CN112110711A - 铜渣基磷酸盐多孔微球的制备方法及其应用 - Google Patents
铜渣基磷酸盐多孔微球的制备方法及其应用 Download PDFInfo
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 97
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 97
- 239000010949 copper Substances 0.000 title claims abstract description 97
- 239000002893 slag Substances 0.000 title claims abstract description 97
- 239000004005 microsphere Substances 0.000 title claims abstract description 73
- 229910019142 PO4 Inorganic materials 0.000 title claims abstract description 41
- 239000010452 phosphate Substances 0.000 title claims abstract description 41
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 41
- 239000000843 powder Substances 0.000 claims abstract description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000001035 drying Methods 0.000 claims abstract description 27
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 21
- 229920002545 silicone oil Polymers 0.000 claims abstract description 21
- 239000012153 distilled water Substances 0.000 claims abstract description 20
- 239000004088 foaming agent Substances 0.000 claims abstract description 20
- 239000002002 slurry Substances 0.000 claims abstract description 16
- 229910021538 borax Inorganic materials 0.000 claims abstract description 15
- 235000010339 sodium tetraborate Nutrition 0.000 claims abstract description 15
- 239000004328 sodium tetraborate Substances 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 239000003463 adsorbent Substances 0.000 claims abstract description 7
- 238000001723 curing Methods 0.000 claims abstract description 7
- 229910001385 heavy metal Inorganic materials 0.000 claims abstract description 6
- 239000002244 precipitate Substances 0.000 claims abstract description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 24
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 19
- 238000002156 mixing Methods 0.000 claims description 12
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical group [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 8
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims description 8
- 235000019837 monoammonium phosphate Nutrition 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 7
- 238000007873 sieving Methods 0.000 claims description 7
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims description 4
- 235000019796 monopotassium phosphate Nutrition 0.000 claims description 4
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims description 4
- 235000019799 monosodium phosphate Nutrition 0.000 claims description 4
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 claims description 4
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 4
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 2
- 229910000388 diammonium phosphate Inorganic materials 0.000 claims description 2
- 235000019838 diammonium phosphate Nutrition 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 11
- 238000000034 method Methods 0.000 abstract description 6
- 239000002245 particle Substances 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000010842 industrial wastewater Substances 0.000 abstract description 2
- 150000002500 ions Chemical class 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 239000002351 wastewater Substances 0.000 abstract description 2
- 238000004065 wastewater treatment Methods 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract 2
- 230000007613 environmental effect Effects 0.000 abstract 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 10
- 239000007788 liquid Substances 0.000 description 10
- 239000003960 organic solvent Substances 0.000 description 5
- 239000003208 petroleum Substances 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000001514 detection method Methods 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 239000004568 cement Substances 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- 229910017976 MgO 4 Inorganic materials 0.000 description 1
- 238000010669 acid-base reaction Methods 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 229910052840 fayalite Inorganic materials 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 210000004127 vitreous body Anatomy 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/34—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing cold phosphate binders
- C04B28/344—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing cold phosphate binders the phosphate binder being present in the starting composition solely as one or more phosphates
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0274—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
- B01J20/0292—Phosphates of compounds other than those provided for in B01J20/048
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
- B01J20/28021—Hollow particles, e.g. hollow spheres, microspheres or cenospheres
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
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Abstract
本发明公开了一种铜渣基磷酸盐多孔微球的制备方法,该方法是将磷酸盐与缓凝剂硼砂加入铜渣粉末中搅拌均匀;将发泡剂和蒸馏水加入混合物中搅拌均匀,获得浆料;在水浴加热、搅拌条件下,将浆料滴加到热的二甲基硅油中,液滴在搅拌机械力和二甲基硅油剪应力的作用下,破碎成微球并迅速凝固沉降,收集沉淀,洗涤干燥,在室温下养护固化后获得铜渣基磷酸盐多孔微球;本发明方法成球率超过85%,粒径大小可调;本发明方法实现了废弃物的回收利用,且工艺简单,原料来源广泛,成本低廉,将铜渣基磷酸盐多孔微球应用在废水中重金属离子的吸附中,吸附率高,且能在工业废水处理中连续使用,吸附剂易回收利用,对环境更加友好。
Description
技术领域
本发明涉及吸附剂载体技术和废水处理领域,尤其涉及一种铜渣基磷酸盐多孔微球的制备方法及其应用。
背景技术
铜渣属于大宗工业固体废弃物,其主要矿物组成是铁橄榄石、磁铁矿及一些脉石组成的无定型玻璃体。目前,铜渣的主要处理方式包括:有价金属的提取回收、制备水泥混凝土、堆存处置。现有技术对铜渣中有价金属的回收率不高,且各种技术均造成大量能源消耗,长期运作经济效益差。铜渣作为制备水泥混凝土的原料,其作为原料之一的掺加量较低,不能大规模应用到生产和生活中,此外,在我国大量铜渣的处理方式为堆存处理,在自然条件下,这些物质很难分解,而且铜渣中的有毒物质会向水、大气和土壤中转移,从而直接参与生态系统循环之中,此种处理方式对生态环境有着长期、潜在、间接、综合性的影响。铜渣堆存既占用大量土地资源、污染环境,又造成资源的浪费。而现在对于重金属离子吸附剂的研究多集中于粉末状吸附剂,但粉末状吸附剂不便应用于工业废水的连续化处理以及填充床中,块状吸附剂吸附能力又不足以解决废水中重金属污染的问题。
发明内容
针对现有技术存在的问题,本发明提供了一种简单、廉价、环保的铜渣基磷酸盐多孔微球的制备方法,该方法步骤如下:
(1)将磷酸盐与缓凝剂硼砂加入铜渣粉末中搅拌均匀;
所述铜渣主要成分为:Fe2O3 55~60wt%、SiO2 20~23wt%、MgO 4~5wt%、Al2O3 3~4wt%、CaO 3~4wt%、ZnO 1~2wt%;
所述铜渣粉末是铜渣在温度70~80℃下干燥24h,研磨过80目筛制得;
所述磷酸盐为磷酸二氢铵、磷酸氢二铵、磷酸二氢钾、磷酸二氢钠中的一种;
所述磷酸盐与铜渣粉末的质量比为0.2~0.6:1,缓凝剂硼砂与铜渣粉末的质量比为0.01~0.1:1;
(2)将发泡剂和蒸馏水加入步骤(1)混合物中搅拌均匀,获得浆料;
所述发泡剂为十二烷基酸钠和双氧水按质量比1~3:2~4的比例混合制得;蒸馏水与铜渣的质量比为0.1~0.3:1;十二烷基硫酸钠与铜渣的质量比为0.01~0.04:1;
(3)在水浴加热、搅拌条件下,将浆料滴加到40~80℃的二甲基硅油中,液滴在搅拌机械力和二甲基硅油剪应力的作用下,破碎成微球并迅速凝固沉降,收集沉淀,洗涤干燥,在室温下养护固化后获得铜渣基磷酸盐多孔微球;
所述搅拌速度为500-1000转/min;干燥温度为30~50℃,养护固化时间为0.5~12h。
本发明方法制得的铜渣基磷酸盐多孔微球的平均粒度在5~800μm。
本发明另一目的是将上述方法制得的铜渣基磷酸盐多孔微球应用在重金属吸附中,实验结果显示铜渣基磷酸盐多孔微球对Pb2+吸附率达到80~95%。
本发明的有益效果:
本发明提出利用铜渣作为铁氧化物的来源,与磷酸盐发生酸碱反应制备铜渣基磷酸盐微球并应用于重金属的吸附,本发明制备的铜渣基磷酸盐多孔微球效率高,成球率超过85%,且其吸附能力得到很大的提高,与传统吸附剂相比,在废水领域中实现了易回收,不会对环境产生二次污染,本发明对环境更加友好,在废水处理领域具有较大的应用前景。
具体实施方式
为了更好地理解本发明的内容,下面通过具体的实施例对本发明作进一步详细说明,但本发明保护范围不局限于所述内容;实施例中使用的铜渣主要成分为:Fe2O358.09wt%、SiO2 22.84wt%、MgO 4.99wt%、Al2O3 3.4wt%、CaO 3.28wt%、ZnO 1.67wt%;
实施例1:
(1)将铜渣置于80℃的电热恒温干燥箱中干燥24h,研磨3h过80目筛制得铜渣粉末;将磷酸二氢铵与缓凝剂硼砂加入铜渣粉末中搅拌均匀;其中磷酸二氢铵与铜渣粉末质量比0.25:1,硼砂与铜渣粉末质量比0.01:1;
(2)取十二烷基硫酸钠、双氧水混合制得发泡剂溶液,将发泡剂溶液和蒸馏水缓慢加入步骤(1)混合物中继续搅拌,混合均匀,搅拌1min,使体系形成均一浆料,其中十二烷基硫酸钠和双氧水按质量比1:1的比例混合制得;铜渣粉末和蒸馏水质量比1:0.2;铜渣粉末与十二烷基硫酸钠质量比1:0.02;
(3)在水浴加热、搅拌(搅拌转速650转/min)条件下,将步骤(2)均一浆料用注射器滴入到60℃二甲基硅油中,液滴受到二甲基硅油剪应力和搅拌机械力的作用,破碎成微球并迅速凝固沉降在反应器底部,将微球捞出,用亲水性有机溶剂(石油醚)冲洗去表面和孔道的二甲基硅油后,再用蒸馏水洗涤,然后将放入40℃恒温干燥箱干燥60min,最后在室温下固化30min,即得铜渣基磷酸盐多孔微球,经检测成球率90.2%,微球粒径10-100μm。
(4)将步骤(3)铜渣基磷酸盐多孔微球0.5g放入100mL浓度为100mg/L的Pb2+溶液中30min,多孔微球对Pb2+的吸附率为94.2%。
实施例2:
(1)将铜渣温度70℃的电热恒温干燥箱中干燥24h,研磨3h过80目筛制得铜渣粉末;将磷酸二氢铵与缓凝剂硼砂加入铜渣粉末中搅拌均匀;其中磷酸二氢铵与铜渣粉末质量比0.4:1,硼砂与铜渣粉末质量比0.02:1;
(2)取十二烷基硫酸钠、双氧水混合制得发泡剂溶液,将发泡剂溶液和蒸馏水缓慢加入步骤(1)混合物中继续搅拌,混合均匀,搅拌1min,使体系形成均一浆料,其中十二烷基硫酸钠和双氧水按质量比1:1的比例混合制得;铜渣粉末和蒸馏水质量比1:0.3;铜渣粉末与十二烷基硫酸钠质量比1:0.02;
(3)在水浴加热、搅拌(搅拌转速750转/min)条件下,将步骤(2)均一浆料滴入到40℃二甲基硅油中,液滴受到二甲基硅油剪应力和搅拌机械力的作用,破碎成微球并迅速凝固沉降在反应器底部,将微球捞出,用亲水性有机溶剂(石油醚)冲洗去表面和孔道的二甲基硅油后,再用蒸馏水洗涤,然后将其放入50℃恒温干燥箱干燥60min,最后在室温下固化40min,即得铜渣基磷酸盐多孔微球,经检测成球率89.8%,微球粒径40-150μm;
(4)将步骤(3)铜渣基磷酸盐多孔微球0.5g放入100mL浓度为100mg/L的Pb2+溶液中30min,孔微球对Pb2+的吸附率为87.6%。
实施例3:
(1)将铜渣置于75℃的电热恒温干燥箱中干燥24h,研磨3h过80目筛制得铜渣粉末;将磷酸二氢钾与缓凝剂硼砂加入铜渣中搅拌均匀;其中磷酸二氢钾与铜渣粉末质量比0.6:1,硼砂与铜渣粉末质量比0.1:1;
(2)取十二烷基硫酸钠、双氧水混合制得发泡剂溶液,将发泡剂溶液和蒸馏水缓慢加入步骤(1)混合物中继续搅拌,混合均匀,搅拌1min,使体系形成均一浆料,其中十二烷基硫酸钠和双氧水按质量比1:3的比例混合制得;铜渣粉末和蒸馏水质量比1:0.3;铜渣粉末与十二烷基硫酸钠质量比1:0.03;
(3)在水浴加热、搅拌(800转/min)条件下,将步骤(2)均一浆料滴入到70℃二甲基硅油中,液滴受到二甲基硅油剪应力和搅拌机械力的作用,破碎成微球并迅速凝固沉降在反应器底部,将微球捞出,用亲水性有机溶剂(石油醚)冲洗去表面和孔道的二甲基硅油后,再用蒸馏水洗涤,然后将其放入35℃恒温干燥箱干燥60min,最后在室温下固化50min,即得铜渣基磷酸盐多孔微球,经检测成球率87.8%,微球粒径50-400μm;
(4)将步骤(3)铜渣基磷酸盐多孔微球0.5g放入100mL浓度为100mg/L的Pb2+溶液中30min,孔微球对Pb2+的吸附率为85.6%。
实施例4:
(1)将铜渣置于80℃的电热恒温干燥箱中干燥24h,研磨3h过80目筛制得铜渣粉末;将磷酸二氢铵与缓凝剂硼砂加入铜渣粉末中搅拌均匀;其中磷酸二氢铵与铜渣粉末质量比0.3:1,硼砂与铜渣粉末质量比0.05:1;
(2)取十二烷基硫酸钠、双氧水混合制得发泡剂溶液,将发泡剂溶液和蒸馏水缓慢加入步骤(1)混合物中继续搅拌,混合均匀,搅拌1分钟,使体系形成均一浆料,其中十二烷基硫酸钠和双氧水按质量比3:4的比例混合制得;铜渣粉末和蒸馏水质量比1:0.1;铜渣粉末与十二烷基硫酸钠质量比1:0.02;
(3)在水浴加热、搅拌(900转/min)条件下,将步骤(2)均一浆料滴入到80℃二甲基硅油中,液滴受到二甲基硅油剪应力和搅拌机械力的作用,破碎成微球并迅速凝固沉降在反应器底部,制得微球,将微球捞出,用亲水性有机溶剂(石油醚)冲洗去表面和孔道的二甲基硅油后,再用蒸馏水洗涤,然后将其放入50℃恒温干燥箱干燥60min,最后在室温下固化5h,即得铜渣基磷酸盐多孔微球,经检测成球率88.7%,微球粒径5-200μm;
(4)将步骤(3)铜渣基磷酸盐多孔微球0.5g放入100mL浓度为100mg/l的Pb2+溶液中30min,孔微球对Pb2+的吸附率为89.5%。
实施例5:
(1)将铜渣置于80℃的电热恒温干燥箱中干燥24h,研磨3h过80目筛制得铜渣粉末;将磷酸二氢钠与缓凝剂硼砂加入铜渣中搅拌均匀;其中磷酸二氢钠与铜渣粉末质量比0.2:1,硼砂与铜渣粉末质量比0.02:1;
(2)取十二烷基硫酸钠、双氧水混合制得发泡剂溶液,将发泡剂溶液和蒸馏水缓慢加入步骤(1)混合物中继续搅拌,混合均匀,搅拌1min,使体系形成均一浆料,其中十二烷基硫酸钠和双氧水按质量比3:2的比例混合制得;铜渣粉末和蒸馏水质量比1:0.1;铜渣粉末与十二烷基硫酸钠质量比1:0.03;
(3)在水浴加热、搅拌(600转/min)条件下,将步骤(2)均一浆料滴入到55℃二甲基硅油中,液滴受到二甲基硅油剪应力和搅拌桨叶机械力的作用,破碎成微球并迅速凝固沉降在反应器底部,将微球捞出,用亲水性有机溶剂(石油醚)冲洗去表面和孔道的二甲基硅油后,再用蒸馏水洗涤,然后将其放入40℃恒温干燥箱干燥60min,最后在室温下固化10h,即得铜渣基磷酸盐多孔微球,经检测成球率93.1%,微球粒径5-300μm;
(4)将步骤(3)铜渣基磷酸盐多孔微球0.5g放入100mL浓度为100mg/L的Pb2+溶液中30min,孔微球对Pb2+的吸附率为87.8%。
Claims (8)
1.一种铜渣基磷酸盐多孔微球的制备方法,其特征在于,步骤如下:
(1)将磷酸盐与缓凝剂硼砂加入铜渣粉末中搅拌均匀;
(2)将发泡剂和蒸馏水加入步骤(1)混合物中搅拌均匀,获得浆料;
(3)在水浴加热、搅拌条件下,将浆料滴加到40~80℃的二甲基硅油中,液滴在搅拌机械力和二甲基硅油剪应力的作用下,破碎成微球并迅速凝固沉降,收集沉淀,洗涤干燥,在室温下养护固化后获得铜渣基磷酸盐多孔微球。
2.根据权利要求1所述的铜渣基磷酸盐多孔微球的制备方法,其特征在于:铜渣粉末是铜渣在70~80℃下干燥24h,研磨过80目筛制得。
3.根据权利要求1所述的铜渣基磷酸盐多孔微球的制备方法,其特征在于:磷酸盐为磷酸二氢铵、磷酸氢二铵、磷酸二氢钾或磷酸二氢钠。
4.根据权利要求1所述的铜渣基磷酸盐多孔微球的制备方法,其特征在于:磷酸盐与铜渣粉末的质量比为0.2~0.6:1,缓凝剂硼砂与铜渣粉末的质量比为0.01~0.1:1。
5.根据权利要求1所述的铜渣基磷酸盐多孔微球的制备方法,其特征在于:发泡剂为十二烷基酸钠和双氧水按质量比1~3:2~4的比例混合制得;蒸馏水与铜渣粉末的质量比为0.1~0.3:1;十二烷基硫酸钠与铜渣粉末的质量比为0.01~0.04:1。
6.根据权利要求1所述的铜渣基磷酸盐多孔微球的制备方法,其特征在于:干燥温度为30~50℃,养护固化时间为0.5~12h。
7.根据权利要求1所述的铜渣基磷酸盐多孔微球的制备方法,其特征在于:搅拌速度为500-1000转/min。
8.权利要求1-7中任一项所述的铜渣基磷酸盐多孔微球的制备方法制得的铜渣基磷酸盐多孔微球在作为重金属吸附剂中的应用。
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