CN107796778A - 子午线轮胎原材料小样红外光谱检测制样方法 - Google Patents
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Abstract
本发明实施例提供了一种橡胶轮胎用原材料红外光谱检测方法，包括以下步骤：称取溴化钾和原材料；预烘干；混料研磨；压片；红外检测，本发明中，预先对压片模具、溴化钾、原材料进行预烘干，然后混料研磨时将脱水烘干的溴化钾、原材料放置在热的压片模具中，从源头上解决了溴化钾吸收水分的问题，本发明方法适用于防老剂、促进剂及树脂类等材料的检测。
Description
技术领域
本发明涉及子午线轮胎用原材料小样检测技术领域，尤其涉及一种子午线轮胎原材料小样红外光谱检测制样方法。
背景技术
采用红外光谱仪对材料进行光谱分析，是检测材料性能的一种常用手段。溴化钾压片法主要用于红外定性分析和结构分析，但溴化钾极易吸水，即使在干燥箱中先烘干，在制样过程中也无法避免因其吸水而导致制出的片出现云雾状、点状等样品不透现象，且检测出谱图易出现水吸收干扰峰；制片效果无法达到标准要求，且会对测定结果造成一定影响。
发明内容
有必要提出一种有效控制红外光谱检测时采用溴化钾压片法制样过程吸水的子午线轮胎原材料小样红外光谱检测制样方法。
一种子午线轮胎原材料小样红外光谱检测制样方法，包括以下步骤：
称取溴化钾和原材料小样；
预烘干：将压片模具、溴化钾、原材料小样分别至于45-55℃的电热板上或恒温干燥箱中预烘干，以进行对溴化钾和原材料小样进行脱水，以对压片模具进行预烘干；
混料研磨：将预烘干后的原材料小样和溴化钾放入玛瑙研钵中顺时针研磨1-2min，至粉末状，使二者混合均匀，得到样品；
压片：将混合均匀的样品置于预热的压片模具的模腔内，合上上模槽和下模槽，施加8-10吨压力进行压片，保持压力30S-1min，拆下上模槽和下模槽，形成样片；
红外检测：将上述样片置于红外光谱仪中进行红外光谱检查分析，得到原材料小样的红外谱图。
本发明方法中，预先对压片模具、溴化钾、原材料小样进行预烘干，然后混料研磨时将脱水烘干的溴化钾、原材料小样放置在热的压片模具中，从源头上解决了溴化钾吸收水分的问题。
本发明方法适用于防老剂、促进剂及树脂类等材料的检测。
附图说明
图1为采用本发明方法压片后的样片。
图2为采用本发明方法压片后的样片的红外光谱图。
图3为采用常规方法压片后的样片。
图4为采用常规方法压片后样片的红外光谱图。
具体实施方式
为了更清楚地说明本发明实施例的技术方案，下面将对实施例中所需要使用的附图作简单的介绍，显而易见地，下面描述中的附图是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。
本发明实施例提供了一种子午线轮胎原材料小样红外光谱检测制样方法，包括以下步骤：
称取溴化钾和原材料小样；
预烘干：将压片模具、溴化钾、原材料小样分别至于45-55℃的电热板上或恒温干燥箱中预烘干，以进行对溴化钾和原材料小样进行脱水，以对压片模具进行预烘干；
混料研磨：将预烘干后的原材料小样和溴化钾放入玛瑙研钵中顺时针研磨1-2min，至粉末状，即原材料小样和溴化钾的直径为2±0.5um，使二者混合均匀，得到样品；
压片：将混合均匀的样品置于预热的压片模具的模腔内，合上上模槽和下模槽，施加8-10吨压力进行压片，保持压力30S-1min，拆下上模槽和下模槽，形成样片；
红外检测：将所制得的透明样片置于红外光谱仪中进行红外光谱检测分析，当样品中的分子中某个基团的振动与发出的红外光的振动频率相同时，该处波长的光就被该物质吸收，通过此方法可确定物质分子结构和鉴别化合物的分析方法，即辐射后通过检测器进行光电转换后的红外谱图。
进一步的，在“预烘干”的步骤中，经过预烘干的压片模具的传热温度在45-55℃。对经过预烘干的原材料小样进行加热减量含量检测，确保检测原材料小样的加热减量含量低于0.5%，以使原材料小样完全脱水，若原材料小样的加热减量含量高于0.5%，则继续对原材料小样进行预烘干。原材料小样的加热减量的含量即为原材料小样的水分含量。
进一步的，在“称取溴化钾和原材料小样”的步骤中，溴化钾和原材料小样的质量比为100mg~200mg：1mg-2mg；
进一步的，在“混料研磨”步骤中，为防止研磨过程吸水，先对玛瑙研砵进行预热，使得玛瑙研钵的温度达到45-55℃，再将预烘干后的原材料小样和溴化钾放入预热后的玛瑙研钵中，进行混料研磨。例如可以先将玛瑙研砵放在电热板上或放在恒温干燥箱中预热。
进一步的，将盛放了预烘干后的原材料小样和溴化钾的预热后的玛瑙研钵放置在电热板上，保持电热板的温度不低于55℃，进行混料研磨。如此，对原材料小样，溴化钾进行了预烘干，对玛瑙研砵进行了预热，在研磨的过程中又将玛瑙研钵放在电热板上，这样从各个方面都做到了温度保护，使得研磨过程中溴化钾不会吸收水分。
进一步的，在“压片”的步骤中，采用压片机对样品进行压片，压片机包括上模槽、下模槽，压片时，先将压片模具放置在下模槽上，然后将样品置于预热的压片模具的模腔内，然后上模槽和下模槽装模，对压片模具进行施压，形成透明样片。该过程中，压片模具经过了预热，样品经过了预烘干，不仅保证了样品的制样规范，同时根据热胀冷缩的原理，样品压片后释压脱模，使样品层与上下模槽易脱模，进一步解决了样品脱模困难的问题。
进一步的，所述电热板的表面具有氟龙涂层或石墨层，进而避免溴化钾对电热板腐蚀。
为了验证本发明的效果，根据上述方法，对子午线轮胎用原材料，即防老剂取样，与溴化钾研磨、混料、压片，如图1，将该样片置于红外光谱仪中进行红外光谱检查分析，得到原材料小样的红外谱图，如图2；
作为对比试验，采用常规方法也称取同一批次的防老剂和溴化钾，进行研磨、混料、压片，如图3，将样片置于红外光谱仪中进行红外光谱检查分析，得到原材料小样的红外谱图，如图4；
由图1可见，压出的样片透明无雾状，由图2可见，红外光谱图透过率曲线无水吸收峰，能够真实反映防老剂的成分。
由图3可见，压出的样片不透明，且有明显的云雾状，该云雾状即为溴化钾吸收空气中的水分，使得吸收的水分覆盖在样片的表面形成云雾状，由图4可见，红外光谱图透过率曲线能够看到明显的水吸收峰，造成对防老剂的成分分析的干扰。
本发明实施例方法中的步骤可以根据实际需要进行顺序调整、合并和删减。
本发明实施例装置中的模块或单元可以根据实际需要进行合并、划分和删减。
以上所揭露的仅为本发明较佳实施例而已，当然不能以此来限定本发明之权利范围，本领域普通技术人员可以理解实现上述实施例的全部或部分流程，并依本发明权利要求所作的等同变化，仍属于发明所涵盖的范围。
Claims (7)
1.一种子午线轮胎原材料红外光谱检测制样方法，其特征在于包括以下步骤：
称取溴化钾和原材料小样；
预烘干：将压片模具、溴化钾、原材料小样分别至于45-55℃的电热板上或恒温干燥箱中预烘干，以进行对溴化钾和原材料小样进行脱水，以对压片模具进行预烘干；
混料研磨：将预烘干后的原材料小样和溴化钾放入玛瑙研钵中顺时针研磨1-2min，至粉末状，使得原材料小样和溴化钾的直径均为2±0.5um，使二者混合均匀，得到样品；
压片：将混合均匀的样品置于预热的压片模具的模腔内，合上上模槽和下模槽，施加8-10吨压力进行压片，保持压力30S-1min，拆下上模槽和下模槽，形成样片；
红外检测：将上述样片置于红外光谱仪中进行红外光谱检查分析，得到原材料小样的红外谱图。
2.如权利要求1所述的子午线轮胎原材料红外光谱检测制样方法，其特征在于：在“预烘干”的步骤中，对经过预烘干的原材料进行加热减量含量检测，确保检测原材料的加热减量含量低于0.5%，以使原材料完全脱水，若原材料的加热减量含量高于0.5%，则继续对原材料进行预烘干。
3.如权利要求1所述的子午线轮胎原材料红外光谱检测制样方法，其特征在于：在“称取溴化钾和原材料”的步骤中，溴化钾和原材料的质量比为100mg~200mg:：mg-2mg。
4.如权利要求1所述的子午线轮胎原材料红外光谱检测制样方法，其特征在于：在“混料研磨”步骤中，为防止研磨过程吸水，先对玛瑙研砵进行预热，使得玛瑙研钵的温度达到45-55℃，再将预烘干后的原材料和溴化钾放入预热后的玛瑙研钵中，进行混料研磨。
5.如权利要求4所述的子午线轮胎原材料红外光谱检测制样方法，其特征在于：将盛放了预烘干后的原材料和溴化钾的预热后的玛瑙研钵放置在电热板上，保持电热板的温度不低于55℃，进行混料研磨。
6.如权利要求1所述的子午线轮胎原材料红外光谱检测制样方法，其特征在于：在“压片”的步骤中，采用压片机对样品进行压片，压片机包括上模槽、下模槽，压片时，先将压片模具放置在下模槽上，然后将样品置于预热的压片模具的模腔内，然后上模槽和下模槽装模，对压片模具进行施压，形成透明样片。
7.如权利要求1所述的子午线轮胎原材料红外光谱检测制样方法，其特征在于：所述电热板的表面具有氟龙涂层或石墨层，进而避免溴化钾对电热板腐蚀。
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