CN117417569B - 一种玻璃纤维复合材料及其制备方法 - Google Patents
一种玻璃纤维复合材料及其制备方法 Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 40
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 38
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- 239000004408 titanium dioxide Substances 0.000 claims abstract description 19
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- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 12
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- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims abstract description 10
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims abstract description 10
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- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims description 15
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- AAKBLFQBZDFKMP-UHFFFAOYSA-H trimagnesium azane diphosphate Chemical compound N.[Mg+2].[Mg+2].[Mg+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O AAKBLFQBZDFKMP-UHFFFAOYSA-H 0.000 abstract description 2
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Abstract
本发明公开了一种玻璃纤维复合材料及其制备方法,通过二氧化钛与硅烷偶联剂进行反应,在二氧化钛表面引入活性氨基基团,再通过氨基基团与丁二酸酐进行反应,氨基与丁二酸酐开环,从而在二氧化钛表面引入大量的活性羧基和硅烷基,提高了二氧化钛与聚丙烯树脂的相容性,进而增强了复合材料的抗静电性能,同时引入的硅烷基在燃烧过程中使得所生成的炭层结构更致密稳定,达到阻燃效果,然后利用硝酸镁、硝酸锰和磷酸氨进行反应,在聚丙烯树脂的表面负载掺杂锰离子的磷酸氨镁,磷酸氨镁在分解过程中吸热并且反应生成不可燃气体,从而使得可燃物的浓度降低,同时生成的二氧化锰具有吸附烟气的作用,减少有毒烟气的产生,进一步提高了阻燃效果。
Description
技术领域
本发明涉及高分子材料技术领域,具体涉及一种玻璃纤维复合材料及其制备方法。
背景技术
玻璃纤维是一种具有优异性能的无机非金属材料,产品具有良好的绝缘性、较强的耐热性和抗腐蚀性以及高强度等特性被广泛应用,同时,它与热固性树脂或者热塑性树脂等有机材料复合形成的玻璃纤维复合材料,被广泛应用于国民经济的各个领域。
玻璃纤维复合材料在实际应用时其抗静电性能和阻燃性能表现在各个领域都较为重要,因此,如何开发兼具抗静电性能和阻燃性能的玻璃纤维复合材料成为本领域技术人员的研究重点,中国专利CN202210090567.7公开了一种一种阻燃型玻璃纤维复合材料及其制备方法,在确保玻璃纤维自身性能不受影响的前提下降低玻璃纤维熔点,增强玻璃纤维阻燃性,玻璃纤维拉丝顺利,最终制得的玻璃纤维复合材料耐火性能好,韧性好,但上述专利所制备的玻璃纤维材料并不具备抗静电性能。
发明内容
针对现有技术的不足,本发明的目的在于提供一种玻璃纤维复合材料及其制备方法,在确保玻璃纤维自身性能不受影响的前提下,增强玻璃纤维的阻燃性能和抗静电性能。
为了实现上述目的,本发明采取如下技术方案:
一种玻璃纤维复合材料的制备方法,包括如下步骤:
(1)将双氧水加入到玻璃纤维中,搅拌均匀,然后加热回流反应,反应结束后,将反应产物进行过滤、洗涤、干燥,即得到羟基化玻璃纤维;
(2)将二氧化钛超声分散在乙醇溶剂中,然后加入硅烷偶联剂,混合均匀,再加入丁二酸酐,室温下搅拌反应2-3h,待反应完成后,将所得产物进行洗涤、干燥,即得到改性二氧化钛;
(3)将聚丙烯树脂加入到去离子水中,超声分散均匀,然后加入硝酸镁、硝酸锰、磷酸氨,用氨水调节溶液pH为9-10,进行搅拌反应,待反应完成后,将反应产物进行过滤、洗涤、干燥,即得到改性聚丙烯树脂;
(4)将改性聚丙烯树脂、改性二氧化钛、六氢苯二甲酸酐、N,N'-乙撑双硬脂酰胺、羧甲基纤维素混合均匀,在双螺杆挤出机中加热至熔融,得到熔融体,将所得熔融体放置在容置槽内,再将羟基化玻璃纤维送入容置槽中,浸润3-5min,然后冷却、切粒,即得玻璃纤维复合材料。
优选的,步骤(1)中,双氧水与玻璃纤维的质量比为20-30:1。
优选的,步骤(1)中,加热回流反应温度为105-110℃,加热回流反应时间为3-5h。
优选的,步骤(2)中,二氧化钛、硅烷偶联剂和丁二酸酐的质量比为5-8:3-5:4-6。
优选的,步骤(2)中,硅烷偶联剂为KH560或KH570。
优选的,步骤(3)中,聚丙烯树脂、硝酸镁、硝酸锰、磷酸氨的质量比为80-100:8-15:4-6:10-20。
优选的,步骤(3)中,搅拌反应温度为40-60℃,搅拌反应时间为2-4h。
优选的,步骤(4)中,改性聚丙烯树脂、改性二氧化钛、六氢苯二甲酸酐、N,N'-乙撑双硬脂酰胺、羧甲基纤维素的质量比为10:2-3:0.5-1:0.1-0.3:0.2-0.4。
优选的,步骤(4)中,羟基化玻璃纤维与改性聚丙烯树脂的质量比为3-6:10。
本发明还提供由上述制备方法所制备得到的玻璃纤维复合材料。
与现有技术相比,本发明具有如下有益效果:
(1)本发明通过二氧化钛与硅烷偶联剂进行反应,在二氧化钛表面引入活性氨基基团,再通过氨基基团与丁二酸酐进行反应,氨基与丁二酸酐开环,从而在二氧化钛表面引入大量的活性羧基和硅烷基,提高了二氧化钛与聚丙烯树脂的相容性,进而增强了复合材料的抗静电性能,同时引入的硅烷基在燃烧过程中使得所生成的炭层结构更致密稳定,阻断了与空气的接触,形成一层耐热保护层,避免高分子材料进一步发生热分解,达到阻燃效果。
(2)本发明利用硝酸镁、硝酸锰和磷酸氨进行反应,在聚丙烯树脂的表面负载掺杂锰离子的磷酸氨镁,磷酸氨镁在分解过程中吸热并且反应生成不可燃气体,从而使得可燃物的浓度降低,同时生成的二氧化锰具有吸附烟气的作用,减少有毒烟气的产生,进一步提高了阻燃效果。
(3)本发明通过引入改性二氧化钛、六氢苯二甲酸酐、N,N'-乙撑双硬脂酰胺和羧甲基纤维素,增强了熔融体的阻燃性能和韧性,同时通过对玻璃纤维进行羟基化改性,增强了玻璃纤维与熔融体的界面相容性,使得最终形成的玻璃纤维复合材料具有优异的阻燃性能、抗静电性能和拉伸强度。
具体实施方式
以下通过具体较佳实施例对本发明作进一步详细说明,但本发明并不仅限于以下的实施例。
需要说明的是,无特殊说明外,本发明中涉及到的化学试剂均通过商业渠道购买。
本发明中所使用的玻璃纤维购自五河县维佳复合材料有限公司,单丝直径为11-17μm,颗粒长径比为13:1;
二氧化钛购自东莞市沃海贸易有限公司,型号为R-FC5钛白粉;
聚丙烯树脂购自上海优晟塑胶有限公司,牌号为PPB-M02-G。
实施例1
一种玻璃纤维复合材料的制备方法,包括如下步骤:
(1)将200g,30wt%的双氧水加入到10g玻璃纤维中,搅拌均匀,然后在105℃下加热回流反应3h,反应结束后,将反应产物进行过滤、洗涤、干燥,即得到羟基化玻璃纤维;
(2)将5g二氧化钛超声分散在150mL乙醇溶剂中,然后加入3g硅烷偶联剂KH560,混合均匀,再加入4g丁二酸酐,室温下搅拌反应2h,待反应完成后,将所得产物进行洗涤、干燥,即得到改性二氧化钛;
(3)将8g聚丙烯树脂加入到150g去离子水中,超声分散均匀,然后加入0.8g硝酸镁、0.4g硝酸锰、1g磷酸氨,用氨水调节溶液pH为10,在40℃下搅拌反应2h,待反应完成后,将反应产物进行过滤、洗涤、干燥,即得到改性聚丙烯树脂;
(4)将10g改性聚丙烯树脂、2g改性二氧化钛、0.5g六氢苯二甲酸酐、0.1g N,N'-乙撑双硬脂酰胺、0.2g羧甲基纤维素混合均匀,在双螺杆挤出机中加热至230℃,熔融混合,得到熔融体,将所得熔融体放置在容置槽内,再将3g羟基化玻璃纤维送入容置槽中,浸润3min,然后冷却、切粒,即得玻璃纤维复合材料,切粒后颗粒的长度为10mm,直径为4mm。
实施例2
一种玻璃纤维复合材料的制备方法,包括如下步骤:
(1)将300g,30wt%的双氧水加入到10g玻璃纤维中,搅拌均匀,然后在110℃下加热回流反应5h,反应结束后,将反应产物进行过滤、洗涤、干燥,即得到羟基化玻璃纤维;
(2)将8g二氧化钛超声分散在150mL乙醇溶剂中,然后加入5g硅烷偶联剂KH560,混合均匀,再加入6g丁二酸酐,室温下搅拌反应3h,待反应完成后,将所得产物进行洗涤、干燥,即得到改性二氧化钛;
(3)将10g聚丙烯树脂加入到150g去离子水中,超声分散均匀,然后加入1.5g硝酸镁、0.6g硝酸锰、2g磷酸氨,用氨水调节溶液pH为10,在60℃下搅拌反应4h,待反应完成后,将反应产物进行过滤、洗涤、干燥,即得到改性聚丙烯树脂;
(4)将10g改性聚丙烯树脂、3g改性二氧化钛、1g六氢苯二甲酸酐、0.3g N,N'-乙撑双硬脂酰胺、0.4g羧甲基纤维素混合均匀,在双螺杆挤出机中加热至230℃,熔融混合,得到熔融体,将所得熔融体放置在容置槽内,再将6g羟基化玻璃纤维送入容置槽中,浸润5min,然后冷却、切粒,即得玻璃纤维复合材料,切粒后颗粒的长度为10mm,直径为4mm。
实施例3
一种玻璃纤维复合材料的制备方法,包括如下步骤:
(1)将250g,30wt%的双氧水加入到10g玻璃纤维中,搅拌均匀,然后在105℃下加热回流反应5h,反应结束后,将反应产物进行过滤、洗涤、干燥,即得到羟基化玻璃纤维;
(2)将6g二氧化钛超声分散在150mL乙醇溶剂中,然后加入4g硅烷偶联剂KH570,混合均匀,再加入6g丁二酸酐,室温下搅拌反应3h,待反应完成后,将所得产物进行洗涤、干燥,即得到改性二氧化钛;
(3)将10g聚丙烯树脂加入到150g去离子水中,超声分散均匀,然后加入1.2g硝酸镁、0.5g硝酸锰、1.5g磷酸氨,用氨水调节溶液pH为10,在50℃下搅拌反应3h,待反应完成后,将反应产物进行过滤、洗涤、干燥,即得到改性聚丙烯树脂;
(4)将10g改性聚丙烯树脂、2.5g改性二氧化钛、0.8g六氢苯二甲酸酐、0.3g N,N'-乙撑双硬脂酰胺、0.3g羧甲基纤维素混合均匀,在双螺杆挤出机中加热至230℃,熔融混合,得到熔融体,将所得熔融体放置在容置槽内,再将4g羟基化玻璃纤维送入容置槽中,浸润5min,然后冷却、切粒,即得玻璃纤维复合材料,切粒后颗粒的长度为10mm,直径为4mm。
对比例1
一种玻璃纤维复合材料的制备方法,包括如下步骤:
(1)将300g,30wt%的双氧水加入到10g玻璃纤维中,搅拌均匀,然后在110℃下加热回流反应5h,反应结束后,将反应产物进行过滤、洗涤、干燥,即得到羟基化玻璃纤维;
(2)将10g聚丙烯树脂加入到150g去离子水中,超声分散均匀,然后加入1.5g硝酸镁、0.6g硝酸锰、2g磷酸氨,用氨水调节溶液pH为10,在60℃下搅拌反应4h,待反应完成后,将反应产物进行过滤、洗涤、干燥,即得到改性聚丙烯树脂;
(3)将10g改性聚丙烯树脂、3g二氧化钛、1g六氢苯二甲酸酐、0.3g N,N'-乙撑双硬脂酰胺、0.4g羧甲基纤维素混合均匀,在双螺杆挤出机中加热至230℃,熔融混合,得到熔融体,将所得熔融体放置在容置槽内,再将6g羟基化玻璃纤维送入容置槽中,浸润5min,然后冷却、切粒,即得玻璃纤维复合材料,切粒后颗粒的长度为10mm,直径为4mm。
对比例2
一种玻璃纤维复合材料的制备方法,包括如下步骤:
(1)将300g,30wt%的双氧水加入到10g玻璃纤维中,搅拌均匀,然后在110℃下加热回流反应5h,反应结束后,将反应产物进行过滤、洗涤、干燥,即得到羟基化玻璃纤维;
(2)将8g二氧化钛超声分散在150mL乙醇溶剂中,然后加入5g硅烷偶联剂KH560,混合均匀,再加入6g丁二酸酐,室温下搅拌反应3h,待反应完成后,将所得产物进行洗涤、干燥,即得到改性二氧化钛;
(3)将10g聚丙烯树脂、3g改性二氧化钛、1g六氢苯二甲酸酐、0.3g N,N'-乙撑双硬脂酰胺、0.4g羧甲基纤维素混合均匀,在双螺杆挤出机中加热至230℃,熔融混合,得到熔融体,将所得熔融体放置在容置槽内,再将6g羟基化玻璃纤维送入容置槽中,浸润5min,然后冷却、切粒,即得玻璃纤维复合材料,切粒后颗粒的长度为10mm,直径为4mm。
对实施例1-3和对比例1-2所制备的玻璃纤维复合材料进行力学性能、抗静电以及阻燃性能测试,其中表面电阻率按照GB/T 31838.3-2019标准进行测试,拉伸强度根据GB/T1040-2006标准进行测试,标准样品为1A型,试验速度为10mm/min,每组测试3个试样,计算平均值,得到拉伸强度;极限氧指数按照GB/T 2406.2-2009进行测试,制成试样尺寸为Ⅰ类型的样条,点燃方法为A,试验结果如下表所示:
最后需要说明的是:以上实施例不以任何形式限制本发明。对本领域技术人员来说,在本发明基础上,可以对其作一些修改和改进。因此,凡在不偏离本发明精神的基础上所做的任何修改或改进,均属于本发明要求保护的范围之内。
Claims (5)
1.一种玻璃纤维复合材料的制备方法,其特征在于,包括如下步骤:
(1)将双氧水加入到玻璃纤维中,搅拌均匀,然后加热回流反应,反应结束后,将反应产物进行过滤、洗涤、干燥,即得到羟基化玻璃纤维;
(2)将二氧化钛超声分散在乙醇溶剂中,然后加入硅烷偶联剂,混合均匀,再加入丁二酸酐,室温下搅拌反应2-3h,待反应完成后,将所得产物进行洗涤、干燥,即得到改性二氧化钛;
(3)将聚丙烯树脂加入到去离子水中,超声分散均匀,然后加入硝酸镁、硝酸锰、磷酸氨,用氨水调节溶液pH为9-10,进行搅拌反应,待反应完成后,将反应产物进行过滤、洗涤、干燥,即得到改性聚丙烯树脂;
(4)将改性聚丙烯树脂、改性二氧化钛、六氢苯二甲酸酐、N,N'-乙撑双硬脂酰胺、羧甲基纤维素混合均匀,在双螺杆挤出机中加热至熔融,得到熔融体,将所得熔融体放置在容置槽内,再将羟基化玻璃纤维送入容置槽中,浸润3-5min,然后冷却、切粒,即得玻璃纤维复合材料;
其中,步骤(1)中,双氧水与玻璃纤维的质量比为20-30:1;
步骤(2)中,二氧化钛、硅烷偶联剂和丁二酸酐的质量比为5-8:3-5:4-6;
步骤(3)中,聚丙烯树脂、硝酸镁、硝酸锰、磷酸氨的质量比为80-100:8-15:4-6:10-20;
步骤(4)中,改性聚丙烯树脂、改性二氧化钛、六氢苯二甲酸酐、N,N'-乙撑双硬脂酰胺、羧甲基纤维素的质量比为10:2-3:0.5-1:0.1-0.3:0.2-0.4;
步骤(4)中,羟基化玻璃纤维与改性聚丙烯树脂的质量比为3-6:10。
2.根据权利要求1所述的制备方法,其特征在于,步骤(1)中,加热回流反应温度为105-110℃,加热回流反应时间为3-5h。
3.根据权利要求1所述的制备方法,其特征在于,步骤(2)中,硅烷偶联剂为KH560或KH570。
4.根据权利要求1所述的制备方法,其特征在于,步骤(3)中,搅拌反应温度为40-60℃,搅拌反应时间为2-4h。
5.如权利要求1-4任一项所述制备方法所制备得到的玻璃纤维复合材料。
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