CN105585188B - 一种无硼超纯水的制备方法 - Google Patents
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
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- C—CHEMISTRY; METALLURGY
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/441—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by reverse osmosis
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/444—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by ultrafiltration or microfiltration
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/469—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
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Abstract
本发明公开了一种无硼超纯水的制备方法,将自来水依次经过超滤、反渗透、EDI装置、UV生物降解、除硼工艺和抛光树脂处理,得到所述无硼超纯水;其中,所述除硼工艺包括多元醇络合反渗透除硼和两级硼特效树脂除硼。本发明制得的超纯水,其硼元素含量小于100PPT,其他元素含量均可达到PPT级,是一种综合性能优异的超纯水,是制备半导体行业超纯化学材料的理想水源。本发明一种无硼超纯水的制备方法,工艺简便,容易实现,其通过多种处理方法联合并用,有效控制水中各物质的含量,并降低工艺成本,制备出高品质PPT级超纯水;通过分步除硼工艺,彻底去除超纯水中顽固的硼杂质,克服了行业难题,是超纯水发展的里程碑。
Description
技术领域
本发明涉及水净化技术领域,特别是涉及一种无硼超纯水的制备方法。
背景技术
在半导体行业中,在纯净的半导体产品中掺入极微量的杂质元素,就会使产品的电阻率发生极大的变化。例如,在纯硼中掺入百万分之—的硼元素,其电阻率就会从214000Ω·cm一下子减小到0.4Ω·cm,也就是硼的导电能为提高了50多万倍。由此可见,半导体行业对化学材料的纯净度要求极高。
超纯水是制备半导体行业所用超纯化学材料不可或缺的原料,其纯净度直接影响超纯化学材料的性能,从而也在一定程度上制约着光半导体行业,尤其是芯片行业的发展。
硼是超纯水中较难除去的杂质元素,其相对较高的含量直接影响超纯化学材料如超纯氨水在半导体产品中的应用。现有超纯水大都采用预处理、反渗透技术、超纯化处理以及后级处理四大步骤,多级过滤、高性能离子交换单元、超滤过滤器、紫外灯、除TOC装置等多种处理方法。但现有这些方法制备的超纯水,其硼含量仍然不能有效去除,或达不到ppt级的要求。
发明内容
本发明主要解决的技术问题是提供一种无硼超纯水的制备方法,能够有效去除水中的硼元素,解决现有超纯水制备工艺存在的上述不足之处。
为解决上述技术问题,本发明采用的一个技术方案是:提供一种无硼超纯水的制备方法,将自来水依次经过超滤、反渗透、EDI装置、UV生物降解、除硼工艺和抛光树脂处理,得到所述无硼超纯水;其中,所述除硼工艺包括多元醇络合反渗透除硼和两级硼特效树脂除硼。
在本发明一个较佳实施例中,所述多元醇络合反渗透除硼的方法为:自来水经UV生物降解处理后,调节其pH值至酸性,然后向其中加入一定量多元醇,搅拌均匀后经反渗透膜过滤除硼。
在本发明一个较佳实施例中,所述pH值为3~6.5;所述多元醇的加入量为1~10ppm/L水。
在本发明一个较佳实施例中,所述多元醇为D-山梨醇、甘露醇、D-果糖和木糖醇中的至少一种。
在本发明一个较佳实施例中,所述两级硼特效树脂除硼方法为:将经多元醇络合反渗透除硼后的自来水引入一级硼特效树脂除硼,然后调节自来水的pH值为8.5~9.5,再引入二级硼特效树脂除硼。
在本发明一个较佳实施例中,所述一级硼特效树脂为没食子酸接枝强酸性阴离子交换树脂;所述二级硼特效树脂为2,3-二羟基-6-磺酸钠接枝强碱性阴离子交换树脂或聚羟基胺苯乙烯树脂类树脂。
本发明的有益效果是:本发明一种无硼超纯水的制备方法,工艺简便,容易实现,其通过多种处理方法联合并用,有效控制水中各物质的含量,并降低工艺成本,制备出高品质PPT级超纯水;通过分步除硼工艺,彻底去除超纯水中顽固的硼杂质,克服了行业难题,是超纯水发展的里程碑。
具体实施方式
下面对本发明的较佳实施例进行详细阐述,以使本发明的优点和特征能更易于被本领域技术人员理解,从而对本发明的保护范围做出更为清楚明确的界定。
本发明实施例包括:
实施例1
一种无硼超纯水的制备方法,具体制备步骤如下:
(1)将经三级预处理去除杂质后的自来水以3~10MPa的压力通过超滤微孔小于0.01微米的中空纤维过滤器,滤除水中的细菌、铁锈、胶体等有害物质,保留水中原有的微量元素和矿物质;
(2)将超滤后的自来水引入反渗透装置,除去水中绝大部分可溶性盐分、微生物和全部的胶体;
(3)将反渗透处理的自来水引入EDI装置中,以电泳法去除自来水中的盐分,并彻底清除水体中的细菌;
(4)将经EDI装置电泳法处理后的自来水用波长为185nm的UV紫外光照射,从而将自来水中的有机物分解为二氧化碳和水;
(5)去除UV生物降解处理后的自来水中的硼元素,主要包括两步除硼工艺,第一步为多元醇络合反渗透除硼,具体方法为:向自来水中加入稀盐酸,调节其pH值为3~6.5,然后向每升自来水中加入1~10ppm的多元醇(包括D-山梨醇、甘露醇、D-果糖和木糖醇中的至少一种),搅拌均匀后,多元醇与自来水中的硼酸形成大分子的络合物,然后再将该含有大分子络合物的自来水以一定的压力引入反渗透装置,去除大分子络合物,从而实现去除硼元素的目的,该方法硼酸的去除率为80%;
第二步为两级硼特效树脂除硼,具体方法为:将经多元醇络合反渗透除硼后的自来水引入一级硼特效树脂,为没食子酸接枝强酸性阴离子交换树脂,恒温搅拌20~60min,使树脂充分吸附自来水中的硼酸,实现对自来水体除硼的目的,同时将吸附后的一级硼特效树脂进行解析,该过程可以除去自来水中95%以上的硼元素;然后加入稀氢氧化钠溶液调节自来水的pH值为8.5~9.5,再引入二级硼特效树脂,为2,3-二羟基-6-磺酸钠接枝强碱性阴离子交换树脂或聚羟基胺苯乙烯树脂类树脂,恒温搅拌20~60min,使树脂充分吸附自来水体中的硼酸,实现对自来水体除硼的目的,同时将吸附后的二级硼特效树脂进行解析,该过程可以除去自来水中全部的硼元素;
(6)将除硼后的自来水引入EC150UP抛光树脂,即超纯水专用混合离子交换树脂,以对自来水进行最后综合精处理,保证超纯水的水质,得到无硼超高纯水。
上述方法得到的超纯水,其硼元素含量小于100PPT,其他元素含量均可达到PPT级,是一种综合性能优异的超纯水,是制备半导体行业超纯化学材料的理想水源。
以上所述仅为本发明的实施例,并非因此限制本发明的专利范围,凡是利用本发明说明书内容所作的等效结构或等效流程变换,或直接或间接运用在其他相关的技术领域,均同理包括在本发明的专利保护范围内。
Claims (3)
1.一种无硼超纯水的制备方法,其特征在于,将自来水依次经过超滤、反渗透、EDI装置、UV生物降解、除硼工艺和抛光树脂处理,得到所述无硼超纯水;其中,所述除硼工艺包括多元醇络合反渗透除硼和两级硼特效树脂除硼;
所述多元醇络合反渗透除硼的方法为:自来水经UV生物降解处理后,调节其pH值至酸性,然后向其中加入一定量多元醇,搅拌均匀后经反渗透膜过滤除硼;
所述两级硼特效树脂除硼方法为:将经多元醇络合反渗透除硼后的自来水引入一级硼特效树脂除硼,然后调节自来水的pH值为8 .5~9 .5,再引入二级硼特效树脂除硼;
所述一级硼特效树脂为没食子酸接枝强酸性阴离子交换树脂;所述二级硼特效树脂为2 ,3-二羟基萘-6-磺酸钠接枝强碱性阴离子交换树脂。
2.根据权利要求1所述的无硼超纯水的制备方法,其特征在于,所述pH值为3~6 .5;所述多元醇的加入量为1~10ppm。
3.根据权利要求2所述的无硼超纯水的制备方法,其特征在于,所述多元醇为D-山梨醇、甘露醇、D-果糖和木糖醇中的至少一种。
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