CN116278245B - 一种预制型橡胶跑道卷材及其制备方法 - Google Patents
一种预制型橡胶跑道卷材及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种预制型橡胶跑道卷材及其制备方法,属于橡胶复合材料技术领域。该跑道卷材由冲突面层、粘结层和抗蠕变减震底层组成,抗蠕变减震底层按照重量份计包括:三元乙丙橡胶80‑100份、丁苯橡胶30‑40份、乙烯‑醋酸乙烯酯橡胶15‑20份、促交联纤维8‑13份、补强剂5‑7份、填料15‑22份、硫化剂1.4‑1.9份、促进剂0.6‑0.8份、润滑剂1.5‑2份、防焦剂0.3‑0.4份和防老剂0.5‑0.6份;促交联纤维表面改性有过氧化物修饰,共热过程中优先在碳纤维的近层形成致密且无交联链的交联层,充分发挥碳纤维高模量特点,从而使得底层材料不易出现蠕变变形,使得跑道材料易于同跑道地基贴合。
Description
技术领域
本发明属于橡胶复合材料技术领域,具体地,涉及一种预制型橡胶跑道卷材及其制备方法。
背景技术
塑胶跑道具有平整度好、抗压强度高、硬度弹性适当、物理性能稳定的特性,有利于运动员速度和技术的发挥,有效地提高运动成绩,降低摔伤率。随着体育竞技行业的发展,塑胶跑道广泛铺设于各种体育馆所、田径场和其他室内外场地。
塑胶跑道一般包括缓冲底层、粘结层和面层,传统的塑胶跑道采用橡胶、沥青等为底层,聚氨酯、橡胶以及耐磨颗粒为面层,通过层层浇铸而成,施工难度大、周期长且造成污染物释放,因此,现有技术一般采用预制塑胶跑道,将塑胶跑道制成卷材,现场铺设即可;但是,预制塑胶跑道在放卷后易出现翘曲、变形等问题,导致塑胶跑道与地基不能紧密贴合,通常需要人工压制并配合加热矫形,大大增加施工难度;在长期试验研究中发现,导致塑胶跑道变形的主要原因为用于跑道底层的橡胶基材料在长期积压或者摆放不规范情况下出现蠕变,为应对橡胶材料的蠕变问题,现有的技术方案主要是向橡胶中混入一定的量的填料,如炭黑、碳纤维、玄武岩纤维等,对于塑胶跑道底层材料而言,为保证卷材的韧性,一般填料的用量不能过大,而填料用量少又难以提升耐蠕变性能,使得塑胶跑道的蠕变问题成为行业内的难点;因此,本申请基于解决跑道底层材料的蠕变问题,提供一种预制型橡胶跑道卷材及其制备方法。
发明内容
为了解决背景技术中提到的技术问题,本发明的目的在于提供一种预制型橡胶跑道卷材及其制备方法。
本发明的目的可以通过以下技术方案实现:
一种预制型橡胶跑道卷材,包括冲突面层和抗蠕变减震底层,两者通过聚氨酯胶黏剂粘合。
所述抗蠕变减震底层按照重量份计包括:三元乙丙橡胶80-100份、丁苯橡胶30-40份、乙烯-醋酸乙烯酯橡胶15-20份、促交联纤维8-13份、补强剂5-7份、填料15-22份、硫化剂1.4-1.9份、促进剂0.6-0.8份、润滑剂1.5-2份、防焦剂0.3-0.4份和防老剂0.5-0.6份。
所述促交联纤维由以下方法制备:
步骤A1:将短切碳纤维和硝酸溶液混合并超声震荡活化处理,离心浓缩后用去离子水调节pH值为3-4,加入烯丙基三乙氧基硅烷,升温至50-60℃搅拌水解1.2-1.5h,之后加入氨水调节pH为中性,静置偶联12h,取底层沉淀洗涤干燥,得到偶联纤维;
进一步地,短切碳纤维和烯丙基三乙氧基硅烷的用量比为100g:8-12mL,硝酸溶液的质量分数为28-35%。
步骤A2:将硫代水杨酸在氮气保护下溶于冰醋酸,加入偶联纤维和二甲基苯基膦,升温至65-75℃,辅以紫外辐照,搅拌反应3.5-4h,反应结束过滤取滤饼洗涤干燥,得到改性基体;
进一步地,偶联纤维、硫代水杨酸和二甲基苯基膦的用量比为100g:4.7-5.5g:0.1-0.15mL,紫外辐照功率为400-500W。
步骤A3:将苯甲酸溶于二甲基亚砜,加入改性基体超声分散,再加入氯化亚砜,升温至75-80℃回流3-3.5h,旋蒸脱除过量的氯化亚砜,再置于冰水浴中在5-10℃恒温,加入氢氧化钠搅拌分散,高速搅拌下缓慢滴加过氧化氢的二甲基亚砜分散液,控制加入反应时间1.4-1.8h,反应结束过滤取滤饼洗涤沥干,得到促交联纤维。
进一步地,改性基体、苯甲酸、氯化亚砜、氢氧化钠和过氧化氢的用量比为100g:3.5-4.2g:12-16mL:5-7g:2.2-2.8mL,过氧化氢的二甲基亚砜分散液中过氧化氢的质量分数为10-15%。
所述抗蠕变减震底层的制备方法,包括如下步骤:
步骤B1:将三元乙丙橡胶、丁苯橡胶、乙烯-醋酸乙烯酯橡胶、润滑剂、防焦剂和防老剂混合投料,升温至100-110℃,密炼9-12min,再加入促交联纤维、补强剂、填料和促进剂,继续密炼2-3min,排胶得到混炼胶;
步骤B2:将混炼胶转至开炼机中,加胶包辊,加入硫化剂并薄通3-4次,下片模压定型,得到坯件;
步骤B3:将坯件置于硫化机中,控制硫化温度为155-170℃,硫化时间为1.9-2.4h,冷却后得到抗蠕变减震底层。
进一步地,硫化剂选自硫磺,促进剂选自TMTD。
一种预制型橡胶跑道卷材的制备方法为:在抗蠕变减震底层的粘接面刷涂聚氨酯胶黏剂,贴合冲突面层,在2.5-3MPa下持压压合3-5min,自然静置固化24h,下料收卷,得到预制型橡胶跑道卷材。
本发明的有益效果:
本发明的跑道卷材为复合结构,其底层以三元乙丙橡胶为主材,在微观结构上,三元乙丙橡胶的主链为饱和碳链,仅在侧链上具有不饱和烯烃结构,将其与丁苯橡胶共混交联,形成部分呈现土工格室结构的交联网络,且连接点引入刚性结构苯环,不易出现永久形变;
另外,在复合橡胶材料中引入一种促交联纤维,其以高模量的碳纤维为基体,通过烯丙基三乙氧基硅烷的偶联作用在表面引入双键修饰,再以硫代水杨酸在水热条件和紫外引发下与接枝的双键点击加成,引入苯甲酸结构,最后通过氧化处理形成表层过氧化物修饰,促交联纤维在与橡胶共热过程中优先裂解,形成大量自由基,夺取橡胶分子链上的活泼氢进行交联反应,优先在碳纤维的近层形成致密且无交联链的交联结构,该种交联结构键能高且均匀,不易产生联结点重排、错位和互锁,具有优异的耐形变性能,再者,致密的橡胶交联层包覆结构提高碳纤维与橡胶基体的结合能力,充分发挥碳纤维高模量特点,从而使得底层材料不易出现蠕变变形,使得跑道材料易于同跑道地基贴合。
具体实施方式
下面将结合本发明实施例,对本发明实施例中的技术方案进行清楚、完整的描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其它实施例,都属于本发明保护的范围。
以下实施例中所采用的原料公开如下:
短切碳纤维,选自PAN基碳纤维,长度为0.2mm,由上海力硕复合材料科技有限公司提供,型号为LSCF0.2-S;
三元乙丙橡胶,由广州得高新材料有限公司提供,型号为K TER 6537;
丁苯橡胶,由广州得高新材料有限公司提供,型号为SSBR-SOL 1205;
乙烯-醋酸乙烯酯橡胶,由东莞市尚君塑胶原料有限公司提供,型号为700H;
补强剂,选自高活性氧化锌,由广州市力本橡胶原料贸易有限公司提供,细度为200目;
填料,选自重质碳酸钙,由石家庄华朗矿产品贸易有限公司提供,细度为325目;
硫化剂,选自橡胶专用硫磺,由河南雷默化工产品有限公司提供,细度为400目;
促进剂,选自促进剂TMTD,由济南骏腾化工有限公司提供;
润滑剂,选自硬脂酸,由东莞市厚达化工有限公司提供,型号为SA-1801;
防焦剂,由青岛鸿运金新材料有限公司提供,型号为HYJ-012;
防老剂,选自防老剂MB,由石家庄品佰化工科技有限公司提供。
实施例1
本实施例制备一种预制型橡胶跑道卷材,具体实施过程如下:
1)制备促交联纤维
1.1、取短切碳纤维和质量分数为35%的硝酸溶液按照固液质量比为1:5混合,施加40kHz超声分散20min,离心取底层沉淀浓缩,去除部分上清液,并加入去离子水调节pH值为3,再加入烯丙基三乙氧基硅烷,升温至60℃,辅以180rpm机械搅拌,水解处理1.2h,水解后加入氨水直至反应液的pH为中性,静置偶联12h,其中,短切碳纤维和烯丙基三乙氧基硅烷的用量比为100g:12mL,偶联后取底层沉淀用乙醇洗涤干燥,制得偶联纤维。
1.2、取硫代水杨酸在氮气保护下投料,加入冰醋酸搅拌至完全溶解,再加入偶联纤维和二甲基苯基膦,升温至75℃,采用UVA紫外灯管辅以500W紫外辐照,同时施加240rpm搅拌反应3.5h,其中,偶联纤维、硫代水杨酸和二甲基苯基膦的用量比为100g:5.5g:0.15mL,反应结束过滤取滤饼用水洗涤干燥,制得改性基体。
1.3、取苯甲酸投料,加入二甲基亚砜搅拌混溶,再加入改性基体以40kHz超声分散5min形成悬浊液,再向悬浊液中加入氯化亚砜,辅以420rpm机械搅拌,升温至80℃回流3h,回流结束旋蒸脱除过量的氯化亚砜,冷却并置于冰水浴中在5-10℃恒温,加入氢氧化钠粉末搅拌分散,提升转速为1000rpm高速搅拌搅拌,取过氧化氢搅拌分散在二甲基亚砜中,控制过氧化氢的质量分数为15%,再将过氧化氢的二甲基亚砜分散液在40min内滴加到反应液中,完全滴加后继续保温搅拌反应,控制过氧化氢的二甲基亚砜分散液的总加入反应时间为1.4h,其中,改性基体、苯甲酸、氯化亚砜、氢氧化钠和过氧化氢的用量比为100g:4.2g:16mL:7g:2.8mL,反应结束过滤取滤饼,用水洗涤、沥干,制得促交联纤维。
2)制备跑道卷材的抗蠕变减震底层
2.1、按照重量份配比计取如下原料:
三元乙丙橡胶90份、丁苯橡胶30份、乙烯-醋酸乙烯酯橡胶20份、促交联纤维8份、补强剂7份、填料22份、硫化剂1.4份、促进剂0.6份、润滑剂1.8份、防焦剂0.3份和防老剂0.5份;
2.2、将三元乙丙橡胶、丁苯橡胶、乙烯-醋酸乙烯酯橡胶、润滑剂、防焦剂和防老剂混合投料,升温至110℃,设置搅拌速率为70rpm,密炼9min,之后加入促交联纤维、补强剂、填料和促进剂,继续密炼2min,排胶制得混炼胶。
2.3、将混炼胶转至开炼机中加胶包辊,加入硫化剂并薄通4次,下片置于模具中模压成型,冷却脱模,制得坯件。
2.4、将坯件置于硫化机中,设置硫化温度为170℃,硫化时间为1.9h,冷却后得到抗蠕变减震底层。
3)制备预制型橡胶跑道卷材
将抗蠕变减震底层的粘接面上刷涂聚氨酯胶黏剂(VoramerTM MR 1045L,以下实施例相同),再将冲突面层的粘接面贴合在胶黏剂层表面,送入压合机,在3MPa下持压压合3min,释压静置固化24h,下料收卷,制得预制型橡胶跑道卷材。
实施例2
本实施例制备一种预制型橡胶跑道卷材,具体实施过程如下:
1)制备促交联纤维
1.1、取短切碳纤维和质量分数为28%的硝酸溶液按照固液质量比为1:6混合,施加40kHz超声分散30min,离心取底层沉淀浓缩,去除部分上清液,并加入去离子水调节pH值为4,再加入烯丙基三乙氧基硅烷,升温至50℃,辅以180rpm机械搅拌,水解处理1.5h,水解后加入氨水直至反应液的pH为中性,静置偶联12h,其中,短切碳纤维和烯丙基三乙氧基硅烷的用量比为100g:8mL,偶联后取底层沉淀用乙醇洗涤干燥,制得偶联纤维。
1.2、取硫代水杨酸在氮气保护下投料,加入冰醋酸搅拌至完全溶解,再加入偶联纤维和二甲基苯基膦,升温至65℃,采用UVA紫外灯管辅以400W紫外辐照,同时施加180rpm搅拌反应4h,其中,偶联纤维、硫代水杨酸和二甲基苯基膦的用量比为100g:4.7g:0.1mL,反应结束过滤取滤饼用水洗涤干燥,制得改性基体。
1.3、取苯甲酸投料,加入二甲基亚砜搅拌混溶,再加入改性基体以40kHz超声分散5min形成悬浊液,再向悬浊液中加入氯化亚砜,辅以420rpm机械搅拌,升温至75℃回流3.5h,回流结束旋蒸脱除过量的氯化亚砜,冷却并置于冰水浴中在5-10℃恒温,加入氢氧化钠粉末搅拌分散,提升转速为800rpm高速搅拌搅拌,取过氧化氢搅拌分散在二甲基亚砜中,控制过氧化氢的质量分数为10%,再将过氧化氢的二甲基亚砜分散液在50min内滴加到反应液中,完全滴加后继续保温搅拌反应,控制过氧化氢的二甲基亚砜分散液的总加入反应时间为1.8h,其中,改性基体、苯甲酸、氯化亚砜、氢氧化钠和过氧化氢的用量比为100g:3.5g:12mL:5g:2.2mL,反应结束过滤取滤饼,用水洗涤、沥干,制得促交联纤维。
2)制备跑道卷材的抗蠕变减震底层
2.1、按照重量份配比计取如下原料:
三元乙丙橡胶80份、丁苯橡胶40份、乙烯-醋酸乙烯酯橡胶15份、促交联纤维13份、补强剂5份、填料15份、硫化剂1.9份、促进剂0.8份、润滑剂1.5份、防焦剂0.4份和防老剂0.6份;
2.2、将三元乙丙橡胶、丁苯橡胶、乙烯-醋酸乙烯酯橡胶、润滑剂、防焦剂和防老剂混合投料,升温至110℃,设置搅拌速率为70rpm,密炼10min,之后加入促交联纤维、补强剂、填料和促进剂,继续密炼2min,排胶制得混炼胶。
2.3、将混炼胶转至开炼机中加胶包辊,加入硫化剂并薄通4次,下片置于模具中模压成型,冷却脱模,制得坯件。
2.4、将坯件置于硫化机中,设置硫化温度为160℃,硫化时间为2.1h,冷却后得到抗蠕变减震底层。
3)制备预制型橡胶跑道卷材
将抗蠕变减震底层的粘接面上刷涂聚氨酯胶黏剂,再将冲突面层的粘接面贴合在胶黏剂层表面,送入压合机,在2.5MPa下持压压合5min,释压静置固化24h,下料收卷,制得预制型橡胶跑道卷材。
实施例3
本实施例制备一种预制型橡胶跑道卷材,具体实施过程如下:
1)制备促交联纤维
1.1、取短切碳纤维和质量分数为32%的硝酸溶液按照固液质量比为1:5混合,施加40kHz超声分散30min,离心取底层沉淀浓缩,去除部分上清液,并加入去离子水调节pH值为3,再加入烯丙基三乙氧基硅烷,升温至55℃,辅以180rpm机械搅拌,水解处理1.4h,水解后加入氨水直至反应液的pH为中性,静置偶联12h,其中,短切碳纤维和烯丙基三乙氧基硅烷的用量比为100g:11mL,偶联后取底层沉淀用乙醇洗涤干燥,制得偶联纤维。
1.2、取硫代水杨酸在氮气保护下投料,加入冰醋酸搅拌至完全溶解,再加入偶联纤维和二甲基苯基膦,升温至72℃,采用UVA紫外灯管辅以460W紫外辐照,同时施加240rpm搅拌反应3.8h,其中,偶联纤维、硫代水杨酸和二甲基苯基膦的用量比为100g:5.0g:0.12mL,反应结束过滤取滤饼用水洗涤干燥,制得改性基体。
1.3、取苯甲酸投料,加入二甲基亚砜搅拌混溶,再加入改性基体以40kHz超声分散5min形成悬浊液,再向悬浊液中加入氯化亚砜,辅以420rpm机械搅拌,升温至80℃回流3.2h,回流结束旋蒸脱除过量的氯化亚砜,冷却并置于冰水浴中在5-10℃恒温,加入氢氧化钠粉末搅拌分散,提升转速为1000rpm高速搅拌搅拌,取过氧化氢搅拌分散在二甲基亚砜中,控制过氧化氢的质量分数为15%,再将过氧化氢的二甲基亚砜分散液在50min内滴加到反应液中,完全滴加后继续保温搅拌反应,控制过氧化氢的二甲基亚砜分散液的总加入反应时间为1.6h,其中,改性基体、苯甲酸、氯化亚砜、氢氧化钠和过氧化氢的用量比为100g:3.9g:15mL:6g:2.5mL,反应结束过滤取滤饼,用水洗涤、沥干,制得促交联纤维。
2)制备跑道卷材的抗蠕变减震底层
2.1、按照重量份配比计取如下原料:
三元乙丙橡胶100份、丁苯橡胶32份、乙烯-醋酸乙烯酯橡胶18份、促交联纤维11份、补强剂6份、填料20份、硫化剂1.7份、促进剂0.7份、润滑剂2份、防焦剂0.3份和防老剂0.5份;
2.2、将三元乙丙橡胶、丁苯橡胶、乙烯-醋酸乙烯酯橡胶、润滑剂、防焦剂和防老剂混合投料,升温至100℃,设置搅拌速率为60rpm,密炼12min,之后加入促交联纤维、补强剂、填料和促进剂,继续密炼3min,排胶制得混炼胶。
2.3、将混炼胶转至开炼机中加胶包辊,加入硫化剂并薄通3次,下片置于模具中模压成型,冷却脱模,制得坯件。
2.4、将坯件置于硫化机中,设置硫化温度为155℃,硫化时间为2.4h,冷却后得到抗蠕变减震底层。
3)制备预制型橡胶跑道卷材
将抗蠕变减震底层的粘接面上刷涂聚氨酯胶黏剂,再将冲突面层的粘接面贴合在胶黏剂层表面,送入压合机,在2.5MPa下持压压合5min,释压静置固化24h,下料收卷,制得预制型橡胶跑道卷材。
对比例
本对比例与实施例3的实施过程相同,将抗蠕变减震底层原料中的促交联纤维替换为相同重量实施例3制备的偶联纤维,将硫磺剂的用量替换为1.7份,其余完全相同。
为了便于测试,将实施例1-实施例3以及对比例的下片料模压成直径为29mm,厚度为12.5mm的圆柱状坯件,再硫化成型,制成试样,参照GB/T19242-2003标准,采用EPLEXOR-500N型动态力学性能频谱仪随试样进行静态压缩蠕变测试,载荷均为50N,测试时间为24h,测试温度分别为0℃、25℃、50℃,具体测试数据如表1所示:
表1
由表1数据可知,本发明制备的预制型橡胶跑道卷材,其抗蠕变减震底层具有良好的耐蠕变性能,特别在50℃高温下,蠕变量仅有0.22-0.29%,远低于现有的碳纤维增强型复合材料。
基于以上测试数据,对实施例1-实施例3制备的抗蠕变减震底层进行使用性能测试,具体测试数据如表2所示:
表2
由表2数据可知,本发明制备的抗蠕变减震底层符合现有塑胶跑道基体材料的技术指标,具有良好的综合性能,适用于塑胶跑道的材料。
在说明书的描述中,参考术语“一个实施例”、“示例”、“具体示例”等的描述意指结合该实施例或示例描述的具体特征、结构、材料或者特点包含于本发明的至少一个实施例或示例中。在本说明书中,对上述术语的示意性表述不一定指的是相同的实施例或示例。而且,描述的具体特征、结构、材料或者特点可以在任何的一个或多个实施例或示例中以合适的方式结合。
以上内容仅仅是对本发明所作的举例和说明,所属本技术领域的技术人员对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代,只要不偏离本发明所定义的范围,均应属于本发明的保护范围。
Claims (6)
1.一种预制型橡胶跑道卷材,包括冲突面层、粘结层和抗蠕变减震底层,其特征在于,抗蠕变减震底层按照重量份计包括:三元乙丙橡胶80-100份、丁苯橡胶30-40份、乙烯-醋酸乙烯酯橡胶15-20份、促交联纤维8-13份、补强剂5-7份、填料15-22份、硫化剂1.4-1.9份、促进剂0.6-0.8份、润滑剂1.5-2份、防焦剂0.3-0.4份和防老剂0.5-0.6份;
所述促交联纤维由以下方法制备:
步骤A1:将短切碳纤维和硝酸溶液混合并超声震荡活化处理,离心浓缩后用去离子水调节pH值为3-4,加入烯丙基三乙氧基硅烷,升温至50-60℃搅拌水解1.2-1.5h,之后加入氨水调节pH为中性,静置偶联12h,取底层沉淀洗涤干燥,得到偶联纤维;
步骤A2:将硫代水杨酸在氮气保护下溶于冰醋酸,加入偶联纤维和二甲基苯基膦,升温至65-75℃,辅以紫外辐照,搅拌反应3.5-4h,反应结束过滤取滤饼洗涤干燥,得到改性基体;
步骤A3:将苯甲酸溶于二甲基亚砜,加入改性基体超声分散,再加入氯化亚砜,升温至75-80℃回流3-3.5h,旋蒸脱除氯化亚砜,再置于冰水浴中在5-10℃恒温,加入氢氧化钠搅拌分散,高速搅拌下缓慢滴加过氧化氢的二甲基亚砜分散液,控制加入反应时间1.4-1.8h,反应结束过滤取滤饼洗涤沥干,得到促交联纤维;
所述抗蠕变减震底层由以下方法制备:
步骤B1:将三元乙丙橡胶、丁苯橡胶、乙烯-醋酸乙烯酯橡胶、润滑剂、防焦剂和防老剂混合投料,在100-110℃密炼9-12min,再加入促交联纤维、补强剂、填料和促进剂继续密炼2-3min,得到混炼胶;
步骤B2:将混炼胶转至开炼机中加胶包辊,加入硫化剂薄通3-4次,下片模压定型,得到坯件;
步骤B3:将坯件置于硫化机中,控制硫化温度为155-170℃,硫化时间为1.9-2.4h,冷却后得到抗蠕变减震底层。
2.根据权利要求1所述的一种预制型橡胶跑道卷材,其特征在于,短切碳纤维和烯丙基三乙氧基硅烷的用量比为100g:8-12mL,硝酸溶液的质量分数为28-35%。
3.根据权利要求2所述的一种预制型橡胶跑道卷材,其特征在于,偶联纤维、硫代水杨酸和二甲基苯基膦的用量比为100g:4.7-5.5g:0.1-0.15mL,紫外辐照功率为400-500W。
4.根据权利要求3所述的一种预制型橡胶跑道卷材,其特征在于,改性基体、苯甲酸、氯化亚砜、氢氧化钠和过氧化氢的用量比为100g:3.5-4.2g:12-16mL:5-7g:2.2-2.8mL,过氧化氢的二甲基亚砜分散液中过氧化氢的质量分数为10-15%。
5.根据权利要求1所述的一种预制型橡胶跑道卷材,其特征在于,硫化剂为硫磺,促进剂为TMTD。
6.一种如权利要求1-5任一项所述的一种预制型橡胶跑道卷材的制备方法,其特征在于,具体方法为:在抗蠕变减震底层的粘接面刷涂聚氨酯胶黏剂,贴合冲突面层,在2.5-3MPa下持压压合3-5min,自然静置固化24h,下料收卷,得到预制型橡胶跑道卷材。
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