CN116262659B - 用于地下水处理的陶粒及其制备方法、应用 - Google Patents
用于地下水处理的陶粒及其制备方法、应用 Download PDFInfo
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- CN116262659B CN116262659B CN202310511746.8A CN202310511746A CN116262659B CN 116262659 B CN116262659 B CN 116262659B CN 202310511746 A CN202310511746 A CN 202310511746A CN 116262659 B CN116262659 B CN 116262659B
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- ceramsite
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- white mud
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- 238000011282 treatment Methods 0.000 title claims abstract description 55
- 239000003673 groundwater Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000919 ceramic Substances 0.000 claims abstract description 54
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 36
- 238000005498 polishing Methods 0.000 claims abstract description 35
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000010802 sludge Substances 0.000 claims abstract description 33
- 239000000203 mixture Substances 0.000 claims abstract description 28
- 239000011159 matrix material Substances 0.000 claims abstract description 26
- 238000010304 firing Methods 0.000 claims abstract description 25
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 20
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 20
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 19
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 19
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000000465 moulding Methods 0.000 claims abstract description 7
- 239000002893 slag Substances 0.000 claims description 26
- 239000000243 solution Substances 0.000 claims description 21
- 230000001590 oxidative effect Effects 0.000 claims description 18
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- 239000007864 aqueous solution Substances 0.000 claims description 8
- 239000003651 drinking water Substances 0.000 claims description 6
- 235000020188 drinking water Nutrition 0.000 claims description 6
- 239000008187 granular material Substances 0.000 claims description 6
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 28
- MMDJDBSEMBIJBB-UHFFFAOYSA-N [O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[NH6+3] Chemical compound [O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[NH6+3] MMDJDBSEMBIJBB-UHFFFAOYSA-N 0.000 abstract description 15
- 229910019142 PO4 Inorganic materials 0.000 abstract description 14
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 abstract description 12
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 abstract description 12
- 239000010452 phosphate Substances 0.000 abstract description 12
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 abstract description 10
- 230000000052 comparative effect Effects 0.000 description 15
- 238000001179 sorption measurement Methods 0.000 description 14
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 11
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 230000000694 effects Effects 0.000 description 7
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- 239000002910 solid waste Substances 0.000 description 4
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 3
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- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 2
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- OERNJTNJEZOPIA-UHFFFAOYSA-N zirconium nitrate Chemical compound [Zr+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O OERNJTNJEZOPIA-UHFFFAOYSA-N 0.000 description 2
- DUFCMRCMPHIFTR-UHFFFAOYSA-N 5-(dimethylsulfamoyl)-2-methylfuran-3-carboxylic acid Chemical compound CN(C)S(=O)(=O)C1=CC(C(O)=O)=C(C)O1 DUFCMRCMPHIFTR-UHFFFAOYSA-N 0.000 description 1
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- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
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- 239000000956 alloy Substances 0.000 description 1
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- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- -1 aluminum sludge Chemical class 0.000 description 1
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- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 239000000701 coagulant Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
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- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000010433 feldspar Substances 0.000 description 1
- 229960005191 ferric oxide Drugs 0.000 description 1
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- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910052622 kaolinite Inorganic materials 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
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- 230000000813 microbial effect Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- UJVRJBAUJYZFIX-UHFFFAOYSA-N nitric acid;oxozirconium Chemical compound [Zr]=O.O[N+]([O-])=O.O[N+]([O-])=O UJVRJBAUJYZFIX-UHFFFAOYSA-N 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
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- 239000007787 solid Substances 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
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- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 description 1
- IPCAPQRVQMIMAN-UHFFFAOYSA-L zirconyl chloride Chemical compound Cl[Zr](Cl)=O IPCAPQRVQMIMAN-UHFFFAOYSA-L 0.000 description 1
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Abstract
本发明公开了一种用于地下水处理的陶粒及其制备方法、应用,涉及水处理领域。其中,陶粒的制备方法包括以下步骤:(1)将铝污泥20~40份,高岭土10~20份,造纸白泥30~50份,陶瓷抛光渣5~15份混合均匀,得到混合物;(2)将混合物成型,得到球形坯体;(3)将球形坯体在950~1050℃烧成,得到陶粒基体;(4)将陶粒基体浸入含锆溶液中,并将含锆溶液中的溶质干燥去除,即得到用于地下水处理的陶粒成品。本发明的陶粒能在较低温度下实现对硝态氮、氨氮、磷酸盐、氟化物的同时处理,降低了处理成本。
Description
技术领域
本发明涉及水处理领域,尤其涉及一种用于地下水处理的陶粒及其制备方法、应用。
背景技术
地下水资源是我国居民生活用水的重要保障。进入新世纪以来,我国的工农业生产***日趋成熟,工业不规范生产、燃料资源的消耗、农业化肥施用以及固废污染等一系列问题,加重了我国地下水的污染。尤其是在一些重工业区、规模化作业农业区,其地下水中的TDS(总溶解固体含量)、磷酸盐、硝酸盐氮、亚硝酸盐氮、氨氮、氟化物均含量较高,需要经过处理。其中,现有技术中多关注氟化物、氨氮等的处理,对硝态氮(硝酸盐氮、亚硝酸盐氮)的研究相对较少。而硝态氮有致癌风险,为此,在我国新出台的《生活饮用水卫生标准》(GB5749-2022)将饮用水中的硝酸盐限量设定为10mg/L(以N计),是2017年相关标准的一半。这对现有的地下处理水生产者提出了极大的挑战。
对于硝态氮,现有的大规模应用的处理方式主要有两类:一类是采用微生物反硝化,但反硝化细菌往往需要一定的温度条件,在一些四季温差较大的区域难以适用;并且反硝化一般需要厌氧控制,成本高;此外,反硝化往往会造成二次污染,如会产生甲醇,又如需要投放一些有机物。另一类是反渗透法,但其设备要求高,成本高,对于一些现有的水厂而言往往难以采用。
另一方面,传统的水厂在水处理的过程中会添加一些铝盐或聚合铝盐等混凝剂提高处理效果,该过程会产生大量含有铝盐的铝污泥沉淀物,即为铝污泥。铝污泥不再能直接排放,且土地填埋的成本较高,因此对其进行资源化利用已经备受关注。
发明内容
本发明所要解决的技术问题在于,提供一种用于水处理的陶粒及其制备方法,该陶粒可同时实现对磷酸盐、氟化物、硝态氮的处理,且处理条件温和,维护成本低。同时实现了传统水厂固废的资源化利用,进一步降低了成本。
本发明还要解决的技术问题在于,提供上述的用于地下水处理的陶粒在地下水处理以制备饮用水中的应用。
为了解决上述技术问题,本发明提供了一种用于地下水处理的陶粒的制备方法,其包括以下步骤:
(1)将铝污泥 20~40份,高岭土 10~20份,造纸白泥 30~50份,陶瓷抛光渣 5~15份混合均匀,得到混合物;其中,铝污泥、高岭土、造纸白泥、陶瓷抛光渣的总用量为100份;
(2)将所述混合物成型,得到球形坯体;
(3)将所述球形坯体在950~1050℃烧成,得到陶粒基体;
(4)将陶粒基体浸入含锆溶液中,并将含锆溶液中的溶质干燥去除,即得到用于地下水处理的陶粒成品。
作为上述技术方案的改进,所述含锆溶液为ZrOCl2水溶液,其浓度为15~30wt%。
作为上述技术方案的改进,所述铝污泥中Fe2O3的含量≥10wt%,CaO的含量≤12wt%,Al2O3的含量≥35wt%。
作为上述技术方案的改进,所述造纸白泥在600℃、氧化性气氛灼烧至恒重后,质量损失率≥30wt%;
所述造纸白泥在950℃、氧化性气氛灼烧至恒重后,其质量损失率≥70wt%。
作为上述技术方案的改进,所述陶瓷抛光渣中CaO的含量≤1.5wt%,SiO2的含量≥63wt%,Al2O3的含量≥20wt%。
作为上述技术方案的改进,所述铝污泥中Fe2O3的含量为12~20wt%,CaO的含量为3~8wt%,Al2O3的含量为38~48wt%;
所述造纸白泥在600℃、氧化性气氛灼烧至恒重后,质量损失率为35~45wt%;在950℃、氧化性气氛灼烧至恒重后,质量损失率为75~85wt%;
所述陶瓷抛光渣CaO的含量为0.3~1.2wt%,SiO2的含量为64~70wt%,Al2O3的含量20.5~23wt%。
作为上述技术方案的改进,步骤(3)中,烧成曲线为:
从室温到350℃,升温速率为15~20℃/min;
在350℃保温5~10min;
从350℃到850℃,升温速率为8~12℃/min;
从850℃到烧成温度,升温速率为5~20℃/min;
在烧成温度保温10~15min。
作为上述技术方案的改进,所述陶粒基体的显气孔率≥55%,筒压强度≥5MPa,堆积密度≥0.9g/cm3。
相应的,本发明还公开了一种用于地下水处理的陶粒,其由上述的用于地下水处理的陶粒的制备方法制备而得。
相应的,本发明还公开了上述的用于地下水处理的陶粒在地下水处理形成饮用水中的应用,处理温度为12~35℃。
实施本发明,具有如下有益效果:
1. 本发明的用于地下水处理的陶粒,采用铝污泥、高岭土、造纸白泥、陶瓷抛光渣制备陶粒基体,然后负载锆,这种陶粒能在较低温度下同时实现对氨氮、硝态氮、磷酸盐、氟化物的同时处理,降低了处理成本。且该陶粒基体多采用铝污泥、造纸白泥、陶瓷抛光渣等固废制成,原料成本低。
2. 本发明的用于地下水处理的陶粒,其陶粒基体以特定化学成分的铝污泥、高岭土、造纸白泥、陶瓷抛光渣制成,并联合特定的烧成曲线,可有效地控制其显气孔率,孔径均匀度,实现对锆的良好负载,提升水处理效果。同时,也更多地保留了原料中活性Al、Fe,进而增强了对磷酸盐、氟化物的处理效果。
附图说明
图1是本发明实施例3中用于地下水处理的陶粒的N2吸附脱附等温曲线图;
图2是本发明实施例3中用于地下水处理的陶粒的BJH孔径分布曲线图。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚,下面对本发明作进一步地详细描述。
本发明提供了一种用于地下水处理的陶粒的制备方法,其包括以下步骤:
S1:将铝污泥 20~40份,高岭土 10~20份,造纸白泥 30~50份,陶瓷抛光渣 5~15份混合均匀,得到混合物;
其中,铝污泥是水厂固废,其含有不定形的铁、铝氢氧化物,也存在一些含有SiO2的高岭石、长石等矿物质。引入铝污泥,不仅提供了陶粒所必需的Al源,也提供了Fe源,Fe在高温释放的气体会优化陶粒的孔道结构,提升显气孔率。优选的,在本发明的一个实施例中,控制铝污泥中Fe2O3的含量≥10wt%,CaO的含量≤12wt%,Al2O3的含量≥35wt%。基于上述控制,不仅可提升陶粒基体的显气孔率,同时还可保留较多的活性Al,提升后续对磷酸盐、氟化物、氨氮的吸附作用。此外,还能保证陶粒基体不过早地烧结,进而使得显气孔率大幅下降。进一步优选的,控制铝污泥中Fe2O3的含量为12~20wt%,示例性的为13wt%、15wt%、17wt%、18.5wt%或19wt%,但不限于此。控制铝污泥中CaO的含量为3~8wt%,示例性的为3.5wt%、4.5wt%、5.5wt%、6.5wt%或7wt%,但不限于此。控制铝污泥中Al2O3的含量为38~48wt%,示例性的为39wt%、41wt%、43wt%、45wt%或47wt%,但不限于此。
铝污泥的用量为20~40重量份,示例性的为22份、26份、30份、34份、38份或39份,但不限于此。
其中,高岭土可提供塑性,便于成型。优选的,在本发明的一个实施例之中,控制高岭土中Al2O3的含量≥37wt%,该成分的高岭土塑性更佳,同时在烧成过程中会形成部分的柱状莫来石,提升陶粒基体的力学性能(如筒压强度等)。
高岭土的用量为10~20重量份,示例性的为11份、13份、15份、17或19份,但不限于此。
其中,造纸白泥是造纸厂所得废渣,其含有大量的纸纤维,也含有一定的碳酸钙。通过引入造纸白泥,一者其可提升成型坯体的性能,减少高岭土的使用,降低原料成本。二者,其大量的纸纤维可分解形成大量的孔道,提升陶粒的吸附性能。进一步的,通过对烧成曲线的控制,还可使得纸纤维在较高温度下(900℃左右)仍有分解释放,进而分解所得气体会包裹在配方中其他微粒的表面,调节其他微粒(如陶瓷抛光渣中的SiC、Fe2O3等)释放气体的速度,从而保证陶粒孔隙的均匀性,提升吸附效果。三者,造纸白泥中含有的较多的钙会降低烧成温度,减少活性Al的转变,提升吸附效果。碳酸钙也会高温分解,进一步提升陶粒的显气孔率,提升陶粒基体的吸附性能。优选的,在本发明的一个实施例之中,造纸白泥在600℃、氧化性气氛灼烧至恒重后,质量损失率≥30wt%;造纸白泥在950℃、氧化性气氛灼烧至恒重后,其质量损失率≥70wt%。基于该控制,可进一步提升对磷酸盐、氟化物的处理效果。进一步优选的,造纸白泥在600℃、氧化性气氛灼烧至恒重后,质量损失率为35~45wt%,示例性的为37wt%、39wt%、41wt%或43wt%,但不限于此。造纸白泥在950℃、氧化性气氛灼烧至恒重后,质量损失率为75~85wt%,示例性的为77wt%、79wt%、81wt%或83wt%,但不限于此。
造纸白泥的用量为30~50重量份,示例性的为33份、35份、37份、39份、41份、43份、45份或47份,但不限于此。
其中,陶瓷抛光渣是陶瓷抛光砖抛光所得废料。一者,陶瓷抛光渣中含有磨头物质SiC,其可在高温下发泡,提升陶粒基体的开口气孔率。同时,由于本发明在配方之中引入了高Ca含量的造纸白泥,其在高温下可降低粘度,其可腐蚀SiC在反应过程中形成的SiO2膜,进而在较低的温度下(约1000℃)分解发泡。而传统的SiC与O2的反应温度约在1200℃左右。二者,陶瓷抛光渣中含有大量高温(1150~1250℃)烧成后的活性物质,也可提升对于磷酸盐、氨氮的吸附能力。优选的,在本发明的一个实施例之中,陶瓷抛光渣CaO的含量≤1.5wt%,SiO2的含量≥63wt%,Al2O3的含量≥20wt%。进一步优选的陶瓷抛光渣CaO的含量为0.3~1.2wt%,示例性的为0.5wt%、0.7wt%、0.9wt%或1.1wt%,但不限于此。陶瓷抛光渣中SiO2的含量为64~70wt%,示例性的为65wt%、67wt%、68wt%或69wt%,但不限于此。陶瓷抛光渣中Al2O3的含量20.5~23wt%,示例性的为21wt%、21.5wt%、22wt%或22.5wt%,但不限于此。
陶瓷抛光渣的用量为5~15重量份,示例性的为6份、8份、10份、12份或14份,但不限于此。
其中,在混合过程中还可加入少量水,以使混合物具有一定的流动性,方便后续成型。混合可采用本领域常用的混料机进行,也可采用球磨机进行,但不限于此。
S2:将混合物成型,得到球形坯体;
具体的,可通过圆盘成球机将混合料成型,但不限于此。成型得到球形坯体在80~100℃下干燥。
S3:将球形坯体在950~1050℃烧成,得到陶粒基体;
具体的,可采用本领域常规的烧成曲线进行烧成,但不限于此。优选的,在本发明的一个实施例之中,烧成曲线为:从室温到350℃,升温速率为15~20℃/min;在350℃保温5~10min;从350℃到850℃,升温速率为8~12℃/min;从850℃到烧成温度(950~1050℃),升温速率为5~20℃/min;在烧成温度保温10~15min。基于该烧成曲线,可有效提升陶粒基体中活性Al、Fe的含量,提升处理磷酸盐、氟化物、氨氮的效率。同时,活性Al、Fe也可提升锆的负载量,提升了硝态氮的处理能力。
具体的,基于上述的配方及制备方法得到的陶粒基体,其显气孔率≥55%,筒压强度≥5MPa,堆积密度≥0.9g/cm3。
S4:将陶粒基体浸入含锆溶液中,并将含锆溶液中的溶质干燥去除,即得到用于地下水处理的陶粒成品。
其中,含锆溶液可为氯化锆水溶液、乙酸锆水溶液、硝酸锆水溶液、硝酸氧锆水溶液或氯化氧锆水溶液,但不限于此。优选的,在本发明的一个实施例之中,含锆溶液为ZrOCl2水溶液,其浓度为15~30wt%。
进一步的,在浸泡含锆溶液之前,可将陶粒采用稀盐酸(5~12wt%)浸泡10~30h,然后漂洗至pH恒定。在浸泡含锆溶液后采用NaOH溶液(5~15wt%)浸泡1~5h,然后漂洗至pH恒定。基于该工艺,可在陶粒基体表面负载Zr,有效提升对氟化物、硝态氮的吸附量。
相应的,本发明还公开了一种用于地下水处理的陶粒,其由上述的用于地下水处理的陶粒的制备方法制备而得。
相应的,本发明还公开了上述的陶粒在地下水处理以制备饮用水的应用。具体的,处理温度可为12~35℃。基于该处理温度,本发明陶粒对氟的去除率≥95%,对氨氮的去除率≥98%,对磷酸盐的去除率≥90%,对硝态氮的去除率≥35%。并且,本发明的陶粒处理温度低,可适用于四季温差较大的区域,如东北老工业区。
下面以具体实施例对本发明进行说明:
实施例1
本实施例提供一种用于地下水处理的陶粒的制备方法,包括以下步骤:
(1)将铝污泥 24份,高岭土 15份,造纸白泥 49份,陶瓷抛光渣 12份混合均匀,得到混合物;
其中,铝污泥中Fe2O3的含量为13.5wt%,CaO的含量为4.3wt%,Al2O3的含量为42.5wt%。高岭土的Al2O3含量为38.3wt%;造纸白泥在600℃、氧化性气氛灼烧至恒重后,质量损失率为25.4wt%。造纸白泥在950℃、氧化性气氛灼烧至恒重后,质量损失率为76.3wt%。陶瓷抛光渣CaO的含量为1.4wt%,SiO2的含量为66.8wt%,Al2O3的含量21.8wt%。
(2)将混合物采用圆盘成球机成型,得到球形坯体,并在85℃下烘干;
(3)将球形坯体烧成,得到陶粒基体;
其中,烧成曲线为:从室温到300℃,升温速率为30℃/min,在300℃保温20min;从300℃到1020℃,升温速率为20℃/min;在1020℃保温15min。
(4)将陶粒基体采用稀盐酸(10wt%)浸泡24h,然后用水漂洗至pH恒定。然后浸入ZrOCl2水溶液(20wt%)中,水浴(80℃)蒸干,采用NaOH溶液(8wt%)浸泡3h,然后用水漂洗至pH恒定,即得。
实施例2
本实施例提供一种用于地下水处理的陶粒的制备方法,包括以下步骤:
(1)将铝污泥 24份,高岭土 15份,造纸白泥 49份,陶瓷抛光渣 12份混合均匀,得到混合物;
其中,铝污泥中Fe2O3的含量为13.5wt%,CaO的含量为4.3wt%,Al2O3的含量为42.5wt%。高岭土的Al2O3含量为38.3wt%;造纸白泥在600℃、氧化性气氛灼烧至恒重后,质量损失率为37.4wt%。造纸白泥在950℃、氧化性气氛灼烧至恒重后,质量损失率为80.5wt%。陶瓷抛光渣CaO的含量为1.4wt%,SiO2的含量为66.8wt%,Al2O3的含量21.8wt%。
(2)将混合物采用圆盘成球机成型,得到球形坯体,并在85℃下烘干;
(3)将球形坯体烧成,得到陶粒基体;
其中,烧成曲线为:从室温到300℃,升温速率为30℃/min,在300℃保温20min;从300℃到1020℃,升温速率为20℃/min;在1020℃保温15min。
(4)将陶粒基体采用稀盐酸(10wt%)浸泡24h,然后用水漂洗至pH恒定。然后浸入ZrOCl2水溶液(20wt%)中,水浴(80℃)蒸干,采用NaOH溶液(8wt%)浸泡3h,然后用水漂洗至pH恒定,即得。
实施例3
本实施例提供一种用于地下水处理的陶粒的制备方法,包括以下步骤:
(1)将铝污泥 24份,高岭土 15份,造纸白泥 49份,陶瓷抛光渣 12份混合均匀,得到混合物;
其中,铝污泥中Fe2O3的含量为13.5wt%,CaO的含量为4.3wt%,Al2O3的含量为42.5wt%。高岭土的Al2O3含量为38.3wt%;造纸白泥在600℃、氧化性气氛灼烧至恒重后,质量损失率为37.4wt%。造纸白泥在950℃、氧化性气氛灼烧至恒重后,质量损失率为80.5wt%。陶瓷抛光渣CaO的含量为1.4wt%,SiO2的含量为66.8wt%,Al2O3的含量21.8wt%。
(2)将混合物采用圆盘成球机成型,得到球形坯体,并在85℃下烘干;
(3)将球形坯体烧成,得到陶粒基体;
其中,烧成曲线为:从室温到350℃,升温速率为16.5℃/min;在350℃保温8min;从350℃到850℃,升温速率为11℃/min;从850℃到1020℃,升温速率为15℃/min;在1020℃保温12min。
对比例1
本对比例提供一种陶粒的制备方法,其与实施例1的区别在于,陶粒基体的配方中不包括铝污泥,其他均与实施例1相同。
对比例2
本对比例提供一种陶粒的制备方法,其与实施例1的区别在于,陶粒基体配方中不包括造纸白泥,其他均与实施例1相同。
对比例3
本对比例提供一种陶粒的制备方法,其与实施例1的区别在于,陶粒基体配方中不包括陶瓷抛光渣,其他均与实施例1相同。
对比例4
本对比例提供一种陶粒的制备方法,其与实施例1的区别在于,陶粒基体配方中不包括铝污泥和造纸白泥,其他均与实施例1相同。
对比例5
本对比例提供一种陶粒的制备方法,其与实施例1的区别在于,陶粒基体配方中不包括铝污泥和陶瓷抛光渣,其他均与实施例1相同。
对比例6
本对比例提供一种陶粒的制备方法,其与实施例1的区别在于,陶粒基体配方中不包括造纸白泥和陶瓷抛光渣,其他均与实施例1相同。
对比例7
本对比例提供一种陶粒的制备方法,其与实施例1的区别在于,不包含步骤(3),即陶粒基体不浸入含锆溶液处理,其余均与实施例1相同。
取各实施例、对比例制得的陶粒,进行实验,具体实验方法如下:
配置氟浓度为10mg/L、磷酸盐浓度为20mg/L,硝态氮浓度为30mg/L,氨氮浓度为5mg/L的原水,置于锥形瓶中,将陶粒按照15g/L的投入量加入锥形瓶中,置于温度为20℃的恒温振荡器中,在140rpm下震荡1h,测定水中氟浓度、磷酸盐浓度、硝态氮浓度、氨氮浓度。具体的测定方法参《水和废水监测分析方法》(第四版),并计算去除率。
实验结果如下表所示:
从表中可以看出,本发明中的陶粒可在低温环境下(20℃)下实现氟化物去除率96.5%以上,氨氮去除率98.3%以上,磷酸盐90.5%以上,硝态氮去除率36.6%以上,实现了对地下水的有效处理,处理后水质完全可以满足相关国家标准的要求。
另将实施例3所得的陶粒进行吸附脱附实验和孔径测定,具体如图1和图2所示。其中,图1是陶粒的N2吸附脱附等温线,由图中可以看出,当p/p0较低时,对N2的吸附量增长缓慢,表明微孔较少。之后在N2在多孔结构内表面由单层逐渐吸附到多层。此后N2的吸附量在0.6~1范围内迅速增加,产生明显的滞后回线,但当相对压力达到1.0时吸附量的增长未结束,反映出有中孔和大孔的存在。根据ICUPA分类可得,该吸附等温线为具有H1型回滞环的Ⅳ型等温线,Ⅳ型等温线通常可在介孔材料中观察到,H1回滞环能反映出吸附材料是一种尺寸较均匀的球形颗粒,属于孔径分布较均匀的介孔材料。图2是陶粒的BJH孔径分布图可知,孔径在2.750nm处有明显的峰值,说明大部分孔径集中在此范围内,符合介孔(2~50nm)结构特征,该孔径可良好的吸收氟化物、氨氮、磷酸盐和硝态氮。
以上所述是发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以做出若干改进和润饰,这些改进和润饰也视为本发明的保护范围。
Claims (6)
1.一种用于地下水处理的陶粒的制备方法,其特征在于,包括以下步骤:
(1)将铝污泥 20~40重量份,高岭土 10~20重量份,造纸白泥 30~50重量份,陶瓷抛光渣 5~15重量份混合均匀,得到混合物;其中,铝污泥、高岭土、造纸白泥、陶瓷抛光渣的总用量为100份;
(2)将所述混合物成型,得到球形坯体;
(3)将所述球形坯体在950~1050℃烧成,得到陶粒基体;
(4)将陶粒基体浸入含锆溶液中,并将含锆溶液中的溶质干燥去除,即得到用于地下水处理的陶粒成品;
所述铝污泥中Fe2O3的含量≥10wt%,CaO的含量≤12wt%,Al2O3的含量≥35wt%;
所述造纸白泥在600℃、氧化性气氛灼烧至恒重后,质量损失率≥30wt%;
所述造纸白泥在950℃、氧化性气氛灼烧至恒重后,其质量损失率≥70wt%;
所述陶瓷抛光渣中CaO的含量≤1.5wt%,SiO2的含量≥63wt%,Al2O3的含量≥20wt%;
其中,步骤(3)中,烧成曲线为:
从室温到350℃,升温速率为15~20℃/min;
在350℃保温5~10min;
从350℃到850℃,升温速率为8~12℃/min;
从850℃到烧成温度,升温速率为5~20℃/min;
在烧成温度保温10~15min。
2.如权利要求1所述的用于地下水处理的陶粒的制备方法,其特征在于,所述含锆溶液为ZrOCl2水溶液,其浓度为15~30wt%。
3.如权利要求1或2所述的用于地下水处理的陶粒的制备方法,其特征在于,所述铝污泥中Fe2O3的含量为12~20wt%,CaO的含量为3~8wt%,Al2O3的含量为38~48wt%;
所述造纸白泥在600℃、氧化性气氛灼烧至恒重后,质量损失率为35~45wt%;在950℃、氧化性气氛灼烧至恒重后,质量损失率为75~85wt%;
所述陶瓷抛光渣CaO的含量为0.3~1.2wt%,SiO2的含量为64~70wt%,Al2O3的含量20.5~23wt%。
4.如权利要求1所述的用于地下水处理的陶粒的制备方法,其特征在于,所述陶粒基体的显气孔率≥55%,筒压强度≥5MPa,堆积密度≥0.9g/cm3。
5.一种用于地下水处理的陶粒,其特征在于,由如权利要求1至4任一项所述的用于地下水处理的陶粒的制备方法制备而得。
6.如权利要求5所述的用于地下水处理的陶粒在地下水处理以制备饮用水中的应用,其特征在于,处理温度为12~35℃。
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