CN109503901A - 一种推进剂混合机专用导静电橡胶及制备方法 - Google Patents
一种推进剂混合机专用导静电橡胶及制备方法 Download PDFInfo
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Abstract
本发明公开了一种推进剂混合机专用导静电橡胶配方及制备方法,该橡胶配方的基体橡胶为丁腈4155,包括硫化剂、硫化活化剂、硫化促进剂,增塑剂、防老剂、导电填料;制作工艺采用双辊开放式炼胶机,通过控制不同的辊距、辊通水温、混炼时间以及加料顺序,能够生产出适用推进剂混合机生产,且橡胶表面电阻值、硬度、抗拉强度、断裂伸长率、密度以及工艺性能的专用导静电橡胶材料。采用本发明的导静电橡胶性能试样制备方法所制备的试样,可有效用于本发明的导静电橡胶的电阻值、力学性能、硬度、密度等性能的测试和预示。
Description
技术领域
本发明涉及固体推进剂制造领域,具体涉及固体推进剂混合过程采用导静电材料。
背景技术
目前,国内绝大多数固体推进剂生产厂家已采用立式混合机进行推进剂混合,其中AP、RDX和HMX等含能材料的加料过程是通过导料槽被自动送入混合机的混合锅内。混合加料时,在混合锅的上部存在这几种组分的粉尘混合物,由于在推进剂料浆中还存在其他易挥发组分,因此在混合锅内形成了多元多相的爆炸危险物。物料与导料槽分离的瞬间将产生静电,当静电荷积累到一定程度时,会出现火花放电,可能激发粉尘及其他易挥发组分混合物着火,进而引起大量推进剂的燃烧或爆炸。
导静电橡胶作为复合导电高分子材料的一种,是以橡胶弹性体为基体添加导电填料制备而成,既保留了基体橡胶的弹性,又具有导电填料的导电性。在固体推进剂混合加料系统中用导静电橡胶代替绝缘橡胶,可提高加料系统表面的导电性,降低静电危险性,起到静电防护的作用。在导静电橡胶材料的选择上,能够工艺要求的主要指标有,表面电阻值≤1.0×104Ω,质地柔软,邵氏硬度≤60°。目前市场上的导静电橡胶表面电阻值标准大多要求≤5×104Ω,邵氏硬度60~75°,其中相对性能较优的HG2949-1999导静电橡胶,经检测表面电阻值能够满足≤1.0×104Ω要求,但邵氏硬度大多超过65°。
发明内容
为满足固体推进剂混合生产工艺要求,本发明通过优选硬度小的导静电橡胶基体橡胶、合理优化导电填料配比、加大软化剂配比、改善混炼工艺性能、优化硫化成型工艺,添加与目前导静电橡胶相同的固体填料、活化剂、硫化体系及防老剂,通过制作试样并测试表面电阻值,保证导静电橡胶导电性能满足目前推进剂生产使用指标,根据力学性能、硬度、密度等性能测试结果,制作出邵氏硬度≤60°、质地柔软、表面电阻值≤1.0×104Ω,且综合性能优异的导静电橡胶配方。该导静电橡胶硫化成型后用于推进剂混合加料系统满足工艺要求。
本发明采用的具体技术方案如下:
一、推进剂混合机专用导静电橡胶配方
基体橡胶为丁腈4155,包括硫化剂、硫化活化剂、硫化促进剂,增塑剂、防老剂、导电填料。
配方质量份数为:基体橡胶,100;硫化剂,1.0~1.8;硫化活化剂,1.5~2.5;硫化促进剂,1.5~2.3;增塑剂,15~25;防老剂,3~5;导电填料,15~35。
上述硫化剂为硫磺或过氧化二异丙苯或过氧化铅,硫化活化剂为硬脂酸和氧化锌,硫化促进剂为促进剂DM或促进剂TMTD或促进剂CZ,增塑剂为邻苯二甲酸二丁酯或邻苯二甲酸二辛脂或磷酸三甲苯酯,防老剂为防老剂D或防老剂RD或防老剂BL,导电填料为导电炭黑和乙炔炭黑。硫化活化剂中硬脂酸和氧化锌的配方质量份数可分别为0.5~2和1.0~2.5。导电填料中导电炭黑和乙炔炭黑的配方质量份数可分别为10~20和5~15。
二、推进剂混合机专用导静电橡胶制备
该推进剂混合机专用导静电橡胶制备,包括三个制备工艺方法:
工艺方法1,一种推进剂混合机专用导静电橡胶制备方法,由以下步骤完成:
步骤一,采用双辊开放式炼胶机,辊距≤0.5mm, 辊通水温30℃~40℃ , 将丁腈4155基体橡胶100份加入炼胶机,塑炼时间≥1min;
步骤二,辊距逐步放大至2 mm~5 mm, 辊通水温30℃~40℃ ,缓慢加入硫化促进剂,混炼时间≥2min;
步骤三,辊距2 mm~5 mm, 辊通水温30℃~40℃ ,缓慢加入硫化活化剂、防老剂,混炼时间≥3min;
步骤四,辊距2 mm~5 mm, 辊通水温30℃~40℃ ,缓慢加入导电填料、增塑剂,混炼≥30min;
步骤五,辊距2 mm~5 mm, 辊通水温30℃~40℃ ,缓慢加入硫化剂,混炼时间≥3min;
步骤六,辊距2 mm~5 mm, 辊通水温30℃~40℃ ,切割薄通,薄通次数不少于10次,混炼时间≥20min;
步骤七,出片。
工艺方法2,一种推进剂混合机专用导静电橡胶配方制备方法,由以下步骤完成:
步骤一,采用双辊开放式炼胶机,辊距≤0.5mm, 辊通水温30℃~40℃ , 将丁腈4155基体橡胶100份加入炼胶机,塑炼时间≥1min;
步骤二,辊距逐步放大至2 mm~5 mm, 辊通水温30℃~40℃ ,缓慢加入硫化促进剂,混炼时间≥2min;
步骤三,辊距2 mm~5 mm, 辊通水温30℃~40℃ ,缓慢加入硫化活化剂、防老剂,混炼时间≥3min;
步骤四,辊距2 mm~5 mm, 辊通水温30℃~40℃ ,缓慢交替加入导电填料中的导电炭黑、乙炔炭黑和增塑剂,混炼≥30min;
步骤五,辊距2 mm~5 mm, 辊通水温30℃~40℃ ,缓慢加入硫化剂,混炼时间≥3min;
步骤六,辊距2 mm~5 mm, 辊通水温30℃~40℃ ,切割薄通,薄通次数不少于10次,混炼时间≥20min;
步骤七,出片。
工艺方法3,一种推进剂混合机专用导静电橡胶配方制备方法,由以下步骤完成:
步骤一,采用双辊开放式炼胶机,辊距≤0.5mm, 辊通水温30℃~40℃ , 将丁腈4155基体橡胶100份加入炼胶机,塑炼时间1min;
步骤二,辊距逐步放大至2 mm~5 mm, 辊通水温30℃~40℃ ,缓慢加入硫化促进剂,混炼时间2min;
步骤三,辊距2 mm~5 mm, 辊通水温30℃~40℃ ,缓慢加入硫化活化剂、防老剂,混炼时间3 min~5min;
步骤四,辊距2 mm~5 mm, 辊通水温30℃~40℃ ,缓慢交替加入导电填料中的导电炭黑、乙炔炭黑和增塑剂,混炼30min;
步骤五,辊距2 mm~5 mm, 辊通水温30℃~40℃ ,缓慢加入硫化剂,混炼时间3min;
步骤六,辊距2 mm~5 mm, 辊通水温30℃~40℃ ,切割薄通,薄通次数不少于10次,混炼时间20 min~30min;
步骤七,出片。
四、推进剂混合机专用导静电橡胶配方所制备的性能试样的制备方法
该推进剂混合机专用导静电橡胶配方所制备的性能试样的制备方法,由以下步骤完成:
步骤一,采用力学试片模具制作成120mm×150 mm×2mm的力学试片;
步骤二,将硫化试片放入平板硫化机内,硫化温度150℃~160℃,硫化时间为60min~70 min,硫化压力为10MPa;
步骤三,硫化结束,降至室温后,用专用橡胶裁片刀将试片裁成标准试片尺寸。
五、导静电橡胶性能试样制备方法
为有效表征所制备的导静电橡胶力学性能和表面电阻值,需制备对应的性能试样,该橡胶性能试样制备方法,由以下步骤完成:
步骤一,采用力学片模具制作成120mm×150 mm×2mm的力学试片;
步骤二,将硫化试片放入平板硫化机内,硫化温度150℃~160℃,硫化时间为60min~70 min,硫化压力为10MPa;
步骤三,硫化结束,降至室温后,用专用橡胶裁片刀将试片裁成标准试片尺寸。
本发明的有益效果为:
本发明所制备的导静电橡胶表面电阻值≤1.0×104Ω,邵氏硬度≤60°,抗拉强度≥6MPa,断裂伸长率≥300%,密度≤1.25g/cm3,应用于固体推进剂混合加料系统上,测试静电电压低于静电电压安全界限,导静电效果良好。采用本发明的导静电橡胶性能试样制备方法所制备的试样,可有效用于本发明的导静电橡胶的电阻值、力学性能、硬度、密度等性能的测试和预示。
具体实施方式
实施例一,一种准用于混合机胶料系统静电防护的导静电橡胶,质量份数:
丁腈4155 100份,邻苯二甲酸二丁酯增塑剂15份,导电炭黑10份,乙炔炭黑5份,氧化锌1.0份,硬脂酸0.5份,促进剂DM1.5份,硫磺硫化剂1.0份,防老剂D 3份。采用工艺方法1,一种推进剂混合机专用导静电橡胶配方制备方法橡胶材料,采用上述导静电橡胶性能试样制备方法橡胶性能试样。制得的导静电胶板性能分别为:密度 1.10g/cm3,邵氏硬度52°,抗拉强度 17.9MPa,断裂伸长率 511%,表面电阻 4.52×103Ω。
实施例二,一种准用于混合机胶料系统静电防护的导静电橡胶,质量份数:
丁腈4155 100份,邻苯二甲酸二丁酯增塑剂20份,导电炭黑15份,乙炔炭黑10份,氧化锌1.5份,硬脂酸1份,促进剂DM 2.0份,硫磺硫化剂1.5份,防老剂D 4份。采用工艺方法1,一种推进剂混合机专用导静电橡胶配方制备方法橡胶材料,采用上述导静电橡胶性能试样制备方法橡胶性能试样。制得的导静电胶板性能分别为:密度 1.15g/cm3,邵氏硬度55°,抗拉强度 15.6MPa,断裂伸长率477%,表面电阻 1.57×103Ω。
实施例三,一种准用于混合机胶料系统静电防护的导静电橡胶,质量份数:
丁腈4155 100份,邻苯二甲酸二丁酯增塑剂25份,导电炭黑20份,乙炔炭黑10份,氧化锌2.5份,硬脂酸2份,促进剂DM 2.3份,硫磺硫化剂1.8份,防老剂D 5份。采用工艺方法2,一种推进剂混合机专用导静电橡胶配方制备方法橡胶材料,采用上述导静电橡胶性能试样制备方法橡胶性能试样。制得的导静电胶板性能分别为:密度 1.20g/cm3,邵氏硬度58°,抗拉强度 13.2MPa,断裂伸长率358%,表面电阻 1.05×103Ω。
实施例四,一种准用于混合机胶料系统静电防护的导静电橡胶,质量份数:
丁腈4155 100份,邻苯二甲酸二丁酯增塑剂15份,导电炭黑10份,乙炔炭黑10份,氧化锌1.0份,硬脂酸0.5份,促进剂DM 1.5份,硫磺硫化剂1.0份,防老剂D 3份。采用工艺方法2,一种推进剂混合机专用导静电橡胶配方制备方法橡胶材料,采用上述导静电橡胶性能试样制备方法橡胶性能试样。制得的导静电胶板性能分别为:密度 1.17g/cm3,邵氏硬度56°,抗拉强度 16.9MPa,断裂伸长率 498%,表面电阻 5.01×103Ω。
实施例五,一种准用于混合机胶料系统静电防护的导静电橡胶,质量份数:
丁腈4155 100份,邻苯二甲酸二丁酯增塑剂20份,导电炭黑10份,乙炔炭黑15份,氧化锌1.5份,硬脂酸1份,促进剂DM 2.0份,硫磺硫化剂1.5份,防老剂D 4份。采用工艺方法3,一种推进剂混合机专用导静电橡胶配方制备方法橡胶材料,采用上述导静电橡胶性能试样制备方法橡胶性能试样。制得的导静电胶板性能分别为:密度 1.21g/cm3,邵氏硬度57°,抗拉强度 13.2MPa,断裂伸长率457%,表面电阻4.13×103Ω。
实施例六,一种准用于混合机胶料系统静电防护的导静电橡胶,质量份数:
丁腈4155 100份,邻苯二甲酸二丁酯增塑剂25份,导电炭黑15份,乙炔炭黑15份,氧化锌2.5份,硬脂酸2份,促进剂DM 2.3份,硫磺硫化剂1.8份,防老剂D 5份。采用工艺方法3,一种推进剂混合机专用导静电橡胶配方制备方法橡胶材料,采用上述导静电橡胶性能试样制备方法橡胶性能试样。制得的导静电胶板性能分别为:密度 1.24g/cm3,邵氏硬度58°,抗拉强度11.12MPa,断裂伸长率358%,表面电阻 1.21×103Ω。
实施例七,一种准用于混合机胶料系统静电防护的导静电橡胶,质量份数:
丁腈4155 100份,邻苯二甲酸二辛脂增塑剂15份,导电炭黑10份,乙炔炭黑5份,氧化锌1.0份,硬脂酸0.5份,促进剂TMTD 1.5份,过氧化二异丙苯硫化剂1.0份,防老剂RD 3份。采用工艺方法2,一种推进剂混合机专用导静电橡胶配方制备方法橡胶材料,采用上述导静电橡胶性能试样制备方法橡胶性能试样。制得的导静电胶板性能分别为:密度 1.10g/cm3,邵氏硬度57°,抗拉强度 9.17MPa,断裂伸长率 327%,表面电阻 6.82×103Ω。
实施例八,一种准用于混合机胶料系统静电防护的导静电橡胶,质量份数:
丁腈4155 100份,磷酸三甲苯酯增塑剂15份,导电炭黑10份,乙炔炭黑5份,氧化锌1.0份,硬脂酸0.5份,促进剂CZ 1.5份,过氧化铅硫化剂1.0份,防老剂BL 3份。采用工艺方法3,一种推进剂混合机专用导静电橡胶配方制备方法橡胶材料,采用上述导静电橡胶性能试样制备方法橡胶性能试样。制得的导静电胶板性能分别为:密度 1.10g/cm3,邵氏硬度59°,抗拉强度 7.21MPa,断裂伸长率 311%,表面电阻 7.35×103Ω。
Claims (9)
1.一种推进剂混合机专用导静电橡胶,配方包括基体橡胶为丁腈4155,包括硫化剂、硫化活化剂、硫化促进剂,其特征在于,配方还包括增塑剂、防老剂、导电填料。
2.根据权利要求1所述的一种推进剂混合机专用导静电橡胶,其特征在于,其配方质量份数为:基体橡胶,100;硫化剂,1.0~1.8;硫化活化剂,1.5~2.5;硫化促进剂,1.5~2.3;增塑剂,15~25;防老剂,3~5;导电填料,15~35。
3.根据权利要求2所述的一种推进剂混合机专用导静电橡胶,其特征在于,配方中,硫化剂为硫磺或过氧化二异丙苯或过氧化铅,硫化活化剂为硬脂酸和氧化锌,硫化促进剂为促进剂DM或促进剂TMTD或促进剂CZ,增塑剂为邻苯二甲酸二丁酯或邻苯二甲酸二辛脂或磷酸三甲苯酯,防老剂为防老剂D或防老剂RD或防老剂BL,导电填料为导电炭黑和乙炔炭黑。
4.根据权利要求3所述的一种推进剂混合机专用导静电橡胶,其特征在于,配方中,硫化活化剂中硬脂酸和氧化锌的配方质量份数分别为0.5~2和1.0~2.5。
5.根据权利要求3或4所述的任一种推进剂混合机专用导静电橡胶配方,其特征在于,导电填料中导电炭黑和乙炔炭黑的配方质量份数分别为10~20和5~15。
6.一种采用权利要求1或2所述的任一种推进剂混合机专用导静电橡胶,其特征在于,所述专用导静电橡胶的制备方法由以下步骤完成:
步骤一,采用双辊开放式炼胶机,辊距≤0.5mm, 辊通水温30℃~40℃ , 将丁腈4155基体橡胶100份加入炼胶机,塑炼时间≥1min;
步骤二,辊距逐步放大至2 mm~5 mm, 辊通水温30℃~40℃ ,缓慢加入硫化促进剂,混炼时间≥2min;
步骤三,辊距2 mm~5 mm, 辊通水温30℃~40℃ ,缓慢加入硫化活化剂、防老剂,混炼时间≥3min;
步骤四,辊距2 mm~5 mm, 辊通水温30℃~40℃ ,缓慢加入导电填料、增塑剂,混炼≥30min;
步骤五,辊距2 mm~5 mm, 辊通水温30℃~40℃ ,缓慢加入硫化剂,混炼时间≥3min;
步骤六,辊距2 mm~5 mm, 辊通水温30℃~40℃ ,切割薄通,薄通次数不少于10次,混炼时间≥20min;
步骤七,出片。
7.一种采用权利要求3所述的一种推进剂混合机专用导静电橡胶,其特征在于,所述专用导静电橡胶制备方法由以下步骤完成:
步骤一,采用双辊开放式炼胶机,辊距≤0.5mm, 辊通水温30℃~40℃ , 将丁腈4155基体橡胶100份加入炼胶机,塑炼时间≥1min;
步骤二,辊距逐步放大至2 mm~5 mm, 辊通水温30℃~40℃ ,缓慢加入硫化促进剂,混炼时间≥2min;
步骤三,辊距2 mm~5 mm, 辊通水温30℃~40℃ ,缓慢加入硫化活化剂、防老剂,混炼时间≥3min;
步骤四,辊距2 mm~5 mm, 辊通水温30℃~40℃ ,缓慢交替加入导电填料中的导电炭黑、乙炔炭黑和增塑剂,混炼≥30min;
步骤五,辊距2 mm~5 mm, 辊通水温30℃~40℃ ,缓慢加入硫化剂,混炼时间≥3min;
步骤六,辊距2 mm~5 mm, 辊通水温30℃~40℃ ,切割薄通,薄通次数不少于10次,混炼时间≥20min;
步骤七,出片。
8.一种采用权利要求7所述的一种推进剂混合机专用导静电橡胶,其特征在于,所述专用导静电橡胶的制备方法由以下步骤完成:
步骤一,采用双辊开放式炼胶机,辊距≤0.5mm, 辊通水温30℃~40℃ , 将丁腈4155基体橡胶100份加入炼胶机,塑炼时间1min;
步骤二,辊距逐步放大至2 mm~5 mm, 辊通水温30℃~40℃ ,缓慢加入硫化促进剂,混炼时间2min;
步骤三,辊距2 mm~5 mm, 辊通水温30℃~40℃ ,缓慢加入硫化活化剂、防老剂,混炼时间3 min~5min;
步骤四,辊距2 mm~5 mm, 辊通水温30℃~40℃ ,缓慢交替加入导电填料中的导电炭黑、乙炔炭黑和增塑剂,混炼30min;
步骤五,辊距2 mm~5 mm, 辊通水温30℃~40℃ ,缓慢加入硫化剂,混炼时间3min;
步骤六,辊距2 mm~5 mm, 辊通水温30℃~40℃ ,切割薄通,薄通次数不少于10次,混炼时间20 min~30min;
步骤七,出片。
9.一种采用权利要求1、2、3、4、7、8所述的任一种推进剂混合机专用导静电橡胶,其特征在于,所述专用导静电橡胶的性能试样制备方法由以下步骤完成:
步骤一,采用力学试片模具制作成120mm×150 mm×2mm的力学试片;
步骤二,将硫化试片放入平板硫化机内,硫化温度150℃~160℃,硫化压力10MPa,硫化时间为60min~70 min;
步骤三,硫化结束,降至室温后,用专用橡胶裁片刀将试片裁成标准试片尺寸。
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Application publication date: 20190322 |