CN115247002A - 一种导静电氧化锌的制备方法 - Google Patents
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 102
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 46
- 230000003068 static effect Effects 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000006185 dispersion Substances 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims description 28
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 24
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims description 18
- 239000011259 mixed solution Substances 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000000243 solution Substances 0.000 claims description 17
- 238000005406 washing Methods 0.000 claims description 13
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 238000001354 calcination Methods 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims description 8
- DAMJCWMGELCIMI-UHFFFAOYSA-N benzyl n-(2-oxopyrrolidin-3-yl)carbamate Chemical compound C=1C=CC=CC=1COC(=O)NC1CCNC1=O DAMJCWMGELCIMI-UHFFFAOYSA-N 0.000 claims description 8
- 239000000725 suspension Substances 0.000 claims description 8
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 7
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 230000007935 neutral effect Effects 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 4
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- 239000012065 filter cake Substances 0.000 claims description 4
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 4
- 238000003828 vacuum filtration Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000003760 magnetic stirring Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 230000008569 process Effects 0.000 claims description 2
- 239000000843 powder Substances 0.000 abstract description 8
- 239000000049 pigment Substances 0.000 abstract description 7
- 239000002245 particle Substances 0.000 abstract description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 5
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 4
- 239000000919 ceramic Substances 0.000 abstract description 3
- 239000003973 paint Substances 0.000 abstract description 3
- 239000005060 rubber Substances 0.000 abstract description 3
- 239000004065 semiconductor Substances 0.000 abstract description 3
- -1 ITO Chemical compound 0.000 abstract description 2
- 239000012752 auxiliary agent Substances 0.000 abstract description 2
- 239000011258 core-shell material Substances 0.000 abstract description 2
- 239000002657 fibrous material Substances 0.000 abstract description 2
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 2
- 239000011147 inorganic material Substances 0.000 abstract description 2
- 238000001556 precipitation Methods 0.000 abstract description 2
- 239000012463 white pigment Substances 0.000 abstract description 2
- 235000014692 zinc oxide Nutrition 0.000 description 33
- 238000012360 testing method Methods 0.000 description 10
- 238000000576 coating method Methods 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 4
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000007900 aqueous suspension Substances 0.000 description 3
- 239000011247 coating layer Substances 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 239000010445 mica Substances 0.000 description 3
- 229910052618 mica group Inorganic materials 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000004438 BET method Methods 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 239000011231 conductive filler Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 238000007561 laser diffraction method Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000003921 particle size analysis Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 229910052903 pyrophyllite Inorganic materials 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- CVNKFOIOZXAFBO-UHFFFAOYSA-J tin(4+);tetrahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[Sn+4] CVNKFOIOZXAFBO-UHFFFAOYSA-J 0.000 description 1
- 239000003039 volatile agent Substances 0.000 description 1
- 230000002087 whitening effect Effects 0.000 description 1
- RNWHGQJWIACOKP-UHFFFAOYSA-N zinc;oxygen(2-) Chemical class [O-2].[Zn+2] RNWHGQJWIACOKP-UHFFFAOYSA-N 0.000 description 1
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/04—Compounds of zinc
- C09C1/043—Zinc oxide
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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Abstract
本发明公开了一种导静电氧化锌的制备方法,本发明属于氧化锌技术领域,本发明公开的导静电氧化锌颜色呈浅的青白色,所以加入颜料中可实现商品的色彩多样化。通过降低颜料、助剂的使用量,可起到降低总成本的作用。且与导电性氧化钛、ITO、ATO等具有导电性能的无机材料相比,具有价格低廉的优点。导电氧化锌粉体粒子为球形,具有易分散、黏度低、沉淀结块率低的优点。它的每个粒子都是一个独立的半导体,所以在分散时粉体结构不容易被破坏,电阻值较稳定。PPy包覆在掺杂纳米氧化锌的表面,形成致密的核‑壳结构,形成立体导电通路,导静电氧化锌可用于涂料、橡胶、纤维材料和陶瓷中作为导静电的白色颜料。
Description
技术领域
本发明属于氧化锌技术领域,具体涉及一种导静电氧化锌的制备方法。
背景技术
随着航空航天、电子、医药、信息等国家战略工业的迅猛发展,人们的生产生活环境对防静电(静电击穿和灰尘控制)、电磁屏蔽功能的要求越来越高。常用的防静电方法为将导电粉体添加到基材中达到消除静电的效果,基体材料主要有橡胶、塑料、涂料、纺织品、陶瓷等。国内使用的导电填料主要有炭黑、导电性氧化钛、导电云母等。导电性炭黑的电阻率难以控制,而且由于本身的颜色,商品化的难度高;导电性氧化钛颜色浅、电阻低,但价格贵,针状结构使它在涂料配合时难分散,且黏度较高。导电云母以它的低电阻、低价格成为目前国内防静电涂料的主要导电材料。但在使用中发现有以下缺点:鳞片状结构,分散难,黏度较高;分散时容易破坏云母的层状结构,导致涂料的电阻值欠缺稳定性;导电涂料的颜色不均一,表面平滑性不好;涂料易沉淀,颜色为暗灰色,不利于明色产品。本领域技术人员亟待开发出一种导静电氧化锌的制备方法以满足现有的应用市场和性能需求。
发明内容
有鉴于此,本发明提供一种导静电氧化锌的制备方法。
一种导静电氧化锌的制备方法,包括以下步骤:第一步、称取纳米氧化锌粉体,加入去离子水中形成固含量30~40%的悬浮分散液,移入反应釜中,控制一定反应温度、pH值,在不断搅拌下滴加10~15%的四氯化锡和三氯化锑的盐酸混合液,同时滴加0.1~0.2mol/L的NaOH溶液,以保持溶液的pH值恒定,待混合液滴完后,再继续熟化30min,然后过滤,用去离子水洗涤至中性,过滤将滤饼60℃烘干至恒重,煅烧,得掺杂纳米氧化锌;第二步、吡咯减压蒸馏后,于0~4℃保存待用,量取6.5~7份吡咯于反应釜中,加入50份蒸馏水搅拌均匀乳液,向其中加入50份质量分数24~25%的对甲苯磺酸溶液混合均匀后,加入第一步得到的掺杂纳米氧化锌,浴比1∶6~8超声分散10~15min,再将混合溶液加入反应釜中,0℃条件下磁力搅拌8~10min,将质量分数16~17%的FeCl3水溶液逐滴加入上述反应釜中,滴加1~1.5h后,于0℃条件下持续5h后反应结束,真空抽滤后用甲醇洗涤2~3次,再用去离子水洗涤2~3次,于60℃干燥12h,即制得导静电氧化锌。
进一步的,所述第一步控制pH值恒定为1.0~2.0,反应温度70~80℃,滴加时间2~4h,其中纳米氧化锌、四氯化锡和三氯化锑的质量比为20~22∶7~9∶1。
进一步的,所述第一步煅烧工艺条件为煅烧温度580~600℃,煅烧时间1.5~2.0h。
进一步的,所述第一步的盐酸为质量浓度为7~9%的盐酸水溶液。
进一步的,所述第一步熟化为温度85~90℃下加热。
本发明的有益效果:
本发明以氧化锌为载体,采用非均匀成核法在其表面包覆一层锑掺杂的二氧化锡制备了掺杂纳米氧化锌。将PPy与纳米粒子复合,制备的复合材料不仅具有高导电性能,同时改善了延展性能,以FeCl3为氧化剂,在纳掺杂纳米氧化锌存在的情况下,以化学氧化聚合法得到导静电氧化锌。白度高,能在介质中得到良好地分散,降低粉体颗粒的内部电阻和接触电阻:颗粒内部电阻的降低可以通过控制掺杂离子的定位取代,产生掺锑的锡氢氧化物沉淀(Sn(OH)4-Sb(OH)3或Sn(OH)4-Sb2O3),这种沉淀物在叶腊石基体表面形成致密的包覆层,但该氢氧化物沉淀本身并不导电,只有通过在适当的条件下煅烧,使包覆层发生脱水反应,形成Sb掺杂的SnO2多晶包覆层,才能得到有导电性能的产品。因此,煅白度化学沉淀法可以很好地做到这一点
本发明相比现有技术具有如下优点:
本发明公开的导静电氧化锌颜色呈浅的青白色,所以加入颜料中可实现商品的色彩多样化。通过降低颜料、助剂的使用量,可起到降低总成本的作用。且与导电性氧化钛、ITO、ATO等具有导电性能的无机材料相比,具有价格低廉的优点。导电氧化锌粉体粒子为球形,具有易分散、黏度低、沉淀结块率低的优点。它的每个粒子都是一个独立的半导体,所以在分散时粉体结构不容易被破坏,电阻值较稳定。PPy包覆在掺杂纳米氧化锌的表面,形成致密的核-壳结构。形成立体导电通路,使绝缘介质产生电极化,甚至击穿导电。氧化锌晶须的导电机理还存在隧道效应,导静电氧化锌主要用于涂料、橡胶、纤维材料和陶瓷中作为导静电的白色颜料。
具体实施方式
实施例1
一种导静电氧化锌的制备方法,包括以下步骤:第一步、称取纳米氧化锌粉体,加入去离子水中形成固含量40%的悬浮分散液,移入反应釜中,控制一定反应温度、pH值,在不断搅拌下滴加15%的四氯化锡和三氯化锑的盐酸混合液,盐酸为质量浓度为7%的盐酸水溶液,控制pH值恒定为2.0,反应温度80℃,滴加时间4h,其中纳米氧化锌、四氯化锡和三氯化锑的质量比为22∶9∶1,同时滴加0.2mol/L的NaOH溶液,以保持溶液的pH值恒定,待混合液滴完后,再继续熟化温度90℃下加热30min,然后过滤,用去离子水洗涤至中性,过滤将滤饼60℃烘干至恒重,煅烧,得掺杂纳米氧化锌;第二步、吡咯减压蒸馏后,于4℃保存待用,量取7份吡咯于反应釜中,加入50份蒸馏水搅拌均匀乳液,向其中加入50份质量分数25%的对甲苯磺酸溶液混合均匀后,加入第一步得到的掺杂纳米氧化锌,浴比1∶8,45kHz下超声分散15min,再将混合溶液加入反应釜中,0℃条件下磁力搅拌10min,将质量分数16%的FeCl3水溶液逐滴加入上述反应釜中,滴加1.5h后,于0℃条件下持续5h后反应结束,真空抽滤后用甲醇洗涤3次,再用去离子水洗涤3次,于60℃干燥12h,即制得导静电氧化锌。
实施例2
一种导静电氧化锌的制备方法,包括以下步骤:第一步、称取纳米氧化锌粉体,加入去离子水中形成固含量30%的悬浮分散液,移入反应釜中,控制一定反应温度、pH值,在不断搅拌下滴加10%的四氯化锡和三氯化锑的盐酸混合液,盐酸为质量浓度为7%的盐酸水溶液,控制pH值恒定为1.0,反应温度70℃,滴加时间2h,其中纳米氧化锌、四氯化锡和三氯化锑的质量比为20∶7∶1,同时滴加0.1mol/L的NaOH溶液,以保持溶液的pH值恒定,待混合液滴完后,再继续熟化温度85℃下加热30min,然后过滤,用去离子水洗涤至中性,过滤将滤饼60℃烘干至恒重,煅烧,得掺杂纳米氧化锌;第二步、吡咯减压蒸馏后,于0℃保存待用,量取6.5份吡咯于反应釜中,加入50份蒸馏水搅拌均匀乳液,向其中加入50份质量分数24%的对甲苯磺酸溶液混合均匀后,加入第一步得到的掺杂纳米氧化锌,浴比1∶6超声分散10min,再将混合溶液加入反应釜中,0℃条件下磁力搅拌8min,将质量分数16%的FeCl3水溶液逐滴加入上述反应釜中,滴加1h后,于0℃条件下持续5h后反应结束,真空抽滤后用甲醇洗涤2次,再用去离子水洗涤2次,于60℃干燥12h,即制得导静电氧化锌。
将实施例1~2的导静电氧化锌进行性能测试,测试的结果见表1
表1实施例1~2的导静电氧化锌性能测试结果
实施例1 | 实施例2 | |
一次粒径,μm | 0.2 | 0.2 |
比表面积,m<sup>2</sup>/g | 35 | 37 |
吸油量,g/100g | 15 | 15 |
水悬浮液pH值 | 7.0 | 7.0 |
粉末电阻率,Ω·cm | 30 | 30 |
水份,wt%≤ | 1 | 1 |
325 目筛余物≤ | 1 | 1 |
L值≥ | 89 | 89 |
注:粒度测定按照GB/T19077-2016进行;振实密度测定按照GB/T21354-2008进行;比表面积测定按GB/T19587-2004进行;吸油量测定按GB/T5211.15-1988进行;水悬浮液pH值测定按照GB/T1717-1986进行;水份测定按照GB/T5211.3-1985进行;筛余物测定按照GB/T5211.14-1988进行;色相测定测定,试样应在105℃烘干2h,10份试样进行,取其平均值,柯尼卡美能达便携式色差计CR-10PLUSφ8mm测试Lab值;光谱中性系列反射标准白板,其反射比值为90%。测试步骤将标准白板置于测试台上,按标准白板标出的X、Y、Z值进行调白;将测试样品倒入压容器内,加压压紧后取出,朝玻璃平板面的样品面作为测试面;将制作好的样品置于试样台上,对准光孔,进行L、A、B测试,读取数值,测试结果保留两位有效数字;平行测定两次,取测试结果的平均值。GB/T1717-1986颜料水悬浮液pH值的测定;GB/T4472-2011化工产品密度相对密度的测定固体密度的测定;GB/T5211.15-1988颜料吸油量的测定;GB/T5211.3-1985颜料在105℃挥发物的测定;GB/T5211.14-1988颜料筛余物的测定机械冲洗法;GB/T19077-2016粒度分析激光衍射法;GB/T19587-2004气体吸附BET法测定固态物质比表面积;GB/T21354-2008粉末产品振实密度测定通用方法;GB/T30544.1-2014纳米技术术语第1部分核心术语;体积电阻率测定方法取5g导静电氧化锌样品放入模具中,在嵌样机上轴向加压成型,压力30MPa,压制成型的薄片直径为30.0mm,厚度为3.6mm,在压片表面涂刷液体电极,在373K烘干后测定其电阻值,最终通过换算得到粉体的体积电阻率值。
Claims (5)
1.一种导静电氧化锌的制备方法,其特征在于,包括以下步骤:第一步、称取纳米氧化锌粉体,加入去离子水中形成固含量30~40%的悬浮分散液,移入反应釜中,控制一定反应温度、pH值,在不断搅拌下滴加10~15%的四氯化锡和三氯化锑的盐酸混合液,同时滴加0.1~0.2mol/L的NaOH溶液,以保持溶液的pH值恒定,待混合液滴完后,再继续熟化30min,然后过滤,用去离子水洗涤至中性,过滤将滤饼60℃烘干至恒重,煅烧,得掺杂纳米氧化锌;第二步、吡咯减压蒸馏后,于0~4℃保存待用,量取6.5~7份吡咯于反应釜中,加入50份蒸馏水搅拌均匀乳液,向其中加入50份质量分数24~25%的对甲苯磺酸溶液混合均匀后,加入第一步得到的掺杂纳米氧化锌,浴比1∶6~8超声分散10~15min,再将混合溶液加入反应釜中,0℃条件下磁力搅拌8~10min,将质量分数16~17%的FeCl3水溶液逐滴加入上述反应釜中,滴加1~1.5h后,于0℃条件下持续5h后反应结束,真空抽滤后用甲醇洗涤2~3次,再用去离子水洗涤2~3次,于60℃干燥12h,即制得导静电氧化锌。
2.根据权利要求1所述的一种导静电氧化锌的制备方法,其特征在于,所述第一步控制pH值恒定为1.0~2.0,反应温度70~80℃,滴加时间2~4h,其中纳米氧化锌、四氯化锡和三氯化锑的质量比为20~22∶7~9∶1。
3.根据权利要求1所述的一种导静电氧化锌的制备方法,其特征在于,所述第一步煅烧工艺条件为煅烧温度580~600℃,煅烧时间1.5~2.0h。
4.根据权利要求1所述的一种导静电氧化锌的制备方法,其特征在于,所述第一步的盐酸为质量浓度为7~9%的盐酸水溶液。
5.根据权利要求1所述的一种导静电氧化锌的制备方法,其特征在于,所述第一步熟化为温度85~90℃下加热。
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