CN117229566A - 一种高效抗紫外硫醇锑复合热稳定剂 - Google Patents
一种高效抗紫外硫醇锑复合热稳定剂 Download PDFInfo
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- YIHGLFOSXSDHNR-UHFFFAOYSA-N 1-(4-tert-butylphenyl)-3-(4-methoxyphenyl)propane-1,3-dione;1,3-diphenylpropane-1,3-dione Chemical compound C=1C=CC=CC=1C(=O)CC(=O)C1=CC=CC=C1.C1=CC(OC)=CC=C1C(=O)CC(=O)C1=CC=C(C(C)(C)C)C=C1 YIHGLFOSXSDHNR-UHFFFAOYSA-N 0.000 claims description 2
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Abstract
本发明提供了一种高效抗紫外硫醇锑复合热稳定剂,具体涉及PVC改性技术领域,以重量百分含量计,包括如下组分:三‑(巯基乙酸异辛酯)锑45%~90%、五‑(巯基乙酸异辛酯)锑0%~55%、紫外线吸收剂0.5%~1.5%、抗析出剂1%~10%、增塑剂2%~6%、增溶剂1%~2%。本发明提供的高效抗紫外硫醇锑复合热稳定剂具有无毒、价格较低且不易变色的优点。
Description
本申请是名为《一种高效抗紫外硫醇锑复合热稳定剂》的专利申请的分案申请,原申请的申请日为2021年09月02日,申请号为202111027656.9。
技术领域
本发明涉及PVC改性技术领域,特别是涉及一种高效抗紫外硫醇锑复合热稳定剂。
背景技术
聚氯乙烯树脂(PVC)结构不稳定,在加工成型中容易降解。而降解会导致材料颜色逐渐加深和机械性能的丧失,所以在其加工过程中必须使用热稳定剂。
在众多的热稳定剂中,如铅、镉等重金属盐热稳定剂,虽然能有效的抑制PVC的降解,但其毒性较大,对环境和人的健康造成巨大影响,已逐渐被禁止使用。目前常用的有机锡热稳定剂无毒、初期着色和热稳定性优越,但其价格昂贵,使用成本较高。同时,硫醇锑是一种新型的PVC热稳定剂,具有良好的初期着色和长效热稳定性性能、价格低和无毒等优点,是目前昂贵有机锡热稳定剂的良好替代品。但目前使用的有机锑热稳定剂存在储存稳定性差和耐紫外光性能差等问题,导致添加有机锑热稳定剂的PVC制品在室外易变色,限制了其在PVC产业用的大规模使用。
故研发出一款无毒、价格较低且不易变色的PVC热稳定剂是技术人员亟待解决的问题。
发明内容
为了克服现有技术的不足,本发明的目的是提供一种高效抗紫外硫醇锑复合热稳定剂。
为实现上述目的,本发明提供了如下方案:
一种高效抗紫外硫醇锑复合热稳定剂,以重量百分含量计,包括如下组分:三-(巯基乙酸异辛酯)锑45%~90%、五-(巯基乙酸异辛酯)锑0%~55%、紫外线吸收剂0.5%~1.5%、抗析出剂1%~10%、增塑剂2%~6%、增溶剂1%~2%;
其中,紫外线吸收剂选自2-羟基-4-正辛氧基二苯甲酮、二苯甲酰甲烷1-[4-(1,1-二甲基乙基)苯基]-3-(4-甲氧基苯基)-1,3-丙二酮、甲氧型肉桂酸乙基己酯、双(2,4-二叔丁基苯基)季戊四醇二磷酸酯中的任意一种,或是选自:2-羟基-4-正辛氧基二苯甲酮和二苯甲酰甲烷质量比为1:1的混合物、2-羟基-4-正辛氧基二苯甲酮和1-[4-(1,1-二甲基乙基)苯基]-3-(4-甲氧基苯基)-1,3-丙二酮质量比为1:1的混合物、2-羟基-4-正辛氧基二苯甲酮和甲氧型肉桂酸乙基己酯质量比为1:1的混合物、2-羟基-4-正辛氧基二苯甲酮和双(2,4-二叔丁基苯基)季戊四醇二磷酸酯质量比为1:1的混合物中的任意一种;抗析出剂选自油醇聚氧乙烯醚-3-磷酸酯、苯酚、邻苯二酚中的任意一种,或是选自:邻苯二酚与油醇聚氧乙烯醚-3-磷酸酯质量比为1:1的混合物、邻苯二酚和苯酚质量比为1:1的混合物中的任意一种;增塑剂选自环氧大豆油和邻苯二甲酸二辛脂中的任意一种,或是环氧大豆油和邻苯二甲酸二辛脂以质量比为1:1的混合物;增溶剂选自聚氧乙烯脱水山梨醇单油酸酯和十三烷醇聚醚-10-磷酸酯中的任意一种,或是聚氧乙烯脱水山梨醇单油酸酯和十三烷醇聚醚-10-磷酸酯以质量比为1:1的的混合物;
三-(巯基乙酸异辛酯)锑的结构式如式(1):
三-(巯基乙酸异辛酯)锑的制备方法为:
将三氧化二锑和巯基乙酸异辛酯以物质的量比为1:6.0~7.2混合均匀,加入催化剂A,在反应溶剂中60℃~120℃的温度条件下,反应3~5小时,减压蒸馏脱水,过滤,得到三-(巯基乙酸异辛酯)锑;
五-(巯基乙酸异辛酯)锑的结构式如式(2):
五-(巯基乙酸异辛酯)锑的制备方法为:
将五氧化二锑和巯基乙酸异辛酯以物质的量比为1:10~12混合均匀,加入催化剂B,在反应溶剂中60℃~120℃的温度条件下,反应3~5小时,减压蒸馏脱水,过滤,得到五-(巯基乙酸异辛酯)锑;
催化剂A和催化剂B均选自SO4 2-/TiO2、SO4 2-/Al2O3、SO4 2-/TiO2-Al2O3、强酸性阳离子交换树脂和全氟磺酸树脂中的任意一种,所述催化剂A和催化剂B的添加量为5%~10%;反应温度为80℃;反应溶剂选自苯、甲苯和水中的任意一种;反应溶剂选自水;五-(巯基乙酸异辛酯)锑的产率为96%~98%。
与现有技术相比,本发明的有益效果是:
与目前市场上现有硫醇锑热稳定剂相比,本发明所得的复合硫醇锑的综合性能及性价比大大提升,产品具有优异的初期着色和长期热稳定性,抗紫外线效果和储存稳定性好,太阳光下长时间爆嗮不变黑和长期放置不析出,PVC加工制品透明度高且抗黄变效果好,解决了传统硫醇锑热稳剂存在储存稳定性差和耐紫外光性能差等问题。
(2)本发明所得硫醇锑复合热稳定剂初期着色和长期热稳定性与甲基锡相当,可替代价格昂贵的甲基锡单独用于PVC透明制品的加工,性价比大大提升。
(3)本发明所得硫醇锑复合热稳定剂的制备工艺简单、绿色环保,反应产率高,催化剂可循环使用,原料简单易得,适合工业化大生产。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案,下面将对实施例中所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅仅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性的前提下,还可以根据这些附图获得其他的附图。
图1为硫醇锑复合热稳定剂动态热稳定性测试示意图;
图2为硫醇锑复合热稳定剂抗紫外性能测试示意图。
具体实施方式
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
在本文中提及“实施例”意味着,结合实施例描述的特定特征、结构或特性可以包含在本申请的至少一个实施例中。在说明书中的各个位置出现该短语并不一定均是指相同的实施例,也不是与其它实施例互斥的独立的或备选的实施例。本领域技术人员显式地和隐式地理解的是,本文所描述的实施例可以与其它实施例相结合。
为使本发明的上述目的、特征和优点能够更加明显易懂,下面结合附图和具体实施方式对本发明作进一步详细的说明。
实施案例1
一种高效抗紫外硫醇锑复合热稳定剂的制备方法,包括下述步骤:
在装有搅拌器、回流冷凝装置的250mL的三口烧瓶中,加入49.04g巯基乙酸异辛酯、11.66g三氧化二锑粉末和2.46gSO4 2-/TiO2催化剂,在80℃条件下反应3小时,停止搅拌加热、冷却、减压蒸馏后过滤得到淡绿色的三-(巯基乙酸异辛酯)锑,产率为96%。
实施案例2
一种高效抗紫外硫醇锑复合热稳定剂的制备方法,包括下述步骤:
在装有搅拌器、回流冷凝装置的250mL的三口烧瓶中,加入58.85g巯基乙酸异辛酯、11.66g三氧化二锑粉末和2.46gSO4 2-/TiO2催化剂,在80℃条件下反应3小时,停止搅拌加热、冷却、减压蒸馏后过滤得到淡绿色的三-(巯基乙酸异辛酯)锑,产率为97%。
实施案例3
一种高效抗紫外硫醇锑复合热稳定剂的制备方法,包括下述步骤:
在装有搅拌器、回流冷凝装置的250mL的三口烧瓶中,加入40.87g巯基乙酸异辛酯、6.47g五氧化二锑粉末和2.0gSO4 2-/Al2O3催化剂,在80℃条件下反应3小时,停止搅拌加热、冷却、减压蒸馏后过滤得到淡绿色的五-(巯基乙酸异辛酯)锑,产率为97%。
实施案例4
一种高效抗紫外硫醇锑复合热稳定剂的制备方法,包括下述步骤:
在装有搅拌器、回流冷凝装置的250mL的三口烧瓶中,加入49.04g巯基乙酸异辛酯、6.47g五氧化二锑粉末和2.0gSO4 2-/Al2O3催化剂,在80℃条件下反应3小时,停止搅拌加热、冷却、减压蒸馏后过滤得到淡绿色的五-(巯基乙酸异辛酯)锑,产率为98%。
产品复配案例
案例1:在装有搅拌器、回流冷凝管装置的250mL三口烧瓶中,加入10g上述合成的三-(巯基乙酸异辛酯)锑,依次分别加入0.1g2-羟基-4-正辛氧基二苯甲酮、0.1g邻苯二酚、0.2g邻苯二甲酸二辛脂和0.1g十三烷醇聚醚-10-磷酸酯,加入完毕后升温至50-60℃搅拌30分钟,冷却即可得硫醇锑复合热稳定剂。
案例2:在装有搅拌器、回流冷凝管装置的250mL三口烧瓶中,加入9g上述合成的三-(巯基乙酸异辛酯)锑和1g五-(巯基乙酸异辛酯)锑,依次分别加入0.1g二苯甲酰甲烷、0.1g苯酚、0.2g环氧大豆油和0.1g十三烷醇聚醚-10-磷酸酯,加入完毕后升温至50-60℃搅拌30分钟,冷却即可得硫醇锑复合热稳定剂。
测试例1
将100gPVC树脂与0.8g合成的硫醇锑复合热稳定剂混合均匀,在开放式塑炼机上混炼,温度为195±2℃,转子速度为40r/min,记录PVC塑化到分解的时间,结果表明混炼时间长达22分钟,如图1所示。
测试例2
将本发明所得硫醇锑复合热稳定剂与市场上现有的硫醇锑产品HTM2080分别装入塑料瓶中在太阳光下暴晒,记录产品的变黑时间,对应产品的抗紫外效果。研究结果表明,太阳下暴晒930分钟都不变黑,如图2所示。
本说明书中各个实施例采用递进的方式描述,每个实施例重点说明的都是与其他实施例的不同之处,各个实施例之间相同相似部分互相参见即可。
本文中应用了具体个例对本发明的原理及实施方式进行了阐述,以上实施例的说明只是用于帮助理解本发明的方法及其核心思想;同时,对于本领域的一般技术人员,依据本发明的思想,在具体实施方式及应用范围上均会有改变之处。综上所述,本说明书内容不应理解为对本发明的限制。
Claims (1)
1.一种高效抗紫外硫醇锑复合热稳定剂,其特征在于,以重量百分含量计,包括如下组分:三-(巯基乙酸异辛酯)锑45%~90%、五-(巯基乙酸异辛酯)锑0%~55%、紫外线吸收剂0.5%~1.5%、抗析出剂1%~10%、增塑剂2%~6%、增溶剂1%~2%;
其中,紫外线吸收剂选自2-羟基-4-正辛氧基二苯甲酮、二苯甲酰甲烷1-[4-(1,1-二甲基乙基)苯基]-3-(4-甲氧基苯基)-1,3-丙二酮、甲氧型肉桂酸乙基己酯、双(2,4-二叔丁基苯基)季戊四醇二磷酸酯中的任意一种,或是选自:2-羟基-4-正辛氧基二苯甲酮和二苯甲酰甲烷质量比为1:1的混合物、2-羟基-4-正辛氧基二苯甲酮和1-[4-(1,1-二甲基乙基)苯基]-3-(4-甲氧基苯基)-1,3-丙二酮质量比为1:1的混合物、2-羟基-4-正辛氧基二苯甲酮和甲氧型肉桂酸乙基己酯质量比为1:1的混合物、2-羟基-4-正辛氧基二苯甲酮和双(2,4-二叔丁基苯基)季戊四醇二磷酸酯质量比为1:1的混合物中的任意一种;抗析出剂选自油醇聚氧乙烯醚-3-磷酸酯、苯酚、邻苯二酚中的任意一种,或是选自:邻苯二酚与油醇聚氧乙烯醚-3-磷酸酯质量比为1:1的混合物、邻苯二酚和苯酚质量比为1:1的混合物中的任意一种;增塑剂选自环氧大豆油和邻苯二甲酸二辛脂中的任意一种,或是环氧大豆油和邻苯二甲酸二辛脂以质量比为1:1的混合物;增溶剂选自聚氧乙烯脱水山梨醇单油酸酯和十三烷醇聚醚-10-磷酸酯中的任意一种,或是聚氧乙烯脱水山梨醇单油酸酯和十三烷醇聚醚-10-磷酸酯以质量比为1:1的的混合物;
三-(巯基乙酸异辛酯)锑的结构式如式(1):
三-(巯基乙酸异辛酯)锑的制备方法为:
将三氧化二锑和巯基乙酸异辛酯以物质的量比为1:6.0~7.2混合均匀,加入催化剂A,在反应溶剂中60℃~120℃的温度条件下,反应3~5小时,减压蒸馏脱水,过滤,得到三-(巯基乙酸异辛酯)锑;
五-(巯基乙酸异辛酯)锑的结构式如式(2):
五-(巯基乙酸异辛酯)锑的制备方法为:
将五氧化二锑和巯基乙酸异辛酯以物质的量比为1:10~12混合均匀,加入催化剂B,在反应溶剂中60℃~120℃的温度条件下,反应3~5小时,减压蒸馏脱水,过滤,得到五-(巯基乙酸异辛酯)锑;
催化剂A和催化剂B均选自SO4 2-/TiO2、SO4 2-/Al2O3、SO4 2-/TiO2-Al2O3、强酸性阳离子交换树脂和全氟磺酸树脂中的任意一种,所述催化剂A和催化剂B的添加量为5%~10%;反应温度为80℃;反应溶剂选自苯、甲苯和水中的任意一种;反应溶剂选自水;五-(巯基乙酸异辛酯)锑的产率为96%~98%。
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