CN115353124B - 一种原卤硫化物绿色氧化祛除工艺 - Google Patents
一种原卤硫化物绿色氧化祛除工艺 Download PDFInfo
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- 229910052736 halogen Inorganic materials 0.000 title claims abstract description 92
- 238000000034 method Methods 0.000 title claims abstract description 52
- 230000003647 oxidation Effects 0.000 title claims abstract description 25
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 25
- -1 halogen sulfide Chemical class 0.000 title claims abstract description 20
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 92
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims abstract description 91
- 150000002367 halogens Chemical class 0.000 claims abstract description 72
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000007864 aqueous solution Substances 0.000 claims description 52
- 239000002131 composite material Substances 0.000 claims description 42
- 239000012798 spherical particle Substances 0.000 claims description 38
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 36
- 238000001354 calcination Methods 0.000 claims description 28
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Chemical compound [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 claims description 24
- 239000011259 mixed solution Substances 0.000 claims description 22
- 238000002156 mixing Methods 0.000 claims description 20
- 230000010355 oscillation Effects 0.000 claims description 13
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 12
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 12
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 12
- 229910052878 cordierite Inorganic materials 0.000 claims description 12
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 claims description 12
- WFLYOQCSIHENTM-UHFFFAOYSA-N molybdenum(4+) tetranitrate Chemical compound [N+](=O)([O-])[O-].[Mo+4].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-] WFLYOQCSIHENTM-UHFFFAOYSA-N 0.000 claims description 12
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 12
- 229910001209 Low-carbon steel Inorganic materials 0.000 claims description 11
- 238000005868 electrolysis reaction Methods 0.000 claims description 11
- 239000010935 stainless steel Substances 0.000 claims description 11
- 229910001220 stainless steel Inorganic materials 0.000 claims description 11
- 238000000227 grinding Methods 0.000 claims description 10
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- 230000001590 oxidative effect Effects 0.000 claims 2
- 230000000694 effects Effects 0.000 abstract description 8
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 238000001556 precipitation Methods 0.000 abstract 1
- 239000012267 brine Substances 0.000 description 17
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 10
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- 238000003756 stirring Methods 0.000 description 9
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- 241001131796 Botaurus stellaris Species 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 4
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 3
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- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 3
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- 238000006243 chemical reaction Methods 0.000 description 2
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- 229910052801 chlorine Inorganic materials 0.000 description 2
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- 239000000047 product Substances 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- 150000004763 sulfides Chemical class 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- MBMLMWLHJBBADN-UHFFFAOYSA-N Ferrous sulfide Chemical compound [Fe]=S MBMLMWLHJBBADN-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- HTBDEQQYMMCKQW-UHFFFAOYSA-N [S].OO Chemical compound [S].OO HTBDEQQYMMCKQW-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical group 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000008239 natural water Substances 0.000 description 1
- 229920001021 polysulfide Polymers 0.000 description 1
- 239000005077 polysulfide Substances 0.000 description 1
- 150000008117 polysulfides Polymers 0.000 description 1
- JLKDVMWYMMLWTI-UHFFFAOYSA-M potassium iodate Chemical compound [K+].[O-]I(=O)=O JLKDVMWYMMLWTI-UHFFFAOYSA-M 0.000 description 1
- 239000001230 potassium iodate Substances 0.000 description 1
- 235000006666 potassium iodate Nutrition 0.000 description 1
- 229940093930 potassium iodate Drugs 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- HYHCSLBZRBJJCH-UHFFFAOYSA-N sodium polysulfide Chemical compound [Na+].S HYHCSLBZRBJJCH-UHFFFAOYSA-N 0.000 description 1
- VGTPCRGMBIAPIM-UHFFFAOYSA-M sodium thiocyanate Chemical compound [Na+].[S-]C#N VGTPCRGMBIAPIM-UHFFFAOYSA-M 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
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- C01D3/00—Halides of sodium, potassium or alkali metals in general
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- C01D3/06—Preparation by working up brines; seawater or spent lyes
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Abstract
本发明公开了一种原卤硫化物绿色氧化祛除工艺,通过向原卤中加入质量浓度40~50%双氧水,进行电化学处理,使得原卤中的硫化物被氧化为单质硫,静置,除去沉淀即可实现原卤硫化物绿色氧化祛除。本发明从源头控制,降低原卤中硫化物含量,硫化物祛除效果好,工艺简单,绿色环保。双氧水的加入量通过原卤中硫化物含量进行确定,精准实现硫化物的祛除,高效彻底,稳定节约。
Description
技术领域
本发明涉及一种原卤处理工艺,具体涉及一种原卤硫化物绿色氧化祛除工艺。属于食盐加工技术领域。
背景技术
硫化物具有毒性、腐蚀性,且有恶臭,如果直接排放会对环境造成极大的污染。我国《污水综合排放标准》对工业废水中硫化物的排放限值进行了严格控制,其中一、二级标准为0.5mg/L,三级标准为1mg/L。因此,生产、生活中的含硫废水必须加以妥善处理。环保部门对含硫废水的排放进行了严格的监督和管制,最新的《生活饮用水卫生标准》(GB5749-2006)也规定生活饮用水中硫化物的含量不得高于20μg/L,但自然水体和生活饮用水源硫化物超标的事件仍时有发生。
原卤是指未用化学或物理方法处理过的卤水。制盐卤水分为天然卤水和人工卤水。天然卤水包括黑卤、黄卤、油(气)田水和咸湖水,天然咸水湖亦可作为天然卤水。将淡水注入井下盐层或用淡水加入固体盐中,使其溶解为含氯化钠较高的溶液,即为人工卤水。原卤中往往含有硫化物(包括硫化氢、硫化钠、硫氰化钠、硫化亚铁、焦硫化钠、多硫化钙、多硫化钠等)等杂质,严重影响卤水的色度及浊度,导致设备结疤,在加工成碘盐时,还会将碘酸钾还原为碘,导致食盐变红或变黄影响产品质量。原卤中硫化物含量居高不下,自然也有环境污染的风险。故原卤中硫化物超标带来环保、质量双重压力,严重制约了制盐工业的发展。
目前通常采用空气吹出法、支条架法、氯气直接氧化法、空气吹出-氯气氧化法、空气吹出-三氯化铁法等方法祛除原卤中的硫化氢,但这些方法仅限于气态形式存在的硫化氢的祛除,而以化合态形式存在的硫化物无法祛除,或者在冷态状况下祛除后经高温加热发生可逆反应再次在高温状态下形成硫化物。
发明内容
本发明的目的是为克服上述现有技术的不足,提供一种原卤硫化物绿色氧化祛除工艺,从源头控制,降低原卤中硫化物含量,工艺简单,绿色环保。
为实现上述目的,本发明采用下述技术方案:
一种原卤硫化物绿色氧化祛除工艺,向原卤中加入质量浓度40~50%双氧水,进行电化学处理,使得原卤中的硫化物被氧化为单质硫,静置,除去沉淀即可。
优选的,双氧水的加入量通过原卤中硫化物含量进行确定,1mg硫化物对应加入1~2mL双氧水。
进一步优选的,原卤中硫化物含量测定参考HZ-HJ-SZ-0144《水质硫化物的测定硫离子选择电极电位滴定法》。
优选的,加入双氧水后以300~500r/min搅拌5~7分钟。
优选的,电化学处理使用低碳钢板为阳极,不锈钢板为阴极,阳极与阴极之间的距离为3~5mm,电流密度为6~8mA/cm2,工作电压为3~4V,电解时间为50~60s。
优选的,在加入双氧水前,先向原卤中加入复合材料,复合材料与原卤的质量比为2~3:100,所述复合材料是通过以下方法制备得到的:
(A)先将100~200目赤泥、100~200目堇青石与质量浓度1~2%聚乙烯醇水溶液研磨混合造粒,煅烧,得到球状颗粒;
(B)然后将1~2mol/L硝酸钴水溶液、1~2mol/L硝酸锶水溶液、1~2mol/L硝酸钼水溶液和1~2mol/L柠檬酸水溶液混合均匀得到混合液,再将球状颗粒完全浸没于混合液中,超声波振荡处理,取出后煅烧,即得所述的复合材料。
进一步优选的,步骤(A)中,赤泥、堇青石与聚乙烯醇水溶液的质量比为25~30:5~6:1。
进一步优选的,步骤(A)中,煅烧的工艺条件为:800~900℃煅烧3~4小时。
进一步优选的,步骤(A)中,球状颗粒的粒径为1~2cm。
进一步优选的,步骤(B)中,硝酸钴水溶液、硝酸锶水溶液、硝酸钼水溶液和柠檬酸水溶液的体积比为1:1:1:1,球状颗粒与混合液的质量比为1:8~10。
进一步优选的,步骤(B)中,超声波振荡处理的工艺条件为:400~500W超声波振荡处理30~40分钟。
进一步优选的,步骤(B)中,煅烧的工艺条件为:800~900℃煅烧4~5小时。
本发明的有益效果:
本发明通过向原卤中加入质量浓度40~50%双氧水,进行电化学处理,使得原卤中的硫化物被氧化为单质硫,静置,除去沉淀即可实现原卤硫化物绿色氧化祛除。本发明从源头控制,降低原卤中硫化物含量,硫化物祛除效果好,工艺简单,绿色环保。双氧水的加入量通过原卤中硫化物含量进行确定,精准实现硫化物的祛除,高效彻底,稳定节约。
本发明将双氧水除硫与电化学处理结合起来,使用低碳钢板为阳极,不锈钢板为阴极,通过控制阳极与阴极之间的距离、电流密度、工作电压、电解时间等实现了原卤中硫化物的彻底祛除,大大降低了原卤中硫化物含量。
在加入双氧水前,先向原卤中加入复合材料,可进一步改善硫化物祛除效果。复合材料是通过以下方法制备得到的:先将赤泥、堇青石与聚乙烯醇水溶液研磨混合造粒,煅烧,得到球状颗粒;然后将硝酸钴水溶液、硝酸锶水溶液、硝酸钼水溶液和柠檬酸水溶液混合均匀得到混合液,再将球状颗粒完全浸没于混合液中,超声波振荡处理,取出后煅烧,即得。球状颗粒对原卤中的杂质具有一定的吸附作用,同时可催化促进硫化物等杂质转化,进一步改善了原卤处理效果,特别是硫化物祛除效果。
具体实施方式
下面结合实施例对本发明进行进一步的阐述,应该说明的是,下述说明仅是为了解释本发明,并不对其内容进行限定。
实施例1:
一种原卤硫化物绿色氧化祛除工艺,向原卤中加入质量浓度40%双氧水,以300r/min搅拌5分钟,进行电化学处理,使得原卤中的硫化物被氧化为单质硫,静置,除去沉淀即可。
双氧水的加入量通过原卤中硫化物含量进行确定,1mg硫化物对应加入1mL双氧水。
原卤中硫化物含量测定参考HZ-HJ-SZ-0144《水质硫化物的测定硫离子选择电极电位滴定法》。
电化学处理使用低碳钢板为阳极,不锈钢板为阴极,阳极与阴极之间的距离为3mm,电流密度为6mA/cm2,工作电压为3V,电解时间为50s。
在加入双氧水前,先向原卤中加入复合材料,复合材料与原卤的质量比为2:100,所述复合材料是通过以下方法制备得到的:
(A)先将25g 100目赤泥、5g 100目堇青石与1g质量浓度1%聚乙烯醇水溶液研磨混合造粒,800℃煅烧3小时,得到粒径1cm的球状颗粒;
(B)然后将1mol/L硝酸钴水溶液、1mol/L硝酸锶水溶液、1mol/L硝酸钼水溶液和1mol/L柠檬酸水溶液按照体积比1:1:1:1混合均匀得到混合液,再将球状颗粒完全浸没于其8倍重量的混合液中,400W超声波振荡处理30分钟,取出,800℃煅烧4小时,即得所述的复合材料。
实施例2:
一种原卤硫化物绿色氧化祛除工艺,向原卤中加入质量浓度50%双氧水,以500r/min搅拌7分钟,进行电化学处理,使得原卤中的硫化物被氧化为单质硫,静置,除去沉淀即可。
双氧水的加入量通过原卤中硫化物含量进行确定,1mg硫化物对应加入2mL双氧水。
原卤中硫化物含量测定参考HZ-HJ-SZ-0144《水质硫化物的测定硫离子选择电极电位滴定法》。
电化学处理使用低碳钢板为阳极,不锈钢板为阴极,阳极与阴极之间的距离为5mm,电流密度为8mA/cm2,工作电压为4V,电解时间为60s。
在加入双氧水前,先向原卤中加入复合材料,复合材料与原卤的质量比为3:100,所述复合材料是通过以下方法制备得到的:
(A)先将30g 200目赤泥、6g 200目堇青石与1g质量浓度2%聚乙烯醇水溶液研磨混合造粒,900℃煅烧4小时,得到粒径2cm的球状颗粒;
(B)然后将2mol/L硝酸钴水溶液、2mol/L硝酸锶水溶液、2mol/L硝酸钼水溶液和2mol/L柠檬酸水溶液按照体积比1:1:1:1混合均匀得到混合液,再将球状颗粒完全浸没于其10倍重量的混合液中,500W超声波振荡处理40分钟,取出,900℃煅烧5小时,即得所述的复合材料。
实施例3:
一种原卤硫化物绿色氧化祛除工艺,向原卤中加入质量浓度40%双氧水,以500r/min搅拌5分钟,进行电化学处理,使得原卤中的硫化物被氧化为单质硫,静置,除去沉淀即可。
双氧水的加入量通过原卤中硫化物含量进行确定,1mg硫化物对应加入2mL双氧水。
原卤中硫化物含量测定参考HZ-HJ-SZ-0144《水质硫化物的测定硫离子选择电极电位滴定法》。
电化学处理使用低碳钢板为阳极,不锈钢板为阴极,阳极与阴极之间的距离为3mm,电流密度为8mA/cm2,工作电压为3V,电解时间为60s。
在加入双氧水前,先向原卤中加入复合材料,复合材料与原卤的质量比为2:100,所述复合材料是通过以下方法制备得到的:
(A)先将30g 100目赤泥、6g 100目堇青石与1g质量浓度2%聚乙烯醇水溶液研磨混合造粒,800℃煅烧4小时,得到粒径1cm的球状颗粒;
(B)然后将2mol/L硝酸钴水溶液、1mol/L硝酸锶水溶液、2mol/L硝酸钼水溶液和1mol/L柠檬酸水溶液按照体积比1:1:1:1混合均匀得到混合液,再将球状颗粒完全浸没于其10倍重量的混合液中,400W超声波振荡处理40分钟,取出,800℃煅烧5小时,即得所述的复合材料。
实施例4:
一种原卤硫化物绿色氧化祛除工艺,向原卤中加入质量浓度50%双氧水,以300r/min搅拌7分钟,进行电化学处理,使得原卤中的硫化物被氧化为单质硫,静置,除去沉淀即可。
双氧水的加入量通过原卤中硫化物含量进行确定,1mg硫化物对应加入1mL双氧水。
原卤中硫化物含量测定参考HZ-HJ-SZ-0144《水质硫化物的测定硫离子选择电极电位滴定法》。
电化学处理使用低碳钢板为阳极,不锈钢板为阴极,阳极与阴极之间的距离为5mm,电流密度为6mA/cm2,工作电压为4V,电解时间为50s。
在加入双氧水前,先向原卤中加入复合材料,复合材料与原卤的质量比为3:100,所述复合材料是通过以下方法制备得到的:
(A)先将25g 200目赤泥、5g 200目堇青石与1g质量浓度1%聚乙烯醇水溶液研磨混合造粒,900℃煅烧3小时,得到粒径2cm的球状颗粒;
(B)然后将1mol/L硝酸钴水溶液、2mol/L硝酸锶水溶液、1mol/L硝酸钼水溶液和2mol/L柠檬酸水溶液按照体积比1:1:1:1混合均匀得到混合液,再将球状颗粒完全浸没于其8倍重量的混合液中,500W超声波振荡处理30分钟,取出,900℃煅烧4小时,即得所述的复合材料。
实施例5:
一种原卤硫化物绿色氧化祛除工艺,向原卤中加入质量浓度45%双氧水,以400r/min搅拌6分钟,进行电化学处理,使得原卤中的硫化物被氧化为单质硫,静置,除去沉淀即可。
双氧水的加入量通过原卤中硫化物含量进行确定,1mg硫化物对应加入1.5mL双氧水。
原卤中硫化物含量测定参考HZ-HJ-SZ-0144《水质硫化物的测定硫离子选择电极电位滴定法》。
电化学处理使用低碳钢板为阳极,不锈钢板为阴极,阳极与阴极之间的距离为4mm,电流密度为7mA/cm2,工作电压为3V,电解时间为55s。
在加入双氧水前,先向原卤中加入复合材料,复合材料与原卤的质量比为2.5:100,所述复合材料是通过以下方法制备得到的:
(A)先将28g 150目赤泥、5.5g 150目堇青石与1g质量浓度1.5%聚乙烯醇水溶液研磨混合造粒,850℃煅烧3.5小时,得到粒径2cm的球状颗粒;
(B)然后将1.5mol/L硝酸钴水溶液、1.5mol/L硝酸锶水溶液、1.5mol/L硝酸钼水溶液和1.5mol/L柠檬酸水溶液按照体积比1:1:1:1混合均匀得到混合液,再将球状颗粒完全浸没于其9倍重量的混合液中,500W超声波振荡处理35分钟,取出,850℃煅烧4.5小时,即得所述的复合材料。
对比例1
一种原卤硫化物绿色氧化祛除工艺,向原卤中加入质量浓度40%双氧水,以300r/min搅拌5分钟,进行电化学处理,使得原卤中的硫化物被氧化为单质硫,静置,除去沉淀即可。
双氧水的加入量通过原卤中硫化物含量进行确定,1mg硫化物对应加入1mL双氧水。
原卤中硫化物含量测定参考HZ-HJ-SZ-0144《水质硫化物的测定硫离子选择电极电位滴定法》。
电化学处理使用低碳钢板为阳极,不锈钢板为阴极,阳极与阴极之间的距离为3mm,电流密度为6mA/cm2,工作电压为3V,电解时间为50s。
对比例2
一种原卤硫化物绿色氧化祛除工艺,向原卤中加入质量浓度40%双氧水,以300r/min搅拌5分钟,进行电化学处理,使得原卤中的硫化物被氧化为单质硫,静置,除去沉淀即可。
双氧水的加入量通过原卤中硫化物含量进行确定,1mg硫化物对应加入1mL双氧水。
原卤中硫化物含量测定参考HZ-HJ-SZ-0144《水质硫化物的测定硫离子选择电极电位滴定法》。
电化学处理使用低碳钢板为阳极,不锈钢板为阴极,阳极与阴极之间的距离为3mm,电流密度为6mA/cm2,工作电压为3V,电解时间为50s。
在加入双氧水前,先向原卤中加入复合材料,复合材料与原卤的质量比为2:100,所述复合材料是通过以下方法制备得到的:
(A)先将25g 100目赤泥与1g质量浓度1%聚乙烯醇水溶液研磨混合造粒,800℃煅烧3小时,得到粒径1cm的球状颗粒;
(B)然后将1mol/L硝酸钴水溶液、1mol/L硝酸锶水溶液、1mol/L硝酸钼水溶液和1mol/L柠檬酸水溶液按照体积比1:1:1:1混合均匀得到混合液,再将球状颗粒完全浸没于其8倍重量的混合液中,400W超声波振荡处理30分钟,取出,800℃煅烧4小时,即得所述的复合材料。
对比例3
一种原卤硫化物绿色氧化祛除工艺,向原卤中加入质量浓度40%双氧水,以300r/min搅拌5分钟,进行电化学处理,使得原卤中的硫化物被氧化为单质硫,静置,除去沉淀即可。
双氧水的加入量通过原卤中硫化物含量进行确定,1mg硫化物对应加入1mL双氧水。
原卤中硫化物含量测定参考HZ-HJ-SZ-0144《水质硫化物的测定硫离子选择电极电位滴定法》。
电化学处理使用低碳钢板为阳极,不锈钢板为阴极,阳极与阴极之间的距离为3mm,电流密度为6mA/cm2,工作电压为3V,电解时间为50s。
在加入双氧水前,先向原卤中加入复合材料,复合材料与原卤的质量比为2:100,所述复合材料是通过以下方法制备得到的:
(A)先将25g 100目赤泥、5g 100目堇青石与1g质量浓度1%聚乙烯醇水溶液研磨混合造粒,800℃煅烧3小时,得到粒径1cm的球状颗粒;
(B)然后将1mol/L硝酸钴水溶液、1mol/L硝酸钼水溶液和1mol/L柠檬酸水溶液按照体积比1:1:1:1混合均匀得到混合液,再将球状颗粒完全浸没于其8倍重量的混合液中,400W超声波振荡处理30分钟,取出,800℃煅烧4小时,即得所述的复合材料。
试验例
为便于比较,实施例1~5和对比例1~3对相同来源的原卤进行处理,通过HZ-HJ-SZ-0144《水质硫化物的测定硫离子选择电极电位滴定法》检测原卤中硫化物含量为173.47mg/L,处理后再次检测所得卤水中硫化物含量,并采用WGZ-200型散射式光电浊度计测试浑浊度,结果见表1。
表1.处理后所得卤水中硫化物含量
硫化物含量(mg/L) | 浊度(JTU) | |
实施例1 | 0.34 | 0.5 |
实施例2 | 0.33 | 0.5 |
实施例3 | 0.28 | 0.4 |
实施例4 | 0.29 | 0.4 |
实施例5 | 0.25 | 0.3 |
对比例1 | 6.57 | 2.8 |
对比例2 | 2.33 | 1.3 |
对比例3 | 2.61 | 1.3 |
由表1可知,实施例1~5的工艺处理后所得卤水中硫化物含量低,浊度低,说明硫化物祛除效果好。
对比例1略去复合材料的加入,对比例2在制备复合材料时略去堇青石,对比例3在制备复合材料时略去硝酸锶水溶液,所得卤水中硫化物含量明显较高,浊度高,说明本发明的复合材料对于硫化物氧化祛除具有促进作用。
上述虽然对本发明的具体实施方式进行了描述,但并非对本发明保护范围的限制,在本发明的技术方案的基础上,本领域技术人员不需要付出创造性劳动即可做出的各种修改或变形仍在本发明的保护范围以内。
Claims (9)
1.一种原卤硫化物绿色氧化祛除工艺,其特征在于,向原卤中加入质量浓度40~50%双氧水,进行电化学处理,使得原卤中的硫化物被氧化为单质硫,静置,除去沉淀即可;
在加入双氧水前,先向原卤中加入复合材料,复合材料与原卤的质量比为2~3:100,所述复合材料是通过以下方法制备得到的:
(A)先将100~200目赤泥、100~200目堇青石与质量浓度1~2%聚乙烯醇水溶液研磨混合造粒,煅烧,得到球状颗粒;
(B)然后将1~2mol/L硝酸钴水溶液、1~2mol/L硝酸锶水溶液、1~2mol/L硝酸钼水溶液和1~2mol/L柠檬酸水溶液混合均匀得到混合液,再将球状颗粒完全浸没于混合液中,超声波振荡处理,取出后煅烧,即得所述的复合材料。
2.根据权利要求1所述的一种原卤硫化物绿色氧化祛除工艺,其特征在于,双氧水的加入量通过原卤中硫化物含量进行确定,1mg硫化物对应加入1~2mL双氧水。
3.根据权利要求1所述的一种原卤硫化物绿色氧化祛除工艺,其特征在于,加入双氧水后以300~500r/min搅拌5~7分钟。
4.根据权利要求1所述的一种原卤硫化物绿色氧化祛除工艺,其特征在于,电化学处理使用低碳钢板为阳极,不锈钢板为阴极,阳极与阴极之间的距离为3~5mm,电流密度为6~8mA/cm2,工作电压为3~4V,电解时间为50~60s。
5.根据权利要求1所述的一种原卤硫化物绿色氧化祛除工艺,其特征在于,步骤(A)中,赤泥、堇青石与聚乙烯醇水溶液的质量比为25~30:5~6:1。
6.根据权利要求1所述的一种原卤硫化物绿色氧化祛除工艺,其特征在于,步骤(A)中,煅烧的工艺条件为:800~900℃煅烧3~4小时。
7.根据权利要求1所述的一种原卤硫化物绿色氧化祛除工艺,其特征在于,步骤(B)中,硝酸钴水溶液、硝酸锶水溶液、硝酸钼水溶液和柠檬酸水溶液的体积比为1:1:1:1,球状颗粒与混合液的质量比为1:8~10。
8.根据权利要求1所述的一种原卤硫化物绿色氧化祛除工艺,其特征在于,步骤(B)中,超声波振荡处理的工艺条件为:400~500W超声波振荡处理30~40分钟。
9.根据权利要求1所述的一种原卤硫化物绿色氧化祛除工艺,其特征在于,步骤(B)中,煅烧的工艺条件为:800~900℃煅烧4~5小时。
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