CN111777942A - 一种防粘连凝胶及其制备方法 - Google Patents

一种防粘连凝胶及其制备方法 Download PDF

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CN111777942A
CN111777942A CN202010653022.3A CN202010653022A CN111777942A CN 111777942 A CN111777942 A CN 111777942A CN 202010653022 A CN202010653022 A CN 202010653022A CN 111777942 A CN111777942 A CN 111777942A
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oil
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camellia oil
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李官强
李刚
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Guizhou Province Shiqian County Fodingshan Wild Camellia Oil Industry Co ltd
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Abstract

本发明属于防粘连技术领域，具体涉及一种防粘连凝胶及其制备方法；采用氢化山茶油、水滑石、改性碳化硅等原料制备了一种可应用于防粘连领域的凝胶，这种凝胶可以应用在金属锅具、食品级的硬质塑料模具以及医用级防粘连纱布等防粘连领域。对人体无毒害作用，可延长不沾涂层在高温下的使用寿命，且所制造的涂层耐磨，导热好，耐腐蚀，抗冲击能力提高，不会由于加热而出现脱落。

Description

一种防粘连凝胶及其制备方法
技术领域
本发明属于防粘连技术领域，具体涉及一种防粘连凝胶及其制备方法。
背景技术
在工业生产及日常生活中,如何防粘连是经常遇到的问题，如工业制造使用的脱模剂，医药领域使用的防粘连隔离膜，日常生活中使用的不粘锅等。
对于不沾锅具而言，常见的、不沾性能最好的有聚四氟乙烯涂层和陶瓷涂层，目前聚四氟乙烯涂层采用水性聚四氟乙烯不沾土料涂覆或将聚四氟乙烯粉末涂料喷涂在金属表面后经高温烘烤后固化得到。由于聚四氟乙烯的熔点限制，不粘锅在错误操作干烧时，聚四氟乙烯涂层会发生软化，以至局部集热高的部位发生熔融。软化或熔融聚四氟乙烯涂层在沸腾的水或油中气泡快速逸出和破裂时冲击力作用下，聚四氟乙烯涂层产生空白区域，水和油可以透过聚四氟乙烯涂层直接涂锅具接触，并在高温下以液态或气态的形式渗入同时在聚四氟乙烯涂层与锅体之间加热，使聚四氟乙烯涂层在空白区域外沿结合力下降，空白区域扩大，最终使聚四氟乙烯涂层成片软化脱落，降低锅具的使用寿命。
在公开号为CN110065149A的专利中公开了一种生产人造石用的喷涂式脱模剂、制备方法及其使用方法，包括以下原料:聚乙烯醇、石蜡、水滑石粉、硅酸镁、硅酸铝镁、氧化锌、氢氧化镁、聚四氟乙烯、纤维素、黄原胶、三聚磷酸钠、碳酸钠、改性山茶油、1-十二烷基-3-甲基咪唑硝酸盐、十八烷基瑚珀单酰胺磺酸二甲；其中，在制备过程S1步骤中，所使用的方法为：在反应釜中加入纤维素、黄原胶、聚乙烯醇、改性山茶油、1-十二烷基-3-甲基咪唑硝酸盐，搅拌升温至85-87℃，使聚乙烯醇完全溶解，制得混合物A。聚乙烯醇不溶于植物油、甲醇、乙二醇等，在95℃以上可溶于水，且熔点在230-240℃，而在此专利中公开的原料中纤维素、黄原胶、聚乙烯醇、1-十二烷基-3-甲基咪唑硝酸盐均为固体，可作为溶剂的只有改性山茶油，通过改性山茶油的制备过程可知，改性山茶油是经过蒸发除水的，即聚乙烯醇是否能溶解、这个制备方法是否可行、这个喷涂式脱模剂是否有效是存在质疑的。
发明内容
本发明为解决上述问题，提供了一种防粘连凝胶及其制备方法。
具体是通过以下技术方案来实现的：
一种防粘连凝胶，其组成按重量份计包括：改性碳化硅10-21份、水滑石14-25份、氢化山茶油11-23份、聚乙烯醇7-13份、琥珀酸溶液4-8份、5-甲基-2-异丙基苯酚2-3份。
具体步骤为：
1、制备氢化山茶油：
a.将山茶籽经磁选吸附筛选清洗后脱壳处理，烘干表面水分后进行冷冻，将冷冻的山茶籽于50-65℃的螺旋榨油机中进行榨油，油渣迅速分离并静置沉降2h过滤，得到毛油；
b.脱胶处理：将毛油加热至50-70℃，加入毛油体积7-11％的磷酸溶液及毛油质量4-6％的磷脂酶，搅拌10-20min后离心得到脱胶山茶油；
c.脱水处理：加入其重量3-5％的无水碳酸钠到脱胶山茶油中搅拌后在真空条件下脱水，再经过滤得到；
d.氢化处理：加入0.1-1.5％的金属催化剂及同等质量的柠檬酸，在温度190-210℃，压力1.0-2.5mpa的条件下对山茶油进行氢化处理，将其切割成粒径为3-5mm的小粒，冷冻。
2、制备改性碳化硅：将碳化硅与其重量5％-13％的石墨烯混合使用球磨机研磨30-40min，再在充入氮气的条件下以900-1000℃的温度烧结得到改性碳化硅。
3、制备混合液：
a.以1g琥珀酸：20ml丙三醇的比例将琥珀酸溶于丙三醇中，加温至40-50℃，搅拌至琥珀酸完全溶解；
b.将聚乙烯醇浸泡在冷水中10-12h使其溶胀，再滴入琥珀酸溶液，同时加热至95℃至聚乙烯醇迅速溶解，此时加入熔融的5-甲基-2-异丙基苯酚及聚乙烯醇溶液质量8-10％的无机盐得到混合液。
4、制备防粘连凝胶：将改性碳化硅和水滑石混合研磨，边研磨边加入粒径在3-5mm的氢化山茶油，得到茶油膏，再将混合液与茶油膏混合后加入1-3％的凝胶化液体搅拌至混合物呈透明果冻状得到；
其中，所述的凝胶化液体是指硼砂、硼酸、铬酸盐、重铬酸盐、高锰酸盐中的任意一种。
进一步，所述的防粘连凝胶可用于不沾涂层、脱模剂、防粘剂、医用防粘连纱布等，优选应用为不沾锅具涂层。
综上所述,本发明的有益效果在于：本发明采用氢化山茶油、石墨烯、水滑石、改性碳化硅等原料制备了一种防粘连凝胶，这种凝胶可以应用在金属锅具、食品级的硬质塑料模具以及医用级防粘连纱布等防粘连领域。对人体无毒害作用，延长不沾涂层在高温下的使用寿命，且所制造的涂层耐磨，导热好，耐腐蚀，抗冲击能力提高，不会由于加热而出现脱落。
其中，山茶油相较于其他植物油而言含有更多的不饱和脂肪酸，在进行氢化时会转化为更多的饱和脂肪酸，使涂层在制造过程中各种原料更好的融合，同时山茶油中含有角鲨烯、茶多酚、山茶甙等多种有益物质，保证烹饪器具在使用时不会产生对人体有害的物质，且随着使用过程中这些有益物质还能缓慢的渗入食物中。将山茶籽进行冷冻后直接榨油，使细胞液泡中的液体迅速结成冰晶，冰晶刺破液泡，内容物流出，使得在后续的榨油过程中出油量更大，且山茶籽油所含的有益成分更多。采用50-65℃的低温榨油可以避免高温造成不饱和脂肪酸发生聚合作用，使后续进行氢化时可以将不饱和脂肪酸全部转变为饱和脂肪酸。在氢化过程中加入的柠檬酸，会与游离的镍、铜等金属离子络合，可减少金属残留。在温度190-210℃，压力1.0-2.5mpa的条件下对山茶油进行极度氢化处理，可以将山茶油中的不饱和脂肪酸全部转变为饱和脂肪酸，氢化不完全会使后续制备茶油膏时茶油膏的状态过软，甚至出现液态油，与改性氮化硅和水滑石不能很好地结合，导致涂层不均匀或是有细小的孔洞出现。采用石墨烯对碳化硅进行改性，先使用球磨将石墨烯和碳化硅进行研磨，会有一层石墨烯附着在碳化硅表面，再在900-1000℃，同时充入氮气的条件下进行烧结，在高温条件下，氮气与游离的硅离子结合形成氮化硅，在石墨烯分子的连接下与碳化硅紧密结合，使其比改性前碳化硅的韧性和耐磨性增加，可提高涂层的抗冲击能力和导热性，且耐酸碱腐蚀，仅能与氢氟酸反应，在高温情况下能与氢氧化钠反应，对于烹饪器具来说日常使用的醋酸、小苏打等是不会对涂层造成腐蚀的。水滑石拥有记忆效应，焙烧温度在600℃以下时其结构都可以恢复，使得制作的涂层稳定性好，不会由于加热而出现脱落或裂纹等现象，将琥珀酸溶于丙三醇中可作为分散剂，将氢化山茶油分子和改性碳化硅一起均匀插入到水滑石分子层中，形成朝外疏水的薄层，同时聚乙烯醇增强分子层的延展性，增强涂层的成膜性，同时，加入5-甲基-2-异丙基苯酚可以增强涂层的防霉性，减少由于湿度过高引起的霉菌滋生，提高烹饪器具在进行食品加工时的食品安全性。加入无机盐可以有效地增加聚乙烯醇的热稳定性，使涂层在高温加热时也不会出现孔洞或脱落的现象。
具体实施方式
下面对本发明的具体实施方式作进一步详细的说明，但本发明并不局限于这些实施方式，任何在本实施例基本精神上的改进或代替，仍属于本发明权利要求所要求保护的范围。
实施例1
一种防粘连凝胶，其组成按重量份计包括：改性碳化硅15份、水滑石20份、氢化山茶油17份、聚乙烯醇10份、琥珀酸溶液6份、5-甲基-2-异丙基苯酚2份。
具体步骤为：
1、制备氢化山茶油：
a.将山茶籽经磁选吸附筛选清洗后脱壳处理，烘干表面水分后进行冷冻，将冷冻的山茶籽于57℃的螺旋榨油机中进行榨油，油渣迅速分离并静置沉降2h过滤，得到毛油；
b.脱胶处理：将毛油加热至60℃，加入毛油体积9％的磷酸溶液及毛油质量5％的磷脂酶，搅拌15min后离心得到脱胶山茶油；
c.脱水处理：加入其重量4％的无水碳酸钠到脱胶山茶油中搅拌后在真空条件下脱水，再经过滤得到；
d.氢化处理：加入0.8％的金属催化剂及同等质量的柠檬酸，在温度200℃，压力2mpa的条件下对山茶油进行氢化处理，将其切割成粒径为4mm的小粒，冷冻。
2、制备改性碳化硅：将碳化硅与其重量9％的石墨烯混合使用球磨机研磨35min，再在充入氮气的条件下以950℃的温度烧结得到改性碳化硅。
3、制备混合液：
a.以1g琥珀酸：20ml丙三醇的比例将琥珀酸溶于丙三醇中，加温至45℃，搅拌至琥珀酸完全溶解；
b.将聚乙烯醇浸泡在冷水中11h使其溶胀，再滴入琥珀酸溶液，同时加热至95℃至聚乙烯醇迅速溶解，此时加入熔融的5-甲基-2-异丙基苯酚及聚乙烯醇溶液质量8-10％的无机盐得到混合液。
4、制备防粘连凝胶：将改性碳化硅和水滑石混合研磨，边研磨边加入粒径在4mm的氢化山茶油，得到茶油膏，再将混合液与茶油膏混合后加入2％的硼酸溶液搅拌至混合物呈透明果冻状得到。
进一步，所述的防粘连凝胶作为不沾涂层的应用方法：将凝胶均匀涂布在锅具内壁，干燥即可。
实施例2
一种防粘连凝胶，其组成按重量份计包括：改性碳化硅21份、水滑石25份、氢化山茶油23份、聚乙烯醇13份、琥珀酸溶液8份、5-甲基-2-异丙基苯酚3份。
具体步骤为：
1、制备氢化山茶油：
a.将山茶籽经磁选吸附筛选清洗后脱壳处理，烘干表面水分后进行冷冻，将冷冻的山茶籽于65℃的螺旋榨油机中进行榨油，油渣迅速分离并静置沉降2h过滤，得到毛油；
b.脱胶处理：将毛油加热至70℃，加入毛油体积11％的磷酸溶液及毛油质量6％的磷脂酶，搅拌20min后离心得到脱胶山茶油；
c.脱水处理：加入其重量5％的无水碳酸钠到脱胶山茶油中搅拌后在真空条件下脱水，再经过滤得到；
d.氢化处理：加入1.5％的金属催化剂及同等质量的柠檬酸，在温度210℃，压力2.5mpa的条件下对山茶油进行氢化处理，将其切割成粒径为5mm的小粒，冷冻。
2、制备改性碳化硅：将碳化硅与其重量13％的石墨烯混合使用球磨机研磨40min，再在充入氮气的条件下以1000℃的温度烧结得到改性碳化硅。
3、制备混合液：
a.以1g琥珀酸：20ml丙三醇的比例将琥珀酸溶于丙三醇中，加温至50℃，搅拌至琥珀酸完全溶解；
b.将聚乙烯醇浸泡在冷水12h中使其溶胀，再滴入琥珀酸溶液，同时加热至95℃至聚乙烯醇迅速溶解，此时加入熔融的5-甲基-2-异丙基苯酚3份及聚乙烯醇溶液质量10％的无机盐得到混合液。
4、制备防粘连凝胶：将改性碳化硅和水滑石混合研磨，边研磨边加入粒径在5mm的氢化山茶油，得到茶油膏，再将混合液与茶油膏混合后加入3％的高锰酸钾溶液搅拌至混合物呈透明果冻状得到。
进一步，所述的防粘连凝胶作为脱模剂的应用方法：可将凝胶直接涂布于模具中待其干燥，也可将凝胶融化后以喷涂的方式涂布在模具中，具体以模具中花纹的精细程度选择不同的涂布方法。
实施例3
一种防粘连凝胶，其组成按重量份计包括：改性碳化硅10份、水滑石14份、氢化山茶油11份、聚乙烯醇7份、琥珀酸溶液4份、5-甲基-2-异丙基苯酚2份。
具体步骤为：
1、制备氢化山茶油：
a.将山茶籽经磁选吸附筛选清洗后脱壳处理，烘干表面水分后进行冷冻，将冷冻的山茶籽于50℃的螺旋榨油机中进行榨油，油渣迅速分离并静置沉降2h过滤，得到毛油；
b.脱胶处理：将毛油加热至50℃，加入毛油体积7％的磷酸溶液及毛油质量4％的磷脂酶，搅拌10min后离心得到脱胶山茶油；
c.脱水处理：加入其重量3％的无水碳酸钠到脱胶山茶油中搅拌后在真空条件下脱水，再经过滤得到；
d.氢化处理：加入0.1％的金属催化剂及同等质量的柠檬酸，在温度190℃，压力1.0mpa的条件下对山茶油进行氢化处理，将其切割成粒径为3mm的小粒，冷冻。
2、制备改性碳化硅：将碳化硅与其重量5％的石墨烯混合使用球磨机研磨30min，再在充入氮气的条件下以900℃的温度烧结得到改性碳化硅。
3、制备混合液：
a.以1g琥珀酸：20ml丙三醇的比例将琥珀酸溶于丙三醇中，加温至40℃，搅拌至琥珀酸完全溶解；
b.将聚乙烯醇浸泡在冷水中10h使其溶胀，再滴入琥珀酸溶液，同时加热至95℃至聚乙烯醇迅速溶解，此时加入熔融的5-甲基-2-异丙基苯酚及聚乙烯醇溶液质量8％的无机盐得到混合液。
4、制备防粘连凝胶：将改性碳化硅和水滑石混合研磨，边研磨边加入粒径在3mm的氢化山茶油，得到茶油膏，再将混合液与茶油膏混合后加入1％的重铬酸钾溶液搅拌至混合物呈透明果冻状得到。
进一步，所述的防粘连凝胶作为医用防粘连剂的应用方法：将脱脂纱布浸在凝胶中，刮去多余的凝胶，干燥，此纱布即可用于包扎伤口，可有效防止新生组织与纱布粘连，避免出现由于粘连导致的新创伤。
一、山茶油化学成分测定
实验1
本实验在与实施例1的同等条件下，不对山茶籽进行冷冻，于90℃下炒制后榨取山茶油，对所榨取的山茶油进行成分分析，测定三次取平均值，并与实施例1进行对比，其结果如表1所示。
其中，角鲨烯及维生素E的测定方法为：将山茶油进行造化后提取不皂化物，浓缩后进行气相色谱-质谱测定，根据外标法计算角鲨烯和维生素E的含量。
出油率(％)＝茶油的质量/油茶籽的质量×100％
表1
项目 角鲨烯(mg/kg) 维生素E(mg/kg) 出油率(％)
实施例1 425.07 345.19 31.54
实验1 249.13 147.62 26.10
由于高温炒制，使得榨取的山茶油中角鲨烯和维生素E的含量大幅降低；不进行冷冻，油脂分子不能完全被榨取。同时，额外对实施例1中山茶油的酸价(以KOH计)进行测定，发现其酸价平均值为1.4，达到国家标准，可以直接作为食用油使用。
二、涂层物理性能对比实验
实验2
本实验以不沾锅涂层为具体应用对象，在与实施例1的同等条件下，将改性碳化硅更换为碳化硅，对制作的涂层进行硬度、孔隙率、耐磨性进行测试，并与实施例1进行对比，其结果如表2所示。
其中，涂层表面硬度根据GB/T9790-1988采用维氏硬度计测定维氏硬度。
涂层孔隙率是根据中华人民共和国机械行业标准JB/T7509-94测定。
耐磨性测试方法：配制浓度为5-10％的洗洁精水，在3M百洁布上附中3.0kgf，左右摆动单程为1次，每300次更换百洁布，当涂层脱落或露出基材时终止试验并记录耐磨次数。
实验3
本实验以不沾锅涂层为具体应用对象，在与实施例1的同等条件下，将改性碳化硅更换为氮化硅，对制作的涂层进行硬度、孔隙率、耐磨性进行测试，并与实施例1进行对比，其结果如表2所示。
实验4
本实验以不沾锅涂层为具体应用对象，在与实施例1的同等条件下，在对碳化硅进行改性时不添加石墨烯，对制作的涂层进行硬度、孔隙率、耐磨性进行测试，并与实施例1进行对比，其结果如表2所示。
表2
项目 硬度(HV) 孔隙率(％) 耐磨次数(次)
实施例1 530 0.4 13400
实验2 440 0.7 11000
实验3 415 0.7 10700
实验4 540 0.5 9400
三、涂层耐腐蚀性对比实验
实验5-7
以不沾锅涂层为具体应用对象，分别使用HF、浓H2SO4、醋酸、NaOH、Na2CO3溶液在加热沸腾后浸泡24h的条件下，对上述实施例及实验2-4中所制备的涂层进行耐腐蚀测试，结果如表3所示。
表3
Figure BDA0002575687850000091
Figure BDA0002575687850000101
其中，碳化硅与氢氟酸反应：SiC+4HF＝＝SiF4↑+CH4↑
在加热沸腾的条件下与浓硫酸反应：SiC+2H2SO4＝＝CO2↑+SiO2+2H2O+SO2↑
在高温条件下与氢氧化钠反应：SiC+2NaOH+2O2＝＝Na2SiO3+CO2↑+H2O
氮化硅在水中加热的条件下与氢氟酸反应：Si3N4+12HF＝＝3SiF4↑+4NH3↑
与氢氧化钠反应：Si3N4+6NaOH+3H2O＝＝3Na2SiO3+4NH3↑
可以看出，单独使用碳化硅或氮化硅制作的涂层耐酸性较好，但结合硬度、孔隙率、耐磨性等综合条件下来以本发明的方法所制作的涂层更好。日常生活中使用到NaOH、HF和浓H2SO4的情况很少，因此，虽然实施例1中的凝胶与这三种化学试剂也有反应，但对日常使用并无较大影响。
四、医药级防粘连测试
选取健康合格清洁级小鼠20只，体重20-24g，雌雄各半，在隔离器中饲养，温度在18-24℃之间，明暗各12h，自由饮水觅食,平均随机分为4组。
实验8-10
将健康小鼠麻醉，背部剪毛，用手术刀在无菌条件下，在背部做直径为1.5厘米的标准伤口，用上述实施例及实验2-4中所制备的凝胶浸润纱布，每天换药，观察小鼠的生命体征及纱布与小鼠伤口的黏连程度。
实验结果：所有实验组的小鼠生存状况良好，对小鼠的生命体征进行测量，显示正常，未出现任何副作用和死亡。
实施例1-3的黏连程度均为不黏连，换药时纱布不与伤口粘连，纱布放置一周后依然柔软，吸水性未受到影响。实验8-10中的纱布在小鼠伤口开始生长新生组织的时候换药均出现不同程度的黏连，并且以凝胶浸润过的纱布在放置一周后纱布变硬，柔韧度降低，吸水性与普通纱布相比有降低。

Claims (9)

1.一种防粘连凝胶，其特征在于，其组成按重量份计包括：改性碳化硅10-21份、水滑石14-25份、氢化山茶油11-23份、聚乙烯醇7-13份、琥珀酸溶液4-8份、5-甲基-2-异丙基苯酚2-3份。
2.如权利要求1所述的一种防粘连凝胶，其特征在于，所述的氢化山茶油，其制备方法为：
a.将山茶籽经磁选吸附筛选清洗后脱壳处理，烘干表面水分后进行冷冻，将冷冻的山茶籽于50-65℃的螺旋榨油机中进行榨油，油渣迅速分离并静置沉降2h过滤，得到毛油；
b.将毛油进行脱胶、脱水处理得到山茶油；
c.氢化处理：加入0.1-1.5％的金属催化剂及同等质量的柠檬酸，在温度190-210℃，压力1.0-2.5mpa的条件下对山茶油进行氢化处理，将其切割成粒径为3-5mm的小粒，冷冻。
3.如权利要求2所述的一种防粘连凝胶，其特征在于，所述的脱胶处理，是将毛油加热至50-70℃，加入磷酸溶液及磷脂酶，搅拌10-20min后离心得到脱胶山茶油。
4.如权利要求2所述的一种防粘连凝胶，其特征在于，所述的脱水处理，是将无水碳酸钠加入到脱胶山茶油中搅拌后在真空条件下脱水，再经过滤得到。
5.如权利要求1所述的一种防粘连凝胶，其特征在于，所述的改性碳化硅，是将碳化硅与其重量5％-13％的石墨烯混合使用球磨机进行研磨，再在充入氮气的条件下进行烧结得到改性碳化硅。
6.如权利要求1所述的一种防粘连凝胶，其特征在于，所述的混合液，是将琥珀酸溶于丙三醇中，加温至40-50℃至琥珀酸完全溶解，再将聚乙烯醇浸泡在冷水中使其溶胀，再滴入琥珀酸溶液，同时加热至95℃至聚乙烯醇迅速溶解，此时加入熔融的5-甲基-2-异丙基苯酚及无机盐得到混合液。
7.一种防粘连凝胶的制备方法，其特征在于，所述制备方法为：对改性碳化硅和水滑石进行研磨，边研磨边加入粒径在3-5mm的氢化山茶油，得到茶油膏，再将混合液与茶油膏混合后加入凝胶化液体搅拌至混合物呈透明果冻状得到。
8.如权利要求7所述的一种防粘连凝胶，其特征在于，所述的凝胶化液体是指硼砂、硼酸、铬酸盐、重铬酸盐、高锰酸盐中的任意一种。
9.一种氢化山茶油在防粘连领域的应用，其特征在于，所述防粘连领域包括但不限于不沾涂层和脱模剂。
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