CN103524822B - 一种发泡硅酮母粒及其制备方法与应用 - Google Patents

一种发泡硅酮母粒及其制备方法与应用 Download PDF

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CN103524822B
CN103524822B CN201310248751.0A CN201310248751A CN103524822B CN 103524822 B CN103524822 B CN 103524822B CN 201310248751 A CN201310248751 A CN 201310248751A CN 103524822 B CN103524822 B CN 103524822B
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赵丽
邬继荣
裴勇兵
汤龙程
蒋剑雄
来国桥
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Hubei Huifu Nano Materials Co Ltd
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Abstract

本发明涉及高分子材料领域，硅酮粉作为添加剂，用量一般都在5份以下，为解决直接添加硅酮粉，与粒料基体共混存在分散不均的问题，本发明提出一种发泡硅酮母粒，由热塑性高分子树脂、硅酮粉、发泡剂、抗氧剂共混制成，各组份的重量份分别为：热塑性高分子树脂100份，硅酮粉70~150份，抗氧剂0.5~1份，发泡剂为2~8份。该母粒具有质轻，密度小，易与粒状热塑性高分子树脂共混分散的优点。

Description

一种发泡硅酮母粒及其制备方法与应用
技术领域
本发明涉及高分子材料领域，具体涉及一种发泡硅酮母粒及其制备方法。
背景技术
有机硅聚合物是一类具有半有机半无机结构的特殊高分子材料，具有独特的优异性能。由于有机硅材料自身的特点，助剂中的有机硅组分与塑料基材碳-碳链高聚物既相容又相异，因而既可相互混合发挥特有作用，又不会被基础聚合物完全“淹没同化”失效，因此应用少量的有机硅助剂即可达到明显的改进效果，应用有机硅材料作塑料加工助剂，常常收到较小的投入即可换取重大效益的理想效果。开发用作塑料助剂的有机硅新材料是目前塑料加工助剂行业的一个研究热点。
    我国现有有机硅生产厂主要生产硅油、硅橡胶等初级材料，但是拥有有机硅深产品（如硅酮母粒）开发的厂家并不多见，且规模小、产品单一、无技术开发能力的乡镇企业和个体户生产厂占了大多数。因此，虽然我国有一些有机硅产品的质量和水平与外国同类产品相近，但总体来说，我国有机硅塑料助剂产品品种少、水平低、质量差且数量难以满足国内需求。外资企业（德固赛、道康宁等）在产品与技术方面都处于垄断地位。因此，在今后一段时间内，组织力量加强有机硅塑料助剂产品的开发力度，向国内市场提供急需的符合应用要求和质量标准的有机硅产品，以此进一步增强该产品的在国内及国际的竞争能力，意义重大。
    硅酮母粒主要用作塑料的加工润滑剂、脱模剂与耐磨性能改型剂。该系列产品是目前最新的优异润滑剂，可克服常用小分子润滑剂难分散、用量大、效率低、易析出等缺点。同时随着汽车用塑料材料的迅速发展，作为聚丙烯、尼龙等汽车塑料耐磨助剂的硅酮母粒也迎来了大好发展契机。
申请号为200510049627.7的中国专利公开了一种有机硅酮微粉的制备方法，该发明具有改善塑料制品加工性、脱模性、耐磨性等功效，一定程度上解决了有机硅和塑料难以相混合，小分子硅油易渗出等问题。但是一般高分子树脂都是粒料，再加上硅酮粉的用量一般在3-5质量份，添加量非常少，因此要实现有机硅粉料在塑料中均一分散，十分困难。
发明内容
硅酮粉作为添加剂，用量一般都在5份以下，为解决直接添加硅酮粉，与粒料基体共混存在分散不均的问题，预制母粒是常用的改善方法。本发明提出一种发泡硅酮母粒，该母粒具有质轻，密度小，易与粒状热塑性高分子树脂共混分散的优点。
本发明还提出了这种发泡硅酮母粒的制备方法与应用。
本发明是通过以下技术方案实现的：一种发泡硅酮母粒由热塑性高分子树脂、硅酮粉、发泡剂、抗氧剂共混制成，各组份的重量份分别为：热塑性高分子树脂100份，硅酮粉70~150份，抗氧剂0.5~1份，发泡剂为2~8份。
所述的热塑性高分子树脂选自聚乙烯、聚丙烯、聚苯乙烯、尼龙、聚酯中一种或者几种任意比例的混合物或者选自乙丙橡胶、马来酸酐接枝聚苯乙烯、马来酸酐接枝聚乙烯等共聚物中的一种。
所述的抗氧化剂为抗氧剂1010与抗氧剂168的共混物，其中抗氧剂1010与抗氧剂168的重量比为1~2：1。抗氧剂1010与抗氧剂168均可市购。
所述的发泡剂选自偶氮二甲酰胺、4,4′-氧二苯磺酰肼、2,2′-偶氮二异丁氰、甲基磺酰基脲、碳酸氢钠、柠檬酸纳中的一种或几种。本发明的发泡硅酮母粒中，因原料含有发泡剂，母粒含有很多泡孔，密度小；相对常见的硅酮粉料、硅酮母料而言,母粒成颗粒状且单位质量颗粒数多,故易于高分子树脂粒料共混分散。
本发明利用发泡技术，降低母粒密度，制得低密度的发泡硅酮母粒，从而使得单位质量的硅酮母粒数显著增加，以极少母粒添加量，来改善高分子塑料颗粒共混效果差的问题。
本发明所述的一种发泡硅酮母粒的制备方法为以下步骤，先将热塑性高分子树脂、硅酮粉、发泡剂、抗氧剂混合均匀，得到混合物料；然后将混合物料放入挤出机，从挤出机中熔融挤出，经水冷拉条切料工序，之后脱水干燥，最后冷却包装，得到发泡硅酮母粒。
本发明所述的一种发泡硅酮母粒在热塑性高分子树脂改性中的应用。在热塑性高分子树脂中添加本发明的发泡硅酮母粒，其中发泡硅酮母粒与热塑性高分子树脂的重量比为1~20：100。作为优选，发泡硅酮母粒与热塑性高分子树脂的重量比为3~5：100。
所述的热塑性高分子树脂选自聚乙烯、聚丙烯、聚苯乙烯、尼龙、聚酯中一种或者几种任意比例的混合物或者选自乙丙橡胶、马来酸酐接枝聚苯乙烯、马来酸酐接枝聚乙烯等共聚物中的一种。作为优选，所述的热塑性高分子树脂与发泡硅酮母粒制备时所用的热塑性高分子树脂同种类。
热塑性高分子树脂改性中添加本发明的发泡硅酮母粒可改善高分子树脂熔体流动性，减少加工能耗，提高生产效率，明显提高高分子树脂的耐磨性、润滑和表面光亮度。可广泛应用于汽车、家电等行业，满足生产和生活中对高分子材料力学性能和表面性能的要求。
与现有技术相比，本发明的有益效果是：
（1）本发明制备的发泡硅酮母粒具有质轻易分散的特点；
（2）将本发明的发泡硅酮母粒应用于热塑性高分子树脂改性中，起到润滑、耐磨的功效。
附图说明
图1是本发明的流程示意图；
图2是实施例1的发泡硅酮母粒断面显微镜照片；
图3为实施例2的发泡硅酮母粒断面显微镜照片。
具体实施方式
下面结合附图和实施例对发明进一步说明，实施例中所用原料均可市购，份数为重量份。
本实施例根据美国试验材料学会标准ASTM D792-08测试发泡硅酮母粒的发泡密度ρf。发泡样品密度计算公式为：
ρf = a / (a+w-b)
a为发泡样品在空气中的质量，w是使发泡样品浸在水中的金属帽在水中的质量，b为发泡样品在水中的质量。
实施例1
将高密度聚乙烯树脂（高密度聚乙烯树脂牌号为5000S，密度0.949-0.953，熔体流动速率为0.8-1.2）100份，发泡剂 （偶氮二甲酰胺）5份，抗氧剂（抗氧剂1010：抗氧剂168 = 1:1）1份，硅酮粉100份，充分混合后经双螺杆挤出机将熔体挤出造粒，挤出温度为170-210℃，挤出速度为20rpm，机头压力为4MPa，得到发泡硅酮母粒1。
发泡硅酮母粒1的密度为0.71 g/ cm3，发泡硅酮母粒1的微观断面显微镜照片如图2所示，泡孔尺寸大，泡孔密集。
实施例2
将高密度聚乙烯树脂（高密度聚乙烯树脂牌号为5000S，密度0.949-0.953，熔体流动速率为0.8-1.2）100份，发泡剂（2,2′-偶氮二异丁氰）7份，抗氧剂（抗氧剂1010：抗氧剂168 = 1:1）1份，硅酮粉130份，充分混合后经双螺杆挤出机将熔体挤出造粒，挤出温度为170-210℃，挤出速度为20rpm，机头压力为4.5MPa，得到发泡硅酮母粒2。
发泡硅酮母粒2的密度0.69g/ cm3，发泡硅酮母粒2的微观断面显微镜照片如图3所示，泡孔尺寸大，泡孔密集。
实施例3
    聚丙烯树脂100份，聚丙烯树脂为高熔体强度聚丙烯（HMSPP），密度为0.905 g/cm, MFR为2.4 g／10 min(230℃，2.16 kg)，发泡剂（4,4′-氧二苯磺酰肼）7份，抗氧剂（抗氧剂1010：抗氧剂168 = 1:1）1份，硅酮粉100份，充分混合后经双螺杆挤出机将熔体挤出造粒，挤出温度为180-220℃，挤出速度为20rpm，机头压力为3.5 MPa，得到发泡硅酮母粒3。
发泡硅酮母粒3的密度为0.68 g/ cm3。
实施例4
高抗冲聚苯乙烯树脂100份（高抗冲聚苯乙烯树脂牌号为492J，熔体流动速率为2.8 g/ 10min；DDL1010），发泡剂（DDL-101，济南奥科化工科技有限公司，组成包含碳酸氢钠与偶氮二甲酰胺）5份，抗氧剂（抗氧剂1010：抗氧剂168 = 1:1）1份，硅酮粉100份，充分混合后经双螺杆挤出机将熔体挤出造粒，挤出温度为175-220℃，挤出速度为20rpm，机头压力为3.8MPa，得到发泡硅酮母粒4。
发泡硅酮母粒4的密度为0.69 g/ cm3。
实施例5
马来酸酐接枝高密度聚乙烯（GPM119，熔体流动速率为1.2 g/ 10min (230℃，2.16 kg)，宁波能之光有限公司产品）；发泡剂（碳酸氢钠2份，柠檬酸钠1份，偶氮二甲酰胺4份），抗氧剂（抗氧剂1010：抗氧剂168 = 1:1）1份，硅酮粉100份，充分混合后经双螺杆挤出机将熔体挤出造粒，挤出温度为165-210℃，挤出速度为20rpm，机头压力为4.1MPa，得到发泡硅酮母粒5。
发泡硅酮母粒5的密度为0.70 g/ cm3。
    后续实验表明，实施例1~5制备的发泡硅酮母粒1~5在改性相应的热塑性高分子树脂时达到了较好的共混效果。

Claims (9)

1.一种发泡硅酮母粒，其特征在于，所述的发泡硅酮母粒由热塑性高分子树脂、硅酮粉、发泡剂、抗氧剂共混制成，各组份的重量份分别为：热塑性高分子树脂100份，硅酮粉70~150份，抗氧剂0.5~1份，发泡剂为2~8份，
所述一种发泡硅酮母粒的制备方法为以下步骤，先将热塑性高分子树脂、硅酮粉、发泡剂、抗氧剂混合均匀，得到混合物料；然后将混合物料放入挤出机，从挤出机中熔融挤出，经水冷拉条切料工序，之后脱水干燥，最后冷却包装，得到发泡硅酮母粒。
2.根据权利要求1所述的一种发泡硅酮母粒，其特征在于，所述的热塑性高分子树脂选自聚乙烯、聚丙烯、聚苯乙烯、尼龙、聚酯中一种或者几种任意比例的混合物或者选自马来酸酐接枝聚苯乙烯、马来酸酐接枝聚乙烯共聚物中的一种。
3.根据权利要求1所述的一种发泡硅酮母粒，其特征在于，所述的抗氧剂为抗氧剂1010与抗氧剂168的共混物，其中抗氧剂1010与抗氧剂168的重量比为1~2：1。
4.根据权利要求1所述的一种发泡硅酮母粒，其特征在于，所述的发泡剂选自偶氮二甲酰胺、4,4′-氧二苯磺酰肼、2,2′-偶氮二异丁腈、甲基磺酰基脲、碳酸氢钠、柠檬酸钠中的一种或几种。
5.一种如权利要求1~4中任一项所述的一种发泡硅酮母粒在热塑性高分子树脂改性中的应用。
6.根据权利要求5所述的一种发泡硅酮母粒在热塑性高分子树脂改性中的应用，其特征在于：在热塑性高分子树脂中添加发泡硅酮母粒，其中发泡硅酮母粒与热塑性高分子树脂的重量比为1~20：100。
7.根据权利要求6所述的一种发泡硅酮母粒在热塑性高分子树脂改性中的应用，其特征在于：在热塑性高分子树脂中添加发泡硅酮母粒，其中发泡硅酮母粒与热塑性高分子树脂的重量比为3~5：100。
8.根据权利要6或7所述的一种发泡硅酮母粒在热塑性高分子树脂改性中的应用，其特征在于：所述的热塑性高分子树脂选自聚乙烯、聚丙烯、聚苯乙烯、尼龙、聚酯中一种或者几种任意比例的混合物或者选自马来酸酐接枝聚苯乙烯、马来酸酐接枝聚乙烯共聚物中的一种。
9.根据权利要8所述的一种发泡硅酮母粒在热塑性高分子树脂改性中的应用，其特征在于：所述的热塑性高分子树脂与发泡硅酮母粒制备时所用的热塑性高分子树脂同种类。
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