CN111188195A - 一种氮化硅纤维表面处理剂及其制备方法 - Google Patents

一种氮化硅纤维表面处理剂及其制备方法 Download PDF

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CN111188195A
CN111188195A CN202010035355.XA CN202010035355A CN111188195A CN 111188195 A CN111188195 A CN 111188195A CN 202010035355 A CN202010035355 A CN 202010035355A CN 111188195 A CN111188195 A CN 111188195A
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许健根
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Guangdong Dongfang Yige New Materials Co ltd
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Abstract

本发明公开了一种氮化硅纤维表面处理剂及其制备方法，该表面处理剂包括以下按照重量份的原料：聚四氟乙烯34‑49份、聚二甲基二烯丙基氯化铵17‑28份、尿素9‑17份、乙氧基化脂肪族烷基胺8‑14份、亲水油剂2‑6份、助剂1.6‑3.9份、增稠剂2‑6份。本发明的表面处理剂在各组分的协同作用下能够有效作用于氮化硅纤维，增强氮化硅纤维的耐高温性能，避免其在高温下发生分解而使强度产生下降，保证其作为耐高温材料的有效使用，同时不会对氮化硅限位的其他性能产生太大影响。

Description

一种氮化硅纤维表面处理剂及其制备方法
技术领域
本发明涉及纤维原料相关领域，具体是一种氮化硅纤维表面处理剂及其制备方法。
背景技术
氮化硅纤维一种耐高温、高强度陶瓷纤维，其化学式为Si3N4，具有类似于碳化硅纤维的力学性能和应用领域，耐化学腐蚀和耐高温性能好，是高性能陶瓷基复合材料的增强纤维之一。该材料是未来航天航空、汽车发动机等耐高温部件最有希望的候选材料，有着广泛的应用前景。
虽然氮化硅纤维的各项性能较为优异，但是仍存在一定的缺陷，比如其在作为耐高温材料时，由于碳化硅纤维由于含有较多的SixCyOz相，故在高温时容易发生分解而使强度急剧下降，因此有必要对碳化硅纤维进行一定的预处理，而较为常见的方式就是利用表面处理剂对碳化硅纤维进行处理。
发明内容
本发明的目的在于提供一种氮化硅纤维表面处理剂及其制备方法，以解决上述问题。
为实现上述目的，本发明提供如下技术方案：
一种氮化硅纤维表面处理剂，包括以下按照重量份的原料：聚四氟乙烯34-49份、聚二甲基二烯丙基氯化铵17-28份、尿素9-17份、乙氧基化脂肪族烷基胺8-14份、亲水油剂2-6份、助剂1.6-3.9份、增稠剂2-6份。
在进一步的方案中：包括以下按照重量份的原料：聚四氟乙烯39-44份、聚二甲基二烯丙基氯化铵20-25份、尿素11-15份、乙氧基化脂肪族烷基胺10-12份、亲水油剂3-5份、助剂2.1-3.3份、增稠剂3-5份。
在进一步的方案中：包括以下按照重量份的原料：聚四氟乙烯42份、聚二甲基二烯丙基氯化铵22份、尿素13份、乙氧基化脂肪族烷基胺11份、亲水油剂4份、助剂2.8份、增稠剂4份。
在进一步的方案中：所述亲水油剂由硅油剂、自乳化硅油、双氨基硅油和聚醚硅油中的至少两种混合而成。
在进一步的方案中：所述亲水油剂由硅油剂和双氨基硅油按照重量比4:3混合而成。
在进一步的方案中：所述助剂为丙二醇、丁醚、乙二醇丁、乙二醇或叔丁醇。
在进一步的方案中：所述增稠剂由羧甲基纤维素和丙二醇藻蛋白酸酯按照重量比1:2混合而成。
所述氮化硅纤维表面处理剂的制备方法，包括以下步骤：
1)将聚二甲基二烯丙基氯化铵溶于质量倍是其2-4倍的去离子水，充分搅拌，分散均匀后得到聚二甲基二烯丙基氯化铵溶液备用；
2)将聚四氟乙烯和乙氧基化脂肪族烷基胺混合，升温至56-71℃，并在该温度下搅拌12-17min，然后再升温至102-115℃，继续搅拌5-9min，得到混合物A；
3)在混合物A中加入聚二甲基二烯丙基氯化铵溶液，混合均匀后再加入尿素，升温至95-107℃，超声波处理5-11min，得到混合物B；
4)在混合物B中加入亲水油剂、助剂和增稠剂，在常温下混合均匀，即得所述氮化硅纤维表面处理剂。
在进一步的方案中：所述步骤3)中超声波功率为800-1100W。
在进一步的方案中：所述步骤3)中聚二甲基二烯丙基氯化铵溶液分至少两次计入到混合物中，加入期间不断搅拌。
相较于现有技术，本发明的有益效果如下：
本发明的表面处理剂在各组分的协同作用下能够有效作用于氮化硅纤维，增强氮化硅纤维的耐高温性能，避免其在高温下发生分解而使强度产生下降，保证其作为耐高温材料的有效使用，同时不会对氮化硅限位的其他性能产生太大影响。
具体实施方式
本发明所列举的各实施例仅用以说明本发明，并非用以限制本发明的范围。对本发明所作的任何显而易知的修饰或变更都不脱离本发明的精神与范围。
实施例1
本发明实施例中，一种氮化硅纤维表面处理剂，包括以下按照重量份的原料：聚四氟乙烯34份、聚二甲基二烯丙基氯化铵17份、尿素9份、乙氧基化脂肪族烷基胺8份、亲水油剂2份、助剂1.6份、增稠剂2份。
其中所述亲水油剂由硅油剂和自乳化硅油按照重量比1:1混合而成；所述助剂为丙二醇；所述增稠剂由羧甲基纤维素和丙二醇藻蛋白酸酯按照重量比1:2混合而成。
本实施例中所述氮化硅纤维表面处理剂的制备方法，包括以下步骤：
1)将聚二甲基二烯丙基氯化铵溶于质量倍是其2倍的去离子水，充分搅拌，分散均匀后得到聚二甲基二烯丙基氯化铵溶液备用；
2)将聚四氟乙烯和乙氧基化脂肪族烷基胺混合，升温至56℃，并在该温度下搅拌12min，然后再升温至102℃，继续搅拌5min，得到混合物A；
3)在混合物A中加入聚二甲基二烯丙基氯化铵溶液，混合均匀后再加入尿素，升温至95℃，超声波处理5min，得到混合物B；
4)在混合物B中加入亲水油剂、助剂和增稠剂，在常温下混合均匀，即得所述氮化硅纤维表面处理剂。
其中，所述步骤3)中超声波功率为800W；所述步骤3)中聚二甲基二烯丙基氯化铵溶液分至少两次计入到混合物中，加入期间不断搅拌。
实施例2
本发明实施例中，一种氮化硅纤维表面处理剂，包括以下按照重量份的原料：聚四氟乙烯39份、聚二甲基二烯丙基氯化铵20份、尿素11份、乙氧基化脂肪族烷基胺10份、亲水油剂3份、助剂2.1份、增稠剂3份。
其中所述亲水油剂由硅油剂和双氨基硅油按照重量比2:3混合而成；所述助剂为丁醚；所述增稠剂由羧甲基纤维素和丙二醇藻蛋白酸酯按照重量比1:2混合而成。
本实施例中所述氮化硅纤维表面处理剂的制备方法，包括以下步骤：
1)将聚二甲基二烯丙基氯化铵溶于质量倍是其2.5倍的去离子水，充分搅拌，分散均匀后得到聚二甲基二烯丙基氯化铵溶液备用；
2)将聚四氟乙烯和乙氧基化脂肪族烷基胺混合，升温至66℃，并在该温度下搅拌14min，然后再升温至108℃，继续搅拌7min，得到混合物A；
3)在混合物A中加入聚二甲基二烯丙基氯化铵溶液，混合均匀后再加入尿素，升温至102℃，超声波处理7min，得到混合物B；
4)在混合物B中加入亲水油剂、助剂和增稠剂，在常温下混合均匀，即得所述氮化硅纤维表面处理剂。
其中，所述步骤3)中超声波功率为900W；所述步骤3)中聚二甲基二烯丙基氯化铵溶液分至少两次计入到混合物中，加入期间不断搅拌。
实施例3
本发明实施例中，一种氮化硅纤维表面处理剂，包括以下按照重量份的原料：聚四氟乙烯42份、聚二甲基二烯丙基氯化铵22份、尿素13份、乙氧基化脂肪族烷基胺11份、亲水油剂4份、助剂2.8份、增稠剂4份。
其中所述亲水油剂由硅油剂和双氨基硅油按照重量比4:3混合而成；所述助剂乙二醇丁；所述增稠剂由羧甲基纤维素和丙二醇藻蛋白酸酯按照重量比1:2混合而成。
本实施例中所述氮化硅纤维表面处理剂的制备方法，包括以下步骤：
1)将聚二甲基二烯丙基氯化铵溶于质量倍是其3.5倍的去离子水，充分搅拌，分散均匀后得到聚二甲基二烯丙基氯化铵溶液备用；
2)将聚四氟乙烯和乙氧基化脂肪族烷基胺混合，升温至67℃，并在该温度下搅拌16min，然后再升温至109℃，继续搅拌8min，得到混合物A；
3)在混合物A中加入聚二甲基二烯丙基氯化铵溶液，混合均匀后再加入尿素，升温至103℃，超声波处理8min，得到混合物B；
4)在混合物B中加入亲水油剂、助剂和增稠剂，在常温下混合均匀，即得所述氮化硅纤维表面处理剂。
其中，所述步骤3)中超声波功率为1000W；所述步骤3)中聚二甲基二烯丙基氯化铵溶液分至少两次计入到混合物中，加入期间不断搅拌。
实施例4
本发明实施例中，一种氮化硅纤维表面处理剂，包括以下按照重量份的原料：聚四氟乙烯44份、聚二甲基二烯丙基氯化铵23份、尿素13份、乙氧基化脂肪族烷基胺14份、亲水油剂4份、助剂2.5份、增稠剂4份。
其中所述亲水油剂由双氨基硅油和聚醚硅油中按照重量比3:4混合而成；所述助剂为叔丁醇；所述增稠剂由羧甲基纤维素和丙二醇藻蛋白酸酯按照重量比1:2混合而成。
本实施例中所述氮化硅纤维表面处理剂的制备方法，包括以下步骤：
1)将聚二甲基二烯丙基氯化铵溶于质量倍是其3.5倍的去离子水，充分搅拌，分散均匀后得到聚二甲基二烯丙基氯化铵溶液备用；
2)将聚四氟乙烯和乙氧基化脂肪族烷基胺混合，升温至58℃，并在该温度下搅拌15min，然后再升温至110℃，继续搅拌8min，得到混合物A；
3)在混合物A中加入聚二甲基二烯丙基氯化铵溶液，混合均匀后再加入尿素，升温至102℃，超声波处理8min，得到混合物B；
4)在混合物B中加入亲水油剂、助剂和增稠剂，在常温下混合均匀，即得所述氮化硅纤维表面处理剂。
其中，所述步骤3)中超声波功率为950W；所述步骤3)中聚二甲基二烯丙基氯化铵溶液分至少两次计入到混合物中，加入期间不断搅拌。
实施例5
本发明实施例中，一种氮化硅纤维表面处理剂，包括以下按照重量份的原料：聚四氟乙烯44份、聚二甲基二烯丙基氯化铵25份、尿素15份、乙氧基化脂肪族烷基胺12份、亲水油剂5份、助剂3.3份、增稠剂5份。
其中所述亲水油剂由硅油剂和双氨基硅油按照重量比1:2混合而成；所述助剂为丙二醇；所述增稠剂由羧甲基纤维素和丙二醇藻蛋白酸酯按照重量比1:2混合而成。
本实施例中所述氮化硅纤维表面处理剂的制备方法，包括以下步骤：
1)将聚二甲基二烯丙基氯化铵溶于质量倍是其4倍的去离子水，充分搅拌，分散均匀后得到聚二甲基二烯丙基氯化铵溶液备用；
2)将聚四氟乙烯和乙氧基化脂肪族烷基胺混合，升温至69℃，并在该温度下搅拌15min，然后再升温至113℃，继续搅拌8min，得到混合物A；
3)在混合物A中加入聚二甲基二烯丙基氯化铵溶液，混合均匀后再加入尿素，升温至103℃，超声波处理9min，得到混合物B；
4)在混合物B中加入亲水油剂、助剂和增稠剂，在常温下混合均匀，即得所述氮化硅纤维表面处理剂。
其中，所述步骤3)中超声波功率为1100W；所述步骤3)中聚二甲基二烯丙基氯化铵溶液分至少两次计入到混合物中，加入期间不断搅拌。
实施例6
本发明实施例中，一种氮化硅纤维表面处理剂，包括以下按照重量份的原料：聚四氟乙烯49份、聚二甲基二烯丙基氯化铵28份、尿素17份、乙氧基化脂肪族烷基胺14份、亲水油剂6份、助剂3.9份、增稠剂6份。
其中所述亲水油剂由自乳化硅油和聚醚硅油按照重量比3:2混合而成；所述助剂为乙二醇；所述增稠剂由羧甲基纤维素和丙二醇藻蛋白酸酯按照重量比1:2混合而成。
本实施例中所述氮化硅纤维表面处理剂的制备方法，包括以下步骤：
1)将聚二甲基二烯丙基氯化铵溶于质量倍是其4倍的去离子水，充分搅拌，分散均匀后得到聚二甲基二烯丙基氯化铵溶液备用；
2)将聚四氟乙烯和乙氧基化脂肪族烷基胺混合，升温至71℃，并在该温度下搅拌17min，然后再升温至115℃，继续搅拌9min，得到混合物A；
3)在混合物A中加入聚二甲基二烯丙基氯化铵溶液，混合均匀后再加入尿素，升温至107℃，超声波处理11min，得到混合物B；
4)在混合物B中加入亲水油剂、助剂和增稠剂，在常温下混合均匀，即得所述氮化硅纤维表面处理剂。
其中，所述步骤3)中超声波功率为1100W；所述步骤3)中聚二甲基二烯丙基氯化铵溶液分至少两次计入到混合物中，加入期间不断搅拌。
本发明的作用机理是：
本发明的表面处理剂在各组分的协同作用下能够有效作用于氮化硅纤维，增强氮化硅纤维的耐高温性能，避免其在高温下发生分解而使强度产生下降，保证其作为耐高温材料的有效使用，同时不会对氮化硅限位的其他性能产生太大影响
以上所述，仅为本公开的具体实施方式，但本公开的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本公开揭露的技术范围内，可轻易想到变化或替换，都应涵盖在本公开的保护范围之内。因此，本公开的保护范围应以权利要求的保护范围为准。

Claims (10)

1.一种氮化硅纤维表面处理剂，其特征在于，包括以下按照重量份的原料：聚四氟乙烯34-49份、聚二甲基二烯丙基氯化铵17-28份、尿素9-17份、乙氧基化脂肪族烷基胺8-14份、亲水油剂2-6份、助剂1.6-3.9份、增稠剂2-6份。
2.根据权利要求1所述的氮化硅纤维表面处理剂，其特征在于，包括以下按照重量份的原料：聚四氟乙烯39-44份、聚二甲基二烯丙基氯化铵20-25份、尿素11-15份、乙氧基化脂肪族烷基胺10-12份、亲水油剂3-5份、助剂2.1-3.3份、增稠剂3-5份。
3.根据权利要求3所述的氮化硅纤维表面处理剂，其特征在于，包括以下按照重量份的原料：聚四氟乙烯42份、聚二甲基二烯丙基氯化铵22份、尿素13份、乙氧基化脂肪族烷基胺11份、亲水油剂4份、助剂2.8份、增稠剂4份。
4.根据权利要求1所述的氮化硅纤维表面处理剂，其特征在于，所述亲水油剂由硅油剂、自乳化硅油、双氨基硅油和聚醚硅油中的至少两种混合而成。
5.根据权利要求4所述的氮化硅纤维表面处理剂，其特征在于，所述亲水油剂由硅油剂和双氨基硅油按照重量比4:3混合而成。
6.根据权利要求1所述的氮化硅纤维表面处理剂，其特征在于，所述助剂丙二醇、丁醚、乙二醇丁、乙二醇或叔丁醇。
7.根据权利要求1所述的氮化硅纤维表面处理剂，其特征在于，所述增稠剂由羧甲基纤维素和丙二醇藻蛋白酸酯按照重量比1:2混合而成。
8.根据权利要求1-7任一所述的氮化硅纤维表面处理剂的制备方法，其特征在于，包括以下步骤：
1)将聚二甲基二烯丙基氯化铵溶于质量倍是其2-4倍的去离子水，充分搅拌，分散均匀后得到聚二甲基二烯丙基氯化铵溶液备用；
2)将聚四氟乙烯和乙氧基化脂肪族烷基胺混合，升温至56-71℃，并在该温度下搅拌12-17min，然后再升温至102-115℃，继续搅拌5-9min，得到混合物A；
3)在混合物A中加入聚二甲基二烯丙基氯化铵溶液，混合均匀后再加入尿素，升温至95-107℃，超声波处理5-11min，得到混合物B；
4)在混合物B中加入亲水油剂、助剂和增稠剂，在常温下混合均匀，即得所述氮化硅纤维表面处理剂。
9.根据权利要求8所述的氮化硅纤维表面处理剂的制备方法，其特征在于，所述步骤3)中超声波功率为800-1100W。
10.根据权利要求8所述的氮化硅纤维表面处理剂的制备方法，其特征在于，所述步骤3)中聚二甲基二烯丙基氯化铵溶液分至少两次计入到混合物中，加入期间不断搅拌。
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