CN115246971B - 用于pvc热稳定剂的改性水铝钙石-豆渣的制备方法 - Google Patents
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Abstract
本发明提出了一种用于PVC热稳定剂的改性水铝钙石‑豆渣的制备方法。该方法包括:(1)将碳酸钠溶于水中,加入氢氧化钙、氢氧化铝和豆渣,搅拌条件下在70~100℃反应0.5~3小时;(2)加入表面改性剂,在70~100℃继续反应10~25小时,将反应得到的固体物脱水干燥后,得到改性水铝钙石‑豆渣。采用本发明提供的技术方案制备的改性水铝钙石‑豆渣复合材料对PVC的热稳定性能优于传统的改性水铝钙石,且生产成本相对较低。
Description
技术领域
本发明涉及塑料加工助剂领域,特别涉及一种用于PVC热稳定剂的改性水铝钙石-豆渣的制备方法。
背景技术
豆渣是豆制品加工过程中的主要副产物,我国每年湿豆渣的产量在2000万吨以上。湿豆渣的蛋白质含量高,含水量高,易腐败变质,不易保存,大部分豆渣仍被直接丢弃,污染环境的同时也造成了资源浪费。因此,豆渣的高值化利用已成为豆制品加工行业急需解决的关键技术问题。
水铝钙石是一种阴离子粘土,具有层状结构以及层间阴离子可调控性等特点,在热稳定剂、阻燃剂、吸附剂和催化等领域具有广泛的应用前景。水铝钙石对聚氯乙烯(PVC)具有热稳定性,原因在于水铝钙石可与PVC降解过程中产生的HCl发生反应,有效抑制HCl对PVC进一步降解的催化作用。近年来,关于水铝钙石作为PVC热稳定剂的报道主要集中在制备条件的优化及表面改性剂的筛选等方面,未见关于水铝钙石基复合材料在PVC热稳定剂中的应用。
为了进一步降低水铝钙石的生产成本,并提升其对PVC的热稳定性能,开发水铝钙石基复合材料是可选途径之一。
发明内容
本发明的目的在于提供一种用于PVC热稳定剂的改性水铝钙石-豆渣的制备方法,该方法以豆制品加工产业的副产物豆渣为原料,具有原材料成本较低的优势,且制备的改性水铝钙石-豆渣对PVC的热稳定性能非常优异。
为了实现以上目的,本发明采取的技术方案是一种用于PVC热稳定剂的改性水铝钙石-豆渣的制备方法,其特征在于,包括以下步骤:
(1)将碳酸钠溶于水中,加入氢氧化钙、氢氧化铝和豆渣,搅拌条件下在70~100℃反应0.5~3小时;其中,氢氧化钙与氢氧化铝的摩尔比为1.8~2.2:1,碳酸钠与氢氧化铝的摩尔比为0.45~0.75:1,豆渣与氢氧化铝的质量比为1~3.5:10,水与氢氧化铝的质量比为10~200:1;
(2)加入表面改性剂,在70~100℃继续反应10~25小时,将反应得到的固体物脱水干燥后,得到改性水铝钙石-豆渣;
所述表面改性剂为硬脂酸钠、硬脂酸锌、油酸钠、聚乙二醇和环氧大豆油中的一种或多种。
进一步的,所述表面改性剂与氢氧化铝的质量比为1~3:10。
本发明提供的技术方案以豆渣、氢氧化钙、氢氧化铝和碳酸钠为原料,加入表面改性剂后,通过水热反应,在豆渣表面原位自组装合成水铝钙石,从而得到分散均匀的改性水铝钙石-豆渣复合材料。豆渣组分中含有纤维素、蛋白质和脂肪等主要组分,豆渣及其水解产物中含有丰富的羟基和胺基基团,具有抑制“锌烧”的作用。水铝钙石可消耗PVC热降解释放的氯化氢,从而抑制PVC的热降解。与现有技术相比,本发明提供的技术方案具有以下优点:(1)所涉及的改性水铝钙石-豆渣对PVC的热稳定性能非常优异,且优于传统的改性水铝钙石,体现出良好的协同作用;(2)以豆渣为原材料制备的改性水铝钙石-豆渣的生产成本低廉;(3)为豆渣的高值化利用提供了新的方法。
具体实施方式
下面对本发明的具体实施方式作进一步的详细说明。对于所属技术领域的技术人员而言,从对本发明的详细说明中,本发明的上述和其他目的、特征和优点将显而易见。
实施例1
将2.23 g Na2CO3(0.021 mol)溶于150 mL水中配制成溶液,加入5.92 g氢氧化钙(0.08 mol)、3.12 g氢氧化铝(0.04 mol)和0.8 g豆渣,搅拌条件下在80℃反应1小时;加入0.7 g硬脂酸钠,在90℃继续反应19小时,将反应得到的固体物脱水干燥后,得到改性水铝钙石-豆渣。
实施例2
将3.18 g Na2CO3(0.03 mol)溶于300 mL水中配制成溶液,加入6.51 g氢氧化钙(0.088 mol)、3.12 g氢氧化铝(0.04 mol)和1 g豆渣,搅拌条件下在95℃反应0.5小时;加入0.9 g聚乙二醇,在95℃继续反应15小时,将反应得到的固体物脱水干燥后,得到改性水铝钙石-豆渣。
实施例3
将1.91 g Na2CO3(0.018 mol)溶于100 mL水中配制成溶液,加入5.33 g氢氧化钙(0.072 mol)、3.12 g氢氧化铝(0.04 mol)和0.5 g豆渣,搅拌条件下在70℃反应3小时;加入0.4 g环氧大豆油,在70℃继续反应25小时,将反应得到的固体物脱水干燥后,得到改性水铝钙石-豆渣。
比较例1
除未添加豆渣外,其余制备过程同实施例1,得到改性水铝钙石。
比较例2
将比较例1制备的改性水铝钙石与0.8 g豆渣进行物理混合,得到改性水铝钙石与豆渣的混合物。
性能测试实验:
将改性水铝钙石-豆渣与其它助剂混合均匀制成PVC用复合热稳定剂,其具体组成为(质量分数):改性水铝钙石-豆渣为73%,硬脂酸锌为15%, 1,3-二甲基-6-氨基脲嘧啶为3%,乙酰丙酮钙为1%,抗氧剂1010为1%,PE蜡为7%。
以改性水铝钙石-豆渣为主要成分制备的PVC复合热稳定剂的性能采用哈普RM-200A转矩流变仪测试,测试条件:料温190℃,实验载荷5 kg,转速35 rpm。测试样品组成:55份PVC(SG-3型)树脂,1.6份复合热稳定剂,12份CaCO3,5份CPE,1.6份钛白粉,0.2份季戊四醇硬脂酸酯,0.2份PE蜡,1份ACR。测试方法:在转矩流变仪中混炼10分钟后取出样品,采用色差仪测试初期白度,并另外取样测试动态热稳定时间。测试结果见表1。
表1:
从表1结果可知,以改性水铝钙石-豆渣为主组分的PVC复合热稳定剂既能显著抑制PVC的初期着色,使PVC制品具有较高的初期白度,又具有较长的动态热稳定时间,综合性能非常优异。从实施例1与比较例1的结果可知,改性水铝钙石-豆渣作为PVC热稳定剂的性能显著优于传统的改性水铝钙石。从实施例1与比较例2的结果可知,通过水热反应制备的改性水铝钙石-豆渣复合材料的性能也显著优于改性水铝钙石与豆渣的物理混合物。
豆渣组分中含有纤维素、蛋白质和脂肪等主要组分,豆渣及其水解产物中含有丰富的羟基和胺基基团,具有抑制“锌烧”的作用。水铝钙石可消耗PVC热降解释放的氯化氢,从而抑制PVC的热降解。通过水热反应,在豆渣表面原位自组装合成水铝钙石,从而得到分散均匀的改性水铝钙石-豆渣复合材料,作为PVC热稳定剂表现出良好的协同作用。
此外,以豆渣为原材料制备改性水铝钙石-豆渣基PVC热稳定剂,既可以降低PVC热稳定剂的生产成本,也为豆渣的高值化利用提供新的途径。
应当理解,本发明虽然已通过以上实施例进行了清楚说明,然而在不背离本发明精神及其实质的情况下,所属技术领域的技术人员当可根据本发明作出各种相应的变化和修正,但这些相应的变化和修正都应属于本发明的权利要求的保护范围。
Claims (2)
1.一种用于PVC热稳定剂的改性水铝钙石-豆渣的制备方法,其特征在于,包括以下步骤:
(1)将碳酸钠溶于水中,加入氢氧化钙、氢氧化铝和豆渣,搅拌条件下在70~100℃反应0.5~3小时;其中,氢氧化钙与氢氧化铝的摩尔比为1.8~2.2:1,碳酸钠与氢氧化铝的摩尔比为0.45~0.75:1,豆渣与氢氧化铝的质量比为1~3.5:10,水与氢氧化铝的质量比为10~200:1;
(2)加入表面改性剂,在70~100℃继续反应10~25小时,将反应得到的固体物脱水干燥后,得到改性水铝钙石-豆渣;
所述表面改性剂为硬脂酸钠、硬脂酸锌、油酸钠、聚乙二醇和环氧大豆油中的一种或多种。
2.根据权利要求1所述的用于PVC热稳定剂的改性水铝钙石-豆渣的制备方法,表面改性剂与氢氧化铝的质量比为1~3:10。
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CN110395753A (zh) * | 2019-07-06 | 2019-11-01 | 王志胜 | 一种粒度均匀高稳定类水滑石的制备方法 |
CN112322066A (zh) * | 2020-11-22 | 2021-02-05 | 邵阳天堂助剂化工有限公司 | Pvc用改性豆渣基环保型复合热稳定剂 |
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