CN113307523A - 一种制备溶水性炭黑的方法、溶水性炭黑及其应用 - Google Patents

一种制备溶水性炭黑的方法、溶水性炭黑及其应用 Download PDF

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CN113307523A
CN113307523A CN202110610164.6A CN202110610164A CN113307523A CN 113307523 A CN113307523 A CN 113307523A CN 202110610164 A CN202110610164 A CN 202110610164A CN 113307523 A CN113307523 A CN 113307523A
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虞立平
李亚红
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Anhui Delui New Materials Technology Co ltd
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Abstract

本发明提供一种制备溶水性炭黑的方法、溶水性炭黑及其应用，包括如下步骤：(1)将氧化石墨烯和炉法炭黑置于水中分散均匀，得分散液；以及(2)将步骤(1)所得的炭黑分散液在恒定温度25℃置于质量分数2.0‑2.5％的硝酸溶液中浸泡1.5时；(3)将步骤(2)所得的炭黑分散浸泡液经过固液分离、烘干得到亲水性炭黑；所述炭黑分散液的炭黑浓度为20‑100g/L；所述炉法炭黑的DBP吸收量为80‑100cm3/100g；所述炉法炭黑的氮吸附比表面积为100‑160m2/g；所述炉法炭黑的平均粒径为25‑30nm。本发明通过选择合适的炭黑，使用质量分数2.0‑2.5％的硝酸溶液，在合适的反应条件下，使其与炭黑进行液相氧化反应，使得氧化后的炭黑具有很好的亲水性，能够在水中具有优异的分散稳定性。

Description

一种制备溶水性炭黑的方法、溶水性炭黑及其应用
技术领域
本发明属于炭黑材料制备技术领域，具体为一种制备溶水性炭黑的方法、溶水性炭黑及其应用。
背景技术
碳黑(carbon black)，又名炭黑，是一种无定形碳。轻、松而极细的黑色粉末，表面积非常大，是含碳物质(煤、天然气、重油、燃料油等)在空气不足的条件下经不完全燃烧或受热分解而得的产物。
水溶性炭黑在建筑材料起到的作用是着色、填充作用,对炭黑的要求是黑度高,着色力强,长时间不变质,耐水冲洗,分散性能好的一款建筑材料专用炭黑，炭黑本身不溶于水，必须通过一定的工艺处理才能满足要求。
有鉴于此，特提出本发明。
发明内容
针对现有的技术方案存在的问题，本发明的目的在于提供一种制备溶水性炭黑的方法、溶水性炭黑及其应用。
为实现上述目的，本发明提供以下技术方案：
一种制备亲水性炭黑的方法，包括如下步骤：
(1)将氧化石墨烯和炉法炭黑置于水中分散均匀，得分散液；以及
(2)将步骤(1)所得的炭黑分散液在恒定温度25℃置于质量分数2.0-2.5％的硝酸溶液中浸泡1.5时；
(3)将步骤(2)所得的炭黑分散浸泡液经过固液分离、烘干得到亲水性炭黑；
所述炉法炭黑的pH值为7-10；
所述炭黑分散液的炭黑浓度为20-100g/L；
所述炉法炭黑的DBP吸收量为80-100cm3/100g；
所述炉法炭黑的氮吸附比表面积为100-160m2/g；
所述炉法炭黑的平均粒径为25-30nm；
所述炉法炭黑与所述硝酸溶液搅拌接触，方式为机械搅拌或超声波搅拌；
所述固液分离为离心分离或过滤分离。
本发明还公开了一种亲水性炭黑，通过上述制备方法获得。
本发明还提供一种根据上述亲水性炭黑在建筑颜料中的应用。
本发明还公开了一种建筑颜料，通过如下方法制备：
(1)将上述的亲水性炭黑研磨制备成着色层涂料；
(2)取珠光颜料作为片状基材，珠光颜料以天然云母、合成云母、SiO2薄片或Al2 O3薄片为基片；
(3)将步骤(1)制备的着色层涂料和硅烷偶联剂混合包覆在步骤(2)片状基材上形成炭黑复合颜料。
进一步的，上述硅烷偶联剂不限于3-氨丙基三乙氧基硅烷；3-氨丙基三甲氧基硅烷；2-氨乙基-3-氨丙基三甲氧基硅烷；2-氨乙基-3-氨丙基甲基二甲氧基硅烷；2-氨乙基-3-氨丙基甲基二乙氧基硅烷。
与现有技术相比，本发明的有益效果是：本发明公开的方法通过选择合适的炭黑，使用质量分数2.0-2.5％的硝酸溶液，在合适的反应条件下，使其与炭黑进行液相氧化反应，使得氧化后的炭黑具有很好的亲水性，能够在水中具有优异的分散稳定性。
具体实施方式
下面将结合本发明实施例，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
取市售平均粒径为25-30nm炉法炭黑(DBP吸收量为90cm3/100g，氮吸附比表面积为140m2/g)300g和氧化石墨烯100g置于水中分散均匀，得分散液，将分散液加入到3L的质量分数2％的硝酸溶液中，在超声波清洗器(KH7200型)中超声振动，使得炭黑在次氯酸钠溶液中分散均匀，控制温度为25℃，持续保温搅拌反应1.5小时。待液相氧化反应结束，将炭黑溶液在离心机中进行脱水处理，控制离心机转速为9000rpm，将亲水性炭黑与水溶液分离。经烘干处理后，即得亲水性炭黑。
将得到的亲水性炭黑研磨制备成着色层涂料；取珠光颜料作为片状基材，珠光颜料以天然云母薄片为基片；将步骤制备的着色层涂料和硅烷偶联剂混合包覆在步骤片状基材上形成炭黑复合颜料，记为颜料Ⅰ。
实施例2
取市售平均粒径为25-30nm炉法炭黑(DBP吸收量为80cm3/100g，氮吸附比表面积为100m2/g)200g和氧化石墨烯100g置于水中分散均匀，得分散液，将分散液加入到4L的质量分数2％的硝酸溶液中，在超声波清洗器(KH7200型)中超声振动，使得炭黑在次氯酸钠溶液中分散均匀，控制温度为25℃，持续保温搅拌反应1.5小时。待液相氧化反应结束，将炭黑溶液在离心机中进行脱水处理，控制离心机转速为9000rpm，将亲水性炭黑与水溶液分离。经烘干处理后，即得亲水性炭黑。
将得到的亲水性炭黑研磨制备成着色层涂料；取珠光颜料作为片状基材，珠光颜料以SiO2薄片为基片；将步骤制备的着色层涂料和硅烷偶联剂混合包覆在步骤片状基材上形成炭黑复合颜料，记为颜料Ⅱ。
实施例3
取市售平均粒径为25-30nm炉法炭黑(DBP吸收量为100cm3/100g，氮吸附比表面积为160m2/g)400g和氧化石墨烯100g置于水中分散均匀，得分散液，将分散液加入到4L的质量分数2％的硝酸溶液中，在超声波清洗器(KH7200型)中超声振动，使得炭黑在次氯酸钠溶液中分散均匀，控制温度为25℃，持续保温搅拌反应1.5小时。待液相氧化反应结束，将炭黑溶液在离心机中进行脱水处理，控制离心机转速为9000rpm，将亲水性炭黑与水溶液分离。经烘干处理后，即得亲水性炭黑。
将得到的亲水性炭黑研磨制备成着色层涂料；取珠光颜料作为片状基材，珠光颜料以Al2O3薄片为基片；将步骤制备的着色层涂料和硅烷偶联剂混合包覆在步骤片状基材上形成炭黑复合颜料，记为颜料Ⅲ。
对比例1
将取市售平均粒径为25-30nm炉法炭黑(DBP吸收量为90cm3/100g，氮吸附比表面积为140m2/g)研磨制备成着色层涂料；取珠光颜料作为片状基材，珠光颜料以天然云母薄片为基片；将步骤制备的着色层涂料和硅烷偶联剂混合包覆在步骤片状基材上形成炭黑复合颜料，记为颜料Ⅳ。
对比例2
取市售平均粒径为25-30nm炉法炭黑(DBP吸收量为80cm3/100g，氮吸附比表面积为100m2/g)研磨制备成着色层涂料；取珠光颜料作为片状基材，珠光颜料以SiO2薄片为基片；将步骤制备的着色层涂料和硅烷偶联剂混合包覆在步骤片状基材上形成炭黑复合颜料，记为颜料Ⅴ。
对比例3
取市售平均粒径为25-30nm炉法炭黑(DBP吸收量为100cm3/100g，氮吸附比表面积为160m2/g)研磨制备成着色层涂料；取珠光颜料作为片状基材，珠光颜料以Al2O3薄片为基片；将步骤制备的着色层涂料和硅烷偶联剂混合包覆在步骤片状基材上形成炭黑复合颜料，记为颜料Ⅵ。
施例1-3所获得的亲水性炭黑烘干后，表面松软，烧杯壁不在析出白色晶体，不需要纯化和分级后处理，可以直接应用。
亲水性炭黑的沉降稳定性分析
对获得的亲水性炭黑进行沉降稳定性分析，将一定量的未氧化的炉法炭黑和亲水性炭黑分别加入到水中摇匀，观察炭黑溶液的变化情况。经过观察，发现样品静置7天后，未氧化的炉法炭黑溶液完全分层，上层溶液完全透明；亲水性炭黑溶液均匀，未出现分层现象。
表1为未经氧化的炉法炭黑与实施例1-3获得的亲水性炭黑的粒度及电位情况。
表1未经氧化的炉法炭黑与实施例1-3获得的亲水性炭黑的粒度及电位情况
为氧化炭黑 实施例1 实施例2 实施例3
CB HCB-1 HCB-2 HCB-3
粒度(nm) 300.2 156.6 145.2 152.3
电位(mV 26.3 -35.2 -32.5 -39.6
注：CB表示市售炉法炭黑
HCB表示亲水性炭黑
结论
经过氧化后的炭黑粒度下降，炭黑溶液的电位值由正值变为负值，表明炭黑在水中的分散稳定性极大提高。
表2为实施例1-3与对比例1-3获得的颜料黑度高，着色力，耐水冲洗性和热稳定性情况。
Figure BDA0003095586210000051
Figure BDA0003095586210000061
着色力采用(ISD，按德国工业标准DIN53.235测试)；
耐水冲洗性按照耐迁移性：测试按照德国工业标准DIN53.775进行；
热稳定性颜色的变化用ISO105A02 1-5级灰卡评价；
结论，通过本发明实施例和对比例的性能参数可以得出，通过亲水性炭黑制备的颜料，其黑度高，着色力强，具有很好的耐水冲洗性和热稳定性。
以上内容仅仅是对本发明结构所作的举例和说明，所属本技术领域的技术人员对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代，只要不偏离本发明的结构或者超越本权利要求书所定义的范围，均应属于本发明的保护范围。

Claims (5)

1.一种制备亲水性炭黑的方法，包括如下步骤：
(1)将氧化石墨烯和炉法炭黑置于水中分散均匀，得分散液；以及
(2)将步骤(1)所得的炭黑分散液在恒定温度25℃置于质量分数2.0-2.5％的硝酸溶液中浸泡1.5时；
(3)将步骤(2)所得的炭黑分散浸泡液经过固液分离、烘干得到亲水性炭黑；
所述炉法炭黑的pH值为7-10；
所述炭黑分散液的炭黑浓度为20-100g/L；
所述炉法炭黑的DBP吸收量为80-100cm3/100g；
所述炉法炭黑的氮吸附比表面积为100-160m2/g；
所述炉法炭黑的平均粒径为25-30nm；
所述炉法炭黑与所述硝酸溶液搅拌接触，方式为机械搅拌或超声波搅拌；
所述固液分离为离心分离或过滤分离。
2.一种亲水性炭黑，通过权利要求1的方法获得。
3.根据权利要求2的亲水性炭黑在建筑颜料中的应用。
4.一种建筑颜料，其特征在于，通过如下方法制备：
(1)将如权利要求2所述的亲水性炭黑研磨制备成着色层涂料；
(2)取珠光颜料作为片状基材，珠光颜料以天然云母、合成云母、SiO2薄片或Al2 O3薄片为基片；
(3)将步骤(1)制备的着色层涂料和硅烷偶联剂混合包覆在步骤(2)的片状基材上形成炭黑复合颜料。
5.根据权利要求4所述的一种建筑颜料，其特征在于，所述硅烷偶联剂不限于3-氨丙基三乙氧基硅烷；3-氨丙基三甲氧基硅烷；2-氨乙基-3-氨丙基三甲氧基硅烷；2-氨乙基-3-氨丙基甲基二甲氧基硅烷；2-氨乙基-3-氨丙基甲基二乙氧基硅烷。
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