CN114854203A - 一种石墨烯浆料的制备方法 - Google Patents
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Abstract
本发明公开了一种石墨烯浆料的制备方法,包括以下步骤:步骤一,石墨烯有机化处理:将石墨烯送入到硅烷偶联剂中,然后再加入丙酮溶剂进行搅拌调节,搅拌转速为100‑200r/min,搅拌时间为10‑20min,然后再加入树脂乳液,继续搅拌15‑25min,随后水洗、干燥。本发明通过对石墨烯进行有机化处理,处理中通过硅烷偶联剂和树脂乳进行联合处理,能够提高有机亲和度,界面剂采用有富马酸二甲酯、聚甲基丙烯酸异丁酯溶液、改性纳米粒共混处理,通过对活化的膨润土进一步的亲有机处理,同时富马酸二甲酯等原料可进一步的改善浆料的界面相容性。
Description
技术领域
本发明涉及石墨烯浆料技术领域,具体涉及一种石墨烯浆料的制备方法。
背景技术
石墨烯是一种由碳原子构成的单层片状结构的新材料。它是一种由碳原子以sp2杂化轨道组成六角型呈蜂巢晶格的平面薄膜,只有一个碳原子厚度的二维材料。石墨烯是目前进入应用领域中最薄的材料和最强韧的材料,还具有巨大的理论比表面积,物理化学性质稳定,可在高工作电压和大电流快速充放电下保持很好的结构稳定性,优异的导电性等等,使得石墨烯及其衍生物在储能材料,环境工程,灵敏传感方面被广泛应用,被称为“黑金”或是“新材料之王”。
现有的石墨烯浆料采用石墨烯无机料与有机原料进行共混处理,而二者之间界面相容性差,很难相容,反而降低浆料的性能。
发明内容
本发明的目的在于提供一种石墨烯浆料的制备方法,以解决上述背景技术中提出的问题。
为实现上述目的,本发明提供如下技术方案:
本发明提供了一种石墨烯浆料的制备方法,包括以下步骤:
步骤一,石墨烯有机化处理:将石墨烯送入到硅烷偶联剂中,然后再加入丙酮溶剂进行搅拌调节,搅拌转速为100-200r/min,搅拌时间为10-20min,然后再加入树脂乳液,继续搅拌15-25min,随后水洗、干燥;
步骤二,界面剂的制备:富马酸二甲酯加入到甲醇中,然后再加入聚甲基丙烯酸异丁酯溶液,随后再加入改性纳米粒,继续搅拌10-20min,搅拌转速为500-1000r/min,搅拌结束,得到界面剂;
步骤三,三维网状乳剂:将丙烯酸乳液加入到硅树脂中,然后进行低速搅拌10-20min,搅拌转速为100-200r/min,然后再加入莫来石粉进行杂化处理,杂化转速为500-600r/min,杂化时间为20-30min,得到三维网状乳剂;
步骤四,石墨烯浆料的制备:将有机化处理的石墨烯、界面剂与三维网状乳剂进行共混处理,然后再加入交联剂,辐照10-20min,得到石墨烯浆料。
优选地,所述树脂乳液为树脂乳与异构十一醇聚氧乙烯醚、邻苯甲酰磺酰亚胺进行共混处理,共混转速为50-100r/min,共混时间为10-20min,得到树脂乳液。
优选地,所述树脂乳为丙烯酸酯乳液、苯乙烯-丙烯酸酯乳液和硅丙乳液的一种或多种。
优选地,所述聚甲基丙烯酸异丁酯溶液的浓度为3-7%。
优选地,所述聚甲基丙烯酸异丁酯溶液的浓度为5%。
优选地,所述改性纳米粒的制备方法为:将膨润土送入到无水乙醇和去离子水中浸泡并超声处理,功率为200-300W,处理时间20-30min,然后用氮气吹干后置于体积比为3:1的70-75%浓硫酸/30-35%过氧化氢混合液中,加热至92-94℃,处理1-2h,处理结束,再水洗,干燥,得到改性纳米粒。
优选地,所述莫来石粉的粒径为30-60mm。
优选地,所述交联剂为过氧化二异丙苯、过氧化苯甲酰中的一种。
优选地,所述步骤四中辐照处理采用质子辐照,辐照功率为210-250W。
与现有技术相比,本发明具有如下的有益效果:
本发明通过对石墨烯进行有机化处理,处理中通过硅烷偶联剂和树脂乳进行联合处理,能够提高有机亲和度,界面剂采用富马酸二甲酯、聚甲基丙烯酸异丁酯溶液、改性纳米粒共混处理,通过对活化的膨润土进一步的亲有机处理,同时富马酸二甲酯等原料可进一步的改善浆料的界面相容性,三维网状乳剂采用丙烯酸乳液、硅树脂和莫来石进行杂化处理,硅树脂与丙烯酸乳液形成三维网状体,而石墨烯和膨润土均具有片层结构,穿插到网状体中提高网状体的稳定性,同时通过莫来石进一步的杂化,进而提高产品的有机、无机双性能,完善产品的界面相容性,从而提高浆料的综合性能。
具体实施方式
下面结合具体实施例,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。
实施例1:
本实施例的一种石墨烯浆料的制备方法,包括以下步骤:
步骤一,石墨烯有机化处理:将石墨烯送入到硅烷偶联剂中,然后再加入丙酮溶剂进行搅拌调节,搅拌转速为100r/min,搅拌时间为10min,然后再加入树脂乳液,继续搅拌15min,随后水洗、干燥;
步骤二,界面剂的制备:富马酸二甲酯加入到甲醇中,然后再加入聚甲基丙烯酸异丁酯溶液,随后再加入改性纳米粒,继续搅拌10min,搅拌转速为500r/min,搅拌结束,得到界面剂;
步骤三,三维网状乳剂:将丙烯酸乳液加入到硅树脂中,然后进行低速搅拌10min,搅拌转速为100r/min,然后再加入莫来石粉进行杂化处理,杂化转速为500r/min,杂化时间为20min,得到三维网状乳剂;
步骤四,石墨烯浆料的制备:将有机化处理的石墨烯、界面剂与三维网状乳剂进行共混处理,然后再加入交联剂,辐照10min,得到石墨烯浆料。
本实施例的树脂乳液为树脂乳与异构十一醇聚氧乙烯醚、邻苯甲酰磺酰亚胺进行共混处理,共混转速为50r/min,共混时间为10min,得到树脂乳液。
本实施例的树脂乳为丙烯酸酯乳液、苯乙烯-丙烯酸酯乳液和硅丙乳液的一种或多种。
本实施例的聚甲基丙烯酸异丁酯溶液的浓度为3%。
本实施例的改性纳米粒的制备方法为:将膨润土送入到无水乙醇和去离子水中浸泡并超声处理,功率为200W,处理时间20min,然后用氮气吹干后置于体积比为3:1的70%浓硫酸/30%过氧化氢混合液中,加热至92℃,处理1h,处理结束,再水洗,干燥,得到改性纳米粒。
本实施例的莫来石粉的粒径为30mm。
本实施例的交联剂为过氧化二异丙苯。
本实施例的步骤四中辐照处理采用质子辐照,辐照功率为210W。
实施例2:
本实施例的一种石墨烯浆料的制备方法,包括以下步骤:
步骤一,石墨烯有机化处理:将石墨烯送入到硅烷偶联剂中,然后再加入丙酮溶剂进行搅拌调节,搅拌转速为200r/min,搅拌时间为20min,然后再加入树脂乳液,继续搅拌25min,随后水洗、干燥;
步骤二,界面剂的制备:富马酸二甲酯加入到甲醇中,然后再加入聚甲基丙烯酸异丁酯溶液,随后再加入改性纳米粒,继续搅拌20min,搅拌转速为1000r/min,搅拌结束,得到界面剂;
步骤三,三维网状乳剂:将丙烯酸乳液加入到硅树脂中,然后进行低速搅拌20min,搅拌转速为200r/min,然后再加入莫来石粉进行杂化处理,杂化转速为600r/min,杂化时间为30min,得到三维网状乳剂;
步骤四,石墨烯浆料的制备:将有机化处理的石墨烯、界面剂与三维网状乳剂进行共混处理,然后再加入交联剂,辐照20min,得到石墨烯浆料。
本实施例的树脂乳液为树脂乳与异构十一醇聚氧乙烯醚、邻苯甲酰磺酰亚胺进行共混处理,共混转速为100r/min,共混时间为20min,得到树脂乳液。
本实施例的树脂乳为丙烯酸酯乳液、苯乙烯-丙烯酸酯乳液和硅丙乳液的一种或多种。
本实施例的聚甲基丙烯酸异丁酯溶液的浓度为7%。
本实施例的改性纳米粒的制备方法为:将膨润土送入到无水乙醇和去离子水中浸泡并超声处理,功率为300W,处理时间30min,然后用氮气吹干后置于体积比为3:1的75%浓硫酸/35%过氧化氢混合液中,加热至94℃,处理2h,处理结束,再水洗,干燥,得到改性纳米粒。
本实施例的莫来石粉的粒径为60mm。
本实施例的交联剂为过氧化二异丙苯。
优选地,所述步骤四中辐照处理采用质子辐照,辐照功率为250W。
实施例3:
本实施例的一种石墨烯浆料的制备方法,包括以下步骤:
步骤一,石墨烯有机化处理:将石墨烯送入到硅烷偶联剂中,然后再加入丙酮溶剂进行搅拌调节,搅拌转速为150r/min,搅拌时间为15min,然后再加入树脂乳液,继续搅拌20min,随后水洗、干燥;
步骤二,界面剂的制备:富马酸二甲酯加入到甲醇中,然后再加入聚甲基丙烯酸异丁酯溶液,随后再加入改性纳米粒,继续搅拌15min,搅拌转速为750r/min,搅拌结束,得到界面剂;
步骤三,三维网状乳剂:将丙烯酸乳液加入到硅树脂中,然后进行低速搅拌15min,搅拌转速为150r/min,然后再加入莫来石粉进行杂化处理,杂化转速为550r/min,杂化时间为25min,得到三维网状乳剂;
步骤四,石墨烯浆料的制备:将有机化处理的石墨烯、界面剂与三维网状乳剂进行共混处理,然后再加入交联剂,辐照15min,得到石墨烯浆料。
本实施例的树脂乳液为树脂乳与异构十一醇聚氧乙烯醚、邻苯甲酰磺酰亚胺进行共混处理,共混转速为75r/min,共混时间为15min,得到树脂乳液。
本实施例的树脂乳为丙烯酸酯乳液、苯乙烯-丙烯酸酯乳液和硅丙乳液的一种或多种。
本实施例的聚甲基丙烯酸异丁酯溶液的浓度为5%。
本实施例的改性纳米粒的制备方法为:将膨润土送入到无水乙醇和去离子水中浸泡并超声处理,功率为250W,处理时间25min,然后用氮气吹干后置于体积比为3:1的72.5%浓硫酸/32.5%过氧化氢混合液中,加热至93℃,处理1.5h,处理结束,再水洗,干燥,得到改性纳米粒。
本实施例的莫来石粉的粒径为45mm。
本实施例的交联剂为过氧化二异丙苯。
本实施例的步骤四中辐照处理采用质子辐照,辐照功率为230W。
对比例1:
采用市场上四川德阳生产的DYXT-GD101/DYXT-GZ101型号的防腐涂料。
采用实施例1-3及对比例1的方法制备的产品进行测试;
组别 | 耐15%盐酸(天) |
实施例1 | 65 |
实施例2 | 68 |
实施例3 | 69 |
对比例1 | 31 |
实施例1-3及对比例1可看出,本发明产品耐15%盐酸高达69天。
对于本领域技术人员而言,显然本发明不限于上述示范性实施例的细节,而且在不背离本发明的精神或基本特征的情况下,能够以其他的具体形式实现本发明。因此,无论从哪一点来看,均应将实施例看作是示范性的,而且是非限制性的,本发明的范围由所附权利要求而不是上述说明限定,因此旨在将落在权利要求的等同要件的含义和范围内的所有变化囊括在本发明内。
此外,应当理解,虽然本说明书按照实施方式加以描述,但并非每个实施方式仅包含一个独立的技术方案,说明书的这种叙述方式仅仅是为清楚起见,本领域技术人员应当将说明书作为一个整体,各实施例中的技术方案也可以经适当组合,形成本领域技术人员可以理解的其他实施方式。
Claims (9)
1.一种石墨烯浆料的制备方法,其特征在于,包括以下步骤:
步骤一,石墨烯有机化处理:将石墨烯送入到硅烷偶联剂中,然后再加入丙酮溶剂进行搅拌调节,搅拌转速为100-200r/min,搅拌时间为10-20min,然后再加入树脂乳液,继续搅拌15-25min,随后水洗、干燥;
步骤二,界面剂的制备:富马酸二甲酯加入到甲醇中,然后再加入聚甲基丙烯酸异丁酯溶液,随后再加入改性纳米粒,继续搅拌10-20min,搅拌转速为500-1000r/min,搅拌结束,得到界面剂;
步骤三,三维网状乳剂:将丙烯酸乳液加入到硅树脂中,然后进行低速搅拌10-20min,搅拌转速为100-200r/min,然后再加入莫来石粉进行杂化处理,杂化转速为500-600r/min,杂化时间为20-30min,得到三维网状乳剂;
步骤四,石墨烯浆料的制备:将有机化处理的石墨烯、界面剂与三维网状乳剂进行共混处理,然后再加入交联剂,辐照10-20min,得到石墨烯浆料。
2.根据权利要求1所述的一种石墨烯浆料的制备方法,其特征在于,所述树脂乳液为树脂乳与异构十一醇聚氧乙烯醚、邻苯甲酰磺酰亚胺进行共混处理,共混转速为50-100r/min,共混时间为10-20min,得到树脂乳液。
3.根据权利要求2所述的一种石墨烯浆料的制备方法,其特征在于,所述树脂乳为丙烯酸酯乳液、苯乙烯-丙烯酸酯乳液和硅丙乳液的一种或多种。
4.根据权利要求1所述的一种石墨烯浆料的制备方法,其特征在于,所述聚甲基丙烯酸异丁酯溶液的浓度为3-7%。
5.根据权利要求4所述的一种石墨烯浆料的制备方法,其特征在于,所述聚甲基丙烯酸异丁酯溶液的浓度为5%。
6.根据权利要求1所述的一种石墨烯浆料的制备方法,其特征在于,所述改性纳米粒的制备方法为:将膨润土送入到无水乙醇和去离子水中浸泡并超声处理,功率为200-300W,处理时间20-30min,然后用氮气吹干后置于体积比为3:1的70-75%浓硫酸/30-35%过氧化氢混合液中,加热至92-94℃,处理1-2h,处理结束,再水洗,干燥,得到改性纳米粒。
7.根据权利要求1所述的一种石墨烯浆料的制备方法,其特征在于,所述莫来石粉的粒径为30-60mm。
8.根据权利要求1所述的一种石墨烯浆料的制备方法,其特征在于,所述交联剂为过氧化二异丙苯、过氧化苯甲酰中的一种。
9.根据权利要求1所述的一种石墨烯浆料的制备方法,其特征在于,所述步骤四中辐照处理采用质子辐照,辐照功率为210-250W。
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