CN110170296A - 一种去除氟化氢气体中水分子的吸附剂的制备方法 - Google Patents
一种去除氟化氢气体中水分子的吸附剂的制备方法 Download PDFInfo
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Abstract
本发明公开了一种去除氟化氢气体中水分子的吸附剂的制备方法,包括:(1)按重量份数,将0.1~2份碱金属氟化物或碱土金属氟化物、3.5~5.5份金属氟化物和0.05~0.5份碱金属氟氢化物加入超纯水中,经搅拌、干燥后,得到含氟复盐颗粒成型体;(2)将含氟复盐颗粒成型体在500~900℃烧结10~120min,得到烧结后的含氟复盐颗粒成型体;(3)将烧结后的含氟复盐颗粒成型体经球磨得到吸附剂产品。本发明具有工艺简单,成本低,绿色环保,产品性能好的优点。
Description
技术领域
本发明涉及分离气体中水分子的吸附剂,特别涉及一种去除氟化氢气体中水分子的吸附剂的制备方法。
背景技术
工业上生产氟化氢(HF)是通过加热萤石(氟化钙)和硫酸反应得到,主要杂质(包括水)通常是通过分级蒸馏而去除的,所得氟化氢的纯度可达99.8%以上,然而,这样制备的氟化氢气体中水分仍有5-1000ppm,无法应用于半导体制造干法刻蚀工艺中。在氟化氢的电子工业应用中,氟化氢中水分的存在对集成电路的成品率、电性能及可靠性都有着巨大的影响。因此,必须对氟化氢中水分进行进一步的去除,才能应用于电子工业中。
对于氟化氢气体中水分的进一步去除,现有的方法主要有氟气接触反应后蒸馏除水法、活性炭吸附法、碳分子筛吸附法、碳酰氟反应除水法、负载氟化镁的活性炭吸附法等。
如中国专利公开号CN101346303A公开了一种通过水与碳酰氟的化学反应,来达到除去水分的目的。不足之处是该工艺在降低水分的同时引入了CO2和其它杂质。
美国专利US5597545公开了一种通过碳分子筛吸附氟化氢中水分的方法,该方法包括:(1)将流体与碳分子筛接触,使得活性炭分子筛吸附水和HF;(2)加热所述碳分子筛,在高于接触的温度下解析水和HF直到被吸附的水被除去;(3)加热所述碳分子筛,在比步骤(2)高的温度下解析氟化氢;(4)分别回收解析出的水和HF。该专利通过碳分子筛先吸附水和HF,再通过不同温度下的解析,分别得到水和HF。不足之处是操作繁琐,除水效率低,成本高。
美国专利US6221132公开了一种用负载卤化镁的活性炭作为吸附剂吸附水的方法,该方法包括,将含水分的氟化氢气流送经包含5-35%氟化镁吸附剂,该吸附剂被负载于活性碳基材上以通过吸附的方式除水,该方法能将氟化氢气体水分降低至1ppm。不足之处是除水效率低,成本高。
发明内容
针对现有技术中存在的缺陷,本发明的目的在于提供一种工艺简单,成本低,绿色环保,产品性能好的去除氟化氢气体中水分子的吸附剂的制备方法。
为了实现上述目的,本发明采用的技术方案为:一种去除氟化氢气体中水分子的吸附剂的制备方法,包括如下步骤:
(1)按重量份数,将0.1~2份碱金属氟化物或碱土金属氟化物、3.5~5.5份金属氟化物和0.05~0.5份碱金属氟氢化物加入超纯水中,经搅拌、干燥后,得到含氟复盐颗粒成型体;
(2)将步骤(1)得到的含氟复盐颗粒成型体烧结,得到烧结后的含氟复盐颗粒成型体;
(3)将步骤(2)得到的烧结后的含氟复盐颗粒成型体经球磨得到吸附剂产品。
作为本发明的优选实施方式,步骤(1)中所述的碱金属氟化物优选为氟化钾或氟化钠。
作为本发明的优选实施方式,步骤(1)中所述的碱土金属氟化物优选为氟化钙或氟化锶。
作为本发明的优选实施方式,步骤(1)中所述的金属氟化物优选为氟化钛、氟化铁、氟化锆、氟化铝中的一种。
作为本发明的优选实施方式,步骤(1)中所述的碱金属氟氢化物优选为氟氢化钾或氟氢化钠。
作为本发明的优选实施方式,步骤(1)中所述的超纯水的用量优选为碱金属氟化物或碱土金属氟化物和金属氟化物总质量的20~30%。
作为本发明的优选实施方式,步骤(1)中所述的搅拌的转速优选为300~500rpm,搅拌的时间优选为5~20min。
作为本发明的优选实施方式,步骤(1)中所述的干燥的温度优选为70~80℃,干燥的时间优选为30~50min。
作为本发明的优选实施方式,步骤(2)中所述的烧结的温度优选为500~900℃,烧结的时间优选为10~120min。
作为本发明的优选实施方式,步骤(3)中所述的吸附剂产品的平均粒径优选为50-2000μm。
本发明中所述的超纯水的电导率≥18·MΩ·cm(25℃)。
本发明中适合的碱金属氟化物包括氟化锂、氟化钾、氟化钠、氟化铯等,优选为氟化钾或氟化钠;适合的碱土金属氟化物包括氟化钡、氟化钙、氟化镁、氟化锶等,优选为氟化钙或氟化锶。
本发明中可采用通式为MFy的金属氟化物,其中,y>0,M为Ti、Hf、Ta、Zr、Al、As、Co、Mn、Fe、Ni、V中的一种。所述金属氟化物优选为氟化钛、氟化铁、氟化锆、氟化铝中的一种。
本发明中,上述各种碱金属氟化物、碱土金属氟化物及金属氟化物作为主要成份制备得到的含氟复盐对氟化氢气体中水分的吸附能力强,选择性高,解吸方便,而且原料便宜易得。
本发明中,为了提高含氟复盐成型后的比表面积及机械强度,含氟复盐颗粒制备过程中可以添加碱金属氟氢化物,在含氟复盐烘干过程中碱金属氟氢化物会分解,放出氟化氢,从而增加含氟复盐的孔隙度,形成孔隙通道结构,从而提高含氟复盐比表面积,增大孔容,并能增高其机械强度。本发明中,碱金属氟氢化物优选为氟氢化钾或氟氢化钠。
本发明中,含氟复盐制备过程中物料粉碎可采用球磨机或其它粉碎设备,所制含氟复盐的形状一般为球型颗粒或圆柱体颗粒,经球磨后含氟复盐颗粒的平均粒径优选为50-500μm。
本发明制得的吸附剂,对水分有较强的选择吸附性,这种吸附不仅有物理吸附,而且还有吸附剂中含氟复盐对水分子化学吸附作用,吸附后,吸附剂中含氟复盐与水分子形成一种具有不同克分子比的化学复合物即含水氟盐(AxMFy·nH2O,其中A为碱金属或碱土金属元素中的一种,M为Ti、Hf、Ta、Zr、Al、As、Co、Mn、Fe、Ni、V中的一种;x>0;y>0),含水氟盐在一定温度下会分解放出H2O。表示式如下所示:
AxMFy·nH2O→AxMFy+nH2O
通过以上反应原理,采用吸附、解吸循环来达到回收吸附剂的目的。
本发明得到的吸附剂用于去除氟化氢气体中水分子时,将制备好的吸附剂填充于吸附塔内,氟化氢气体通过负载有吸附剂的吸附塔,氟化氢气体中水分子通过吸附剂的选择性吸附而去除,从而水分子被截留。
与现有技术相比,本发明的优点在于:
1、产品除水效率高,本发明得到的吸附剂产品中含氟复盐颗粒化学结构稳定,不会引入新的杂质,对氟化氢气体中水分子的吸附率和选择性高,处理后氟化氢气体中水分含量在0.5ppm以下,所得的高纯度氟化氢能够应用于显示面板和超大规模集成电路等行业。
2、产品除水成本低,本发明得到的吸附剂产品对水分有较强的选择吸附性截留,这种吸附不仅有物理吸附,而且还有含氟复盐对水分子的化学吸附作用,吸附后,吸附剂中含氟复盐与水分子形成一种具有不同克分子比的化学复合物即含水氟盐,含水氟盐在一定温度下会分解放出H2O,可通过采用吸附、解吸循环来达到回收吸附剂的目的,显著降低了除水成本。
3、产品比表面积大,机械强度高,本发明得到的吸附剂产品中含有的碱金属氟氢化物在烘干过程中会分解,放出氟化氢,增加吸附剂产品的孔隙度,形成孔隙通道结构,从而显著提高吸附剂产品比表面积,增大孔容,并能增大其机械强度,本发明得到的吸附剂产品比表面积在810m2/kg以上。
4、工艺简单,成本低,绿色环保,本发明生产原料易得,反应条件温和,显著降低了生产成本。
具体实施方式
以下通过实施例对本发明的技术方案进行进一步详细描述,但本发明并不仅限于以下实施例。
实施例1:(1)称取0.2公斤氟化钾粉粒和5.0公斤氟化钛粉粒,加入1200克超纯水和250克氟氢化钠,在300rpm搅拌转速下混合20min后,于70℃下干燥50min,得到含氟复盐颗粒成型体;
(2)将步骤(1)得到的含氟复盐颗粒成型体在550℃中保温60min进行烧结,得到烧结后的含氟复盐颗粒成型体;
(3)将步骤(2)得到的烧结后的含氟复盐颗粒成型体经球磨得到平均粒径为1200μm的吸附剂产品。
实施例2:(1)称取0.5公斤氟化钾粉粒和5.5公斤氟化钛粉粒,加入1300克超纯水和150克氟氢化钠,在350rpm搅拌转速下混合15min后,于72℃下干燥45min,得到含氟复盐颗粒成型体;
(2)将步骤(1)得到的含氟复盐颗粒成型体在650℃中保温100min进行烧结,得到烧结后的含氟复盐颗粒成型体;
(3)将步骤(2)得到的烧结后的含氟复盐颗粒成型体经球磨得到平均粒径为600μm的吸附剂产品。
实施例3:(1)称取0.8公斤氟化钠粉粒和4.5公斤氟化铁粉粒,加入1400克超纯水和500克氟氢化钾,在400rpm搅拌转速下混合10min后,于75℃下干燥40min,得到含氟复盐颗粒成型体;
(2)将步骤(1)得到的含氟复盐颗粒成型体在750℃中保温20min进行烧结,得到烧结后的含氟复盐颗粒成型体;
(3)将步骤(2)得到的烧结后的含氟复盐颗粒成型体经球磨得到平均粒径为300μm的吸附剂产品。
实施例4:(1)称取1.5公斤氟化钙粉粒和3.5公斤氟化锆粉粒,加入1500克超纯水和300克氟氢化钾,在450rpm搅拌转速下混合10min后,于78℃下干燥35min,得到含氟复盐颗粒成型体;
(2)将步骤(1)得到的含氟复盐颗粒成型体在900℃中保温10min进行烧结,得到烧结后的含氟复盐颗粒成型体;
(3)将步骤(2)得到的烧结后的含氟复盐颗粒成型体经球磨得到平均粒径为1500μm的吸附剂产品。
实施例5:(1)称取2.0公斤氟化锶粉粒和5.0公斤氟化铝粉粒,加入1800克超纯水和50克氟氢化钾,在500rpm搅拌转速下混合5min后,于80℃下干燥30min,得到含氟复盐颗粒成型体;
(2)将步骤(1)得到的含氟复盐颗粒成型体在800℃中保温20min进行烧结,得到烧结后的含氟复盐颗粒成型体;
(3)将步骤(2)得到的烧结后的含氟复盐颗粒成型体经球磨得到平均粒径为100μm的吸附剂产品。
性能测试:
将制备好的吸附剂填充于吸附塔内,氟化氢气体通过负载有吸附剂的吸附塔,氟化氢气体中水分子通过吸附剂的选择性吸附而去除,收集处理后的氟化氢气体,取样分析,结果见表1。其中:
氟化氢气体中水分含量测试采用芬兰GASERA干涉公司的痕量级光声多气体仪(型号:F10S)
比表面积测定:按GB/T 19587-2004《气体吸附BET法测定固态物质比表面积》执行。
表1实施例1~5制备得到吸附剂的性能
由表1所列数据可知,实施例1-5制得的吸附剂都能有效脱除氟化氢气体中的水分,其在24h后测量氟化氢样品的水分浓度低于0.5ppm。
Claims (10)
1.一种去除氟化氢气体中水分子的吸附剂的制备方法,其特征在于,包括如下步骤:
(1)按重量份数,将0.1~2份碱金属氟化物或碱土金属氟化物、3.5~5.5份金属氟化物和0.05~0.5份碱金属氟氢化物加入超纯水中,经搅拌、干燥后,得到含氟复盐颗粒成型体;
(2)将步骤(1)得到的含氟复盐颗粒成型体烧结,得到烧结后的含氟复盐颗粒成型体;
(3)将步骤(2)得到的烧结后的含氟复盐颗粒成型体经球磨得到吸附剂产品。
2.根据权利要求1所述的去除氟化氢气体中水分子的吸附剂的制备方法,其特征在于,步骤(1)中所述的碱金属氟化物为氟化钾或氟化钠。
3.根据权利要求1所述的去除氟化氢气体中水分子的吸附剂的制备方法,其特征在于,步骤(1)中所述的碱土金属氟化物为氟化钙或氟化锶。
4.根据权利要求1所述的去除氟化氢气体中水分子的吸附剂的制备方法,其特征在于,步骤(1)中所述的金属氟化物为氟化钛、氟化铁、氟化锆、氟化铝中的一种。
5.根据权利要求1所述的去除氟化氢气体中水分子的吸附剂的制备方法,其特征在于,步骤(1)中所述的碱金属氟氢化物为氟氢化钾或氟氢化钠。
6.根据权利要求1所述的去除氟化氢气体中水分子的吸附剂的制备方法,其特征在于,步骤(1)中所述的超纯水的用量为碱金属氟化物或碱土金属氟化物和金属氟化物总质量的20~30%。
7.根据权利要求1所述的去除氟化氢气体中水分子的吸附剂的制备方法,其特征在于,步骤(1)中所述的搅拌的转速为300~500rpm,搅拌的时间为5~20min。
8.根据权利要求1所述的去除氟化氢气体中水分子的吸附剂的制备方法,其特征在于,步骤(1)中所述的干燥的温度为70~80℃,干燥的时间为30~50min。
9.根据权利要求1所述的去除氟化氢气体中水分子的吸附剂的制备方法,其特征在于,步骤(2)中所述的烧结的温度为500~900℃,烧结的时间为10~120min。
10.根据权利要求1所述的去除氟化氢气体中水分子的吸附剂的制备方法,其特征在于,步骤(3)中所述的吸附剂产品的平均粒径为50-2000μm。
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2021208949A1 (zh) * | 2020-04-15 | 2021-10-21 | 浙江博瑞电子科技有限公司 | 一种hf电子气体深度纯化材料的制备及应用方法 |
CN114522660A (zh) * | 2022-02-11 | 2022-05-24 | 福建德尔科技有限公司 | 新型改性氟化钠专用吸附剂、制备及应用 |
CN115487522A (zh) * | 2022-09-06 | 2022-12-20 | 内蒙古东岳金峰氟化工有限公司 | 氟化氢提纯***及工艺 |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3976447A (en) * | 1973-04-26 | 1976-08-24 | Pennwalt Corporation | Removal of hydrogen fluoride from gaseous mixture by absorption on alkaline earth metal fluoride |
CN1836771A (zh) * | 2005-03-25 | 2006-09-27 | 金正义 | 氟化氢吸附剂及其制法和应用 |
-
2019
- 2019-04-23 CN CN201910328241.1A patent/CN110170296A/zh active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3976447A (en) * | 1973-04-26 | 1976-08-24 | Pennwalt Corporation | Removal of hydrogen fluoride from gaseous mixture by absorption on alkaline earth metal fluoride |
CN1836771A (zh) * | 2005-03-25 | 2006-09-27 | 金正义 | 氟化氢吸附剂及其制法和应用 |
Non-Patent Citations (2)
Title |
---|
上海钾盐工程技术研究中心: "《中国钾盐工业概览》", 31 July 2009 * |
符德学: "《实用无机化工工艺学》", 30 September 1999 * |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2021208949A1 (zh) * | 2020-04-15 | 2021-10-21 | 浙江博瑞电子科技有限公司 | 一种hf电子气体深度纯化材料的制备及应用方法 |
CN114522660A (zh) * | 2022-02-11 | 2022-05-24 | 福建德尔科技有限公司 | 新型改性氟化钠专用吸附剂、制备及应用 |
CN115487522A (zh) * | 2022-09-06 | 2022-12-20 | 内蒙古东岳金峰氟化工有限公司 | 氟化氢提纯***及工艺 |
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