc oxide and tetrabenzylthiuram disulfide.
[0012] A method for preparing a sealing ring material is as follows: nitrile rubber and chloroprene rubber are mixed and milled onto a roll, an accelerator, an antioxidant, and an anti-sticking agent are added for a first mixing, followed by the addition of a CNT composite reinforcing agent and reinforcing filler for a second mixing, and finally a vulcanizing agent is added for thinning and sheeting to obtain the sealing ring material.
[0013] The beneficial effects of this invention are: This invention discloses a CNT composite reinforcing agent suitable for rubber systems. It is prepared by an addition reaction of alkyl thiols and diallylamine to obtain intermediate 1 with bibranched alkyl chains. Then, allyl iodine replaces the secondary amine in intermediate 1 to form a tertiary amine compound, intermediate 2. Subsequently, 3-chloropropyltrimethoxysilane undergoes a quaternization reaction with intermediate 2 to obtain a modifier. Finally, the modifier is hydrolyzed and coupled onto the surface of carbon nanotubes. Carbon nanotubes themselves possess extremely high strength and modulus. The alkyl chain modification introduced by the modifier improves the dispersibility of the carbon nanotubes, facilitating a uniform reinforcing effect. Compared with existing coupled carbon nanotube materials, this method offers advantages in various aspects. Its quaternary ammonium structure and thioether structure promote the vulcanization and strengthening of the unsaturated double bonds in its molecule with the rubber matrix, effectively improving the bonding strength between carbon nanotubes and the rubber matrix, and further enhancing the strengthening effect of carbon nanotubes. Its bibranched alkyl chains interpenetrate between the cross-linking interface of carbon nanotubes and rubber to form a toughening effect, improving the bonding toughness between carbon nanotubes and rubber. When subjected to external force, carbon nanotubes and rubber macromolecules can undergo greater elastic deformation. On the one hand, the strength and toughness of the material are synergistically improved. On the other hand, this elastic deformation endows the material with excellent resistance to permanent compression deformation and creep resistance, resulting in a more stable sealing effect when applied to sealing rings. Detailed Implementation
[0014] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.
[0015] Example 1: Preparation of sealing ring material, the specific implementation process is as follows: (1) Preparation of CNT composite reinforcing agent Step A1: Premix diallylamine, benzoyl peroxide, and acetone, purge with nitrogen for protection, heat to 30°C, stir at 60 rpm, and irradiate with 120 W / m² UV light. Slowly add alkyl thiols and react for 2.5 h. The alkyl thiols are selected from n-octyl mercaptan. The feed ratio of diallylamine, n-octyl mercaptan, benzoyl peroxide, and acetone is 0.1 mol: 0.2 mol: 0.07 g: 60 mL. After the reaction is complete, add 50 ppm sodium sulfite to quench the reaction. Remove acetone by rotary evaporation. Wash the substrate with water and dry to obtain intermediate 1.
[0016] Step A2: Take intermediate 1, potassium carbonate, 15-crown ether-5 and tetrahydrofuran, premix them, preheat to 30℃, stir at 120 rpm, take allyl iodine in equal amounts divided into five portions, add them intermittently for 10 min, control the total reaction time of allyl iodine addition to 2.5 h, and then continue to heat to 55℃ and react for 1 h. The feed ratio of intermediate 1, allyl iodine, potassium carbonate, 15-crown ether-5 and tetrahydrofuran is 0.1 mol: 0.1 mol: 0.5 g: 6 mL: 100 mL. After the reaction is completed, remove tetrahydrofuran by rotary evaporation, wash the substrate with water and dry to obtain intermediate 2.
[0017] Step A3: Mix intermediate 2,3-chloropropyltrimethoxysilane, potassium iodide, hydroquinone, and dioxane, heat to 90°C, stir at 30 rpm, and reflux for 20 h. The feed ratio of intermediate 2,3-chloropropyltrimethoxysilane, potassium iodide, hydroquinone, and dioxane is 0.1 mol: 0.105 mol: 0.9 g: 40 mg: 150 mL. After the reaction is completed, remove dioxane by rotary evaporation under reduced pressure to obtain the modifier.
[0018] Step A4: Mix the modifier, dimethylacetamide, ethanol and deionized water, adjust the pH to 3 with hydrochloric acid, add carbon nanotubes and ultrasonically disperse, stir for 3 hours, then neutralize with ammonia water and let stand for 24 hours. The carbon nanotubes are selected from TNMPH1 type raw materials. The feeding ratio of carbon nanotubes, modifier, dimethylacetamide, ethanol and deionized water is 10g:0.6g:10mL:10mL:15mL. Finally, take the precipitate, wash with water and dry to obtain CNT composite reinforcing agent.
[0019] (2) Preparation of sealing ring material Ingredients: Raw materials are prepared according to the following proportions by weight: 100 parts of nitrile rubber (Nancar® 1052 type raw material used in this implementation); 15 parts of chloroprene rubber (CR322 type raw material used in this implementation); 10 parts of CNT composite reinforcing agent (self-made in this embodiment); 12 parts of reinforcing filler (carbon black N330 and carbon black N660 compounded in a mass ratio of 2:1 used in this implementation); 1.9 parts of vulcanizing agent (sulfur used in this implementation); 1 part of accelerator (zinc oxide and tetrabenzylthiuram disulfide compounded in a mass ratio of 5:1 used in this implementation); 2 parts of antioxidant (antioxidant RD and 85# microcrystalline wax compounded in a mass ratio of 1:1 used in this implementation); and 2.2 parts of anti-adhesion agent (industrial grade stearic acid used in this implementation).
[0020] Mixing: Nitrile rubber and chloroprene rubber are rolled at 60°C until they are wrapped around the rolls. Accelerators, antioxidants and anti-sticking agents are added for a first mixing. Then CNT composite reinforcing agent and reinforcing filler are added for a second mixing. Finally, vulcanizing agent is added and the mixture is passed through the rolls four times. After sheeting, the sealing ring material is obtained.
[0021] Example 2: Preparation of sealing ring material, the specific implementation process is as follows: (1) Preparation of CNT composite reinforcing agent Step A1: Premix diallylamine, benzoyl peroxide, and acetone, purge with nitrogen, heat to 55°C, stir at 90 rpm, and irradiate with 200 W / m² UV light. Slowly add alkyl thiolsitol and react for 4 h. The alkyl thiolsitol is selected from n-octadecyl mercaptan. The feed ratio of diallylamine, n-octadecyl mercaptan, benzoyl peroxide, and acetone is 0.1 mol: 0.2 mol: 0.11 g: 120 mL. After the reaction is complete, add 50 ppm sodium sulfite to quench the reaction. Remove acetone by rotary evaporation. Wash the substrate with water and dry to obtain intermediate 1.
[0022] Step A2: Take intermediate 1, potassium carbonate, 15-crown ether-5 and tetrahydrofuran, premix them, preheat to 40℃, stir at 180 rpm, take allyl iodine in equal amounts divided into five portions, add them intermittently for 20 min, control the total reaction time of allyl iodine addition to 4 h, and then continue to heat to 65℃ and react for 1.5 h. The feed ratio of intermediate 1, allyl iodine, potassium carbonate, 15-crown ether-5 and tetrahydrofuran is 0.1 mol: 0.1 mol: 0.8 g: 10 mL: 170 mL. After the reaction is completed, remove tetrahydrofuran by rotary evaporation, wash the substrate with water and dry to obtain intermediate 2.
[0023] Step A3: Mix intermediate 2,3-chloropropyltrimethoxysilane, potassium iodide, hydroquinone, and dioxane, heat to 100℃, stir at 50 rpm, and reflux for 30 h. The feed ratio of intermediate 2,3-chloropropyltrimethoxysilane, potassium iodide, hydroquinone, and dioxane is 0.1 mol: 0.11 mol: 1.4 g: 60 mg: 240 mL. After the reaction is completed, remove dioxane by rotary evaporation under reduced pressure to obtain the modifier.
[0024] Step A4: Mix the modifier, dimethylacetamide, ethanol and deionized water, adjust the pH to 2 with hydrochloric acid, add carbon nanotubes and ultrasonically disperse, stir for 4 hours, then neutralize with ammonia water and let stand for 24 hours. The carbon nanotubes are selected from TNMPH1 type raw materials. The feeding ratio of carbon nanotubes, modifier, dimethylacetamide, ethanol and deionized water is 10g:0.8g:15mL:20mL:25mL. Finally, take the precipitate, wash with water and dry to obtain CNT composite reinforcing agent.
[0025] (2) Preparation of sealing ring material Ingredients: Raw materials are prepared according to parts by weight: 100 parts of nitrile rubber (Nancar® 1052 type raw material used in the implementation); 20 parts of chloroprene rubber (CR322 type raw material used in the implementation); 15 parts of CNT composite reinforcing agent (self-made in this embodiment); 17 parts of reinforcing filler (carbon black N330 and carbon black N660 compounded in a mass ratio of 2:1 in the implementation); 2.3 parts of vulcanizing agent (sulfur used in the implementation); 1.4 parts of accelerator (zinc oxide and tetrabenzylthiuram disulfide compounded in a mass ratio of 5:1 in the implementation); 3 parts of antioxidant (antioxidant RD and 85# microcrystalline wax compounded in a mass ratio of 1:1 in the implementation); and 2.8 parts of anti-adhesion agent (industrial grade stearic acid used in the implementation).
[0026] Mixing: Nitrile rubber and chloroprene rubber are rolled at 60°C until they are wrapped around the rolls. Accelerators, antioxidants and anti-sticking agents are added for a first mixing. Then CNT composite reinforcing agent and reinforcing filler are added for a second mixing. Finally, vulcanizing agent is added and the mixture is passed through the rolls four times. After sheeting, the sealing ring material is obtained.
[0027] Example 3: Preparation of sealing ring material, the specific implementation process is as follows: (1) Preparation of CNT composite reinforcing agent Step A1: Premix diallylamine, benzoyl peroxide, and acetone, purge with nitrogen for protection, heat to 45°C, stir at 90 rpm, and irradiate with 150 W / m² UV light. Slowly add alkyl thiols and react for 3.2 h. The alkyl thiols are selected from n-tetradecyl thiols. The feed ratio of diallylamine, n-tetradecyl thiols, benzoyl peroxide, and acetone is 0.1 mol: 0.2 mol: 0.1 g: 95 mL. After the reaction is complete, add 50 ppm sodium sulfite to quench the reaction. Remove acetone by rotary evaporation. Wash the substrate with water and dry to obtain intermediate 1.
[0028] Step A2: Take intermediate 1, potassium carbonate, 15-crown ether-5 and tetrahydrofuran, premix them, preheat to 35℃, stir at 180 rpm, take allyl iodine in equal amounts divided into five portions, add them intermittently for 15 min, control the total reaction time of allyl iodine addition to 3.5 h, and then continue to heat to 60℃ and react for 1.2 h. The feed ratio of intermediate 1, allyl iodine, potassium carbonate, 15-crown ether-5 and tetrahydrofuran is 0.1 mol: 0.1 mol: 0.7 g: 8 mL: 120 mL. After the reaction is completed, remove tetrahydrofuran by rotary evaporation, wash the substrate with water and dry to obtain intermediate 2.
[0029] Step A3: Mix intermediate 2,3-chloropropyltrimethoxysilane, potassium iodide, hydroquinone, and dioxane, heat to 100℃, stir at 30 rpm, and reflux for 25 h. The feed ratio of intermediate 2,3-chloropropyltrimethoxysilane, potassium iodide, hydroquinone, and dioxane is 0.1 mol: 0.108 mol: 1.1 g: 50 mg: 220 mL. After the reaction is completed, remove dioxane by rotary evaporation under reduced pressure to obtain the modifier.
[0030] Step A4: Mix the modifier, dimethylacetamide, ethanol and deionized water, adjust the pH to 3 with hydrochloric acid, add carbon nanotubes and ultrasonically disperse, then stir for 3.5 h, neutralize with ammonia water and let stand for 24 h. The carbon nanotubes are selected from TNMPH1 type raw materials. The feeding ratio of carbon nanotubes, modifier, dimethylacetamide, ethanol and deionized water is 10 g: 0.7 g: 12 mL: 15 mL: 20 mL. Finally, take the precipitate, wash with water and dry to obtain CNT composite reinforcing agent.
[0031] (2) Preparation of sealing ring material Ingredients: Raw materials are prepared according to the following weight proportions: 100 parts of nitrile rubber (Nancar® 1052 type raw material used in this implementation); 17 parts of chloroprene rubber (CR322 type raw material used in this implementation); 12 parts of CNT composite reinforcing agent (self-made in this embodiment); 14 parts of reinforcing filler (carbon black N330 and carbon black N660 compounded in a mass ratio of 2:1 used in this implementation); 2.1 parts of vulcanizing agent (sulfur used in this implementation); 1.1 parts of accelerator (zinc oxide and tetrabenzylthiuram disulfide compounded in a mass ratio of 5:1 used in this implementation); 2.5 parts of antioxidant (antioxidant RD and 85# microcrystalline wax compounded in a mass ratio of 1:1 used in this implementation); and 2.4 parts of anti-adhesion agent (industrial grade stearic acid used in this implementation).
[0032] Mixing: Nitrile rubber and chloroprene rubber are rolled at 60°C until they are wrapped around the rolls. Accelerators, antioxidants and anti-sticking agents are added for a first mixing. Then CNT composite reinforcing agent and reinforcing filler are added for a second mixing. Finally, vulcanizing agent is added and the mixture is passed through the rolls four times. After sheeting, the sealing ring material is obtained.
[0033] Comparative Example 1, referring to Example 3, replaces the CNT composite reinforcing agent with the same weight of carbon nanotubes, and the rest of the implementation process is exactly the same.
[0034] Comparative Example 2: Carbon nanotubes were treated with silane coupling agent KH-570 to replace the CNT composite reinforcing agent, as detailed below: The silane coupling agent KH-570, ethanol, and deionized water were mixed, and the pH was adjusted to 3 with hydrochloric acid. The mixture was stirred and hydrolyzed at room temperature for 30 min. Carbon nanotubes were then added and ultrasonically dispersed. After stirring for 3 h, the mixture was neutralized with ammonia water and allowed to stand for 24 h. The feed ratio of carbon nanotubes, silane coupling agent KH-570, ethanol, and deionized water was 10 g: 0.6 g: 20 mL: 30 mL. The precipitate was washed with water and dried to obtain KH-570-coupled carbon nanotubes. The rest of the process was exactly the same.
[0035] The prepared sealing ring material was placed in a vulcanizing machine, and the vulcanization conditions were controlled at 170℃ × 10MPa for 15 min. After natural standing for 24 h, samples were taken. The Shore A hardness of the samples was tested according to GB / T 531.1-2008 standard; the tensile properties of the samples were tested according to GB / T 528-2009 standard at a tensile rate of 500 mm / min; the tear strength of the samples was tested according to GB / T 529-2008 standard; the permanent compression deformation of the samples was tested according to GB / T 7759.1-2015 standard at a compression rate of 30% and a temperature of 80℃; and the creep of the samples was tested according to GB / T 19242-2003 standard. The specific test results are shown in Table 1. Table 1
[0036] As can be seen from the test results in Table 1, the sealing ring material prepared in the example has moderate hardness, superior toughness and tear resistance, and in particular, the permanent deformation and creep are significantly reduced, resulting in more stable sealing performance.
[0037] In the description of this specification, the references to terms such as "an embodiment," "example," "specific example," etc., indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of the present invention. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples.
[0038] The above description is merely an example and illustration of the present invention. Those skilled in the art can make various modifications or additions to the specific embodiments described, or use similar methods to replace them, as long as they do not deviate from the invention or exceed the scope defined in the claims, all of which should fall within the protection scope of the present invention.
Claims
1. A sealing ring material, characterized in that, The product comprises, by weight, 100 parts of nitrile rubber, 15-20 parts of chloroprene rubber, 10-15 parts of CNT composite reinforcing agent, 12-17 parts of reinforcing filler, 1.9-2.3 parts of vulcanizing agent, 1-1.4 parts of accelerator, 2-3 parts of antioxidant and 2.2-2.8 parts of anti-sticking agent; The CNT composite reinforcing agent is prepared by the following steps: Step A1: premix diallylamine, benzoyl peroxide and acetone, protect with nitrogen, heat to 30-55°C, stir and assist with 120-200W / m 2 UV irradiation, slowly add alkyl mercaptan, react for 2.5-4h, add sodium sulfite to quench, remove acetone by rotary evaporation, wash the substrate with water and dry to obtain intermediate 1, wherein the feed ratio of diallylamine, alkyl mercaptan, benzoyl peroxide and acetone is 0.1mol:0.2mol:0.07-0.11g:60-120mL, and the alkyl mercaptan is selected from one of n-octyl mercaptan, n-tetradecyl mercaptan and n-octadecyl mercaptan; Step A2: Premix intermediate 1, potassium carbonate, 15-crown ether-5 and tetrahydrofuran, preheat to 30-40℃, stir and intermittently add allyl iodine and react for 2.5-4h, then continue to heat to 55-65℃ and react for 1-1.5h. After the reaction is completed, remove tetrahydrofuran by rotary evaporation, wash the substrate with water and dry to obtain intermediate 2. The feed ratio of intermediate 1, allyl iodine, potassium carbonate, 15-crown ether-5 and tetrahydrofuran is 0.1mol:0.1mol:0.5-0.8g:6-10mL:100-170mL. Step A3: Mix intermediate 2,3-chloropropyltrimethoxysilane, potassium iodide, hydroquinone, and dioxane, heat to 90-100℃, stir and reflux for 20-30 hours, and remove dioxane by rotary evaporation under reduced pressure after the reaction is completed to obtain the modifier. The feed ratio of intermediate 2,3-chloropropyltrimethoxysilane, potassium iodide, hydroquinone, and dioxane is 0.1mol:0.105-0.11mol:0.9-1.4g:40-60mg:150-240mL. Step A4: Mix the modifier, dimethylacetamide, ethanol and deionized water, adjust the pH to 2-3 with hydrochloric acid, add carbon nanotubes and ultrasonically disperse, stir for 3-4 hours, then neutralize with ammonia water, let stand for 24 hours, take the precipitate, wash with water and dry to obtain CNT composite reinforcing agent. The feeding ratio of carbon nanotubes, modifier, dimethylacetamide, ethanol and deionized water is 10g:0.6-0.8g:10-15mL:10-20mL:15-25mL.
2. The sealing ring material according to claim 1, characterized in that, The vulcanizing agent is sulfur, and the accelerator is a compound of zinc oxide and tetrabenzylthiuram disulfide.
3. A method for preparing the sealing ring material according to claim 2, characterized in that, Specifically, the process involves mixing nitrile rubber and chloroprene rubber and then rolling them onto rollers. Accelerators, antioxidants, and anti-sticking agents are added for a first mixing process. CNT composite reinforcing agents and reinforcing fillers are then added for a second mixing process. Finally, vulcanizing agents are added and the mixture is sheeted to obtain the sealing ring material.
Citation Information
Patent Citations
Amino-modified and thiol-group-modified magnetic carbon nanotube composite material and preparation method thereof
CN104399431A
Preparation process for improving bonding capacity of carbon nanotube with rubber molecule
CN1803939A