CN112090391A - 一种除磷净水剂及其制备方法 - Google Patents
一种除磷净水剂及其制备方法 Download PDFInfo
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- CN112090391A CN112090391A CN202010894128.2A CN202010894128A CN112090391A CN 112090391 A CN112090391 A CN 112090391A CN 202010894128 A CN202010894128 A CN 202010894128A CN 112090391 A CN112090391 A CN 112090391A
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- solution
- purifying agent
- water purifying
- heating
- sodium alginate
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 239000012629 purifying agent Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000002131 composite material Substances 0.000 claims abstract description 48
- 239000000835 fiber Substances 0.000 claims abstract description 45
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000000661 sodium alginate Substances 0.000 claims abstract description 39
- 235000010413 sodium alginate Nutrition 0.000 claims abstract description 39
- 229940005550 sodium alginate Drugs 0.000 claims abstract description 39
- 239000010802 sludge Substances 0.000 claims abstract description 32
- 239000011258 core-shell material Substances 0.000 claims abstract description 29
- 239000011148 porous material Substances 0.000 claims abstract description 29
- 239000002905 metal composite material Substances 0.000 claims abstract description 25
- 239000004005 microsphere Substances 0.000 claims abstract description 25
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims abstract description 15
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 14
- 229920002401 polyacrylamide Polymers 0.000 claims abstract description 14
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims abstract description 13
- 239000002245 particle Substances 0.000 claims abstract description 13
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims abstract description 12
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000011204 carbon fibre-reinforced silicon carbide Substances 0.000 claims abstract description 5
- 239000011248 coating agent Substances 0.000 claims abstract description 4
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- 239000000243 solution Substances 0.000 claims description 66
- 238000003756 stirring Methods 0.000 claims description 51
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 49
- 229910052698 phosphorus Inorganic materials 0.000 claims description 49
- 239000011574 phosphorus Substances 0.000 claims description 49
- 238000004321 preservation Methods 0.000 claims description 36
- 238000009987 spinning Methods 0.000 claims description 33
- 239000010410 layer Substances 0.000 claims description 31
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 27
- 238000002156 mixing Methods 0.000 claims description 26
- 239000008367 deionised water Substances 0.000 claims description 21
- 229910021641 deionized water Inorganic materials 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 19
- 239000011259 mixed solution Substances 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 14
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 14
- 238000001694 spray drying Methods 0.000 claims description 14
- 238000009210 therapy by ultrasound Methods 0.000 claims description 14
- 239000010936 titanium Substances 0.000 claims description 14
- 229910052719 titanium Inorganic materials 0.000 claims description 14
- 239000007787 solid Substances 0.000 claims description 12
- VLDPXPPHXDGHEW-UHFFFAOYSA-N 1-chloro-2-dichlorophosphoryloxybenzene Chemical compound ClC1=CC=CC=C1OP(Cl)(Cl)=O VLDPXPPHXDGHEW-UHFFFAOYSA-N 0.000 claims description 9
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 9
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 claims description 9
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 claims description 9
- 239000004793 Polystyrene Substances 0.000 claims description 9
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 claims description 9
- 229920003257 polycarbosilane Polymers 0.000 claims description 9
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- 238000005245 sintering Methods 0.000 claims description 8
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 238000010041 electrostatic spinning Methods 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 7
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 7
- 239000007921 spray Substances 0.000 claims description 7
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- 238000001179 sorption measurement Methods 0.000 abstract description 9
- 239000000203 mixture Substances 0.000 description 12
- 239000010865 sewage Substances 0.000 description 12
- 239000000126 substance Substances 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 6
- 239000002351 wastewater Substances 0.000 description 6
- 238000004062 sedimentation Methods 0.000 description 5
- 241000894006 Bacteria Species 0.000 description 3
- 229910021536 Zeolite Inorganic materials 0.000 description 3
- 238000005273 aeration Methods 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical group [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 3
- 238000010170 biological method Methods 0.000 description 3
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000012851 eutrophication Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000010457 zeolite Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 235000003891 ferrous sulphate Nutrition 0.000 description 2
- 239000011790 ferrous sulphate Substances 0.000 description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 238000004065 wastewater treatment Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 241000195493 Cryptophyta Species 0.000 description 1
- WYWFMUBFNXLFJK-UHFFFAOYSA-N [Mo].[Sb] Chemical compound [Mo].[Sb] WYWFMUBFNXLFJK-UHFFFAOYSA-N 0.000 description 1
- JAQXDZTWVWLKGC-UHFFFAOYSA-N [O-2].[Al+3].[Fe+2] Chemical compound [O-2].[Al+3].[Fe+2] JAQXDZTWVWLKGC-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000031018 biological processes and functions Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 229920002301 cellulose acetate Polymers 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
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- 238000007865 diluting Methods 0.000 description 1
- 230000035622 drinking Effects 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
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- 238000005728 strengthening Methods 0.000 description 1
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- B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
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Abstract
本发明公开了一种除磷净水剂,该净水剂包括具有次级微球结构层的复合核壳纤维、污泥陶粒、聚丙烯酰胺、聚合硫酸铝、海藻酸钠凝胶改性金属复合物多孔材料;所述具有次级微球结构层的复合核壳纤维是在核壳结构的C/SiC复合纤维表面沉积多孔纳米氧化钛颗粒涂层;所述海藻酸钠凝胶改性金属复合物多孔材料是海藻酸钠凝胶为载体,负载硝酸锰、氯化铁作为活性组分。本发明还公开了该除磷净水剂的制备方法。本发明提供的除磷净水剂吸附能力大,对水体无二次污染,且制备简单,成本低。
Description
技术领域:
本发明涉及废水处理领域,具体涉及一种除磷净水剂及其制备方法。
背景技术:
水作为人类生命当中最为宝贵的自然资源,所以,一旦水资源遭受污染,势必会造成饮用被污染水的人们身患疾病甚至于死亡。造成水体污染的主要原由为农村污水、生活污水以及城市工业污水的排放等。此外,水体富营养化已经成为我国大部分湖泊水体存在的共同问题,水体富营养化不仅会危害水中水生生物的生长,还会影响人体健康。导致这一问题的原因就是大量富含氮、磷等营养元素的市政污水不经处理或处理不完全便排入水体。研究表明:与氮相比,磷是造成水体富营养化的限制因子,当水体中的P>0.01mg/L时就可以刺激藻类生长。目前大多数城市污水处理厂出水磷元素浓度偏高,有些甚至无法达到排放标准。
目前,城市污水处理厂常用的除磷工艺有生物法和化学法。生物法是利用聚磷菌厌氧释磷、好氧吸磷的特性,将磷元素从污水中去除。但是,脱氮菌与聚磷菌本身在碳源、泥龄长短及生长环境上都存在差异,常规的城市污水处理厂工艺需要同时兼顾脱氮除磷,因此很难使出水TP浓度低于1mg/L,必须辅以深度处理强化除磷工艺。世界上许多国家已经做出大量工作,并开展了实际工程,在美国等一些经济发达国家已经得到推广。深度除磷技术也分为生物法和化学法,其中,强化生物除磷成本高,故目前污水处理厂大都采用化学方法深度除磷,即投加化学除磷剂使之与水体中的磷发生化学反应生成沉淀,通过固液分离以达到去除磷的目的。
专利CN200410062964.5公开了一种利用传统污水处理工艺脱氮除磷的工艺,就是在沉砂池末端或初沉池出水口或曝气池曝气段及其出口投加化学除磷剂,同时回流二沉池30%~60%活性污泥及部分剩余污泥至初沉池,使传统污水处理工艺具有生物—化学协同除磷功能;同时在二沉池末端串联曝气沸石生物滤池,利用沸石的物理吸附和生物作用去除二沉池出水中的氨氮,并通过化学—生物协同再生使沸石保持稳定的吸附容量。化学除磷剂为硫酸铝、硫酸亚铁或者二者的混合盐。专利 CN201310196388.2公开了一种污水处理用复合除磷剂及其制备方法,本发明将铝加工废料置于酸液中,常压搅拌反应,控制温度为90-100℃;反应两小时后,加入三氯化铁,搅拌后静止聚合;抽取上层清液于复配池中,制得氧化铝铁溶胶溶液,碱化度控制在30~60%;待氧化铝铁溶胶溶液温度降至40℃以下时,按照0.2-5%的比例,投加季铵盐类有机高分子化合物,搅拌加水调整密度,即得产品。由上述现有技术可知,现有的除磷剂主要为聚合氯化铝、聚合硫酸铁、氯化铁、硫酸铝等产品,其在用于废水除磷时投加量大,除磷效果差,除磷成本高,严重制约了化学除磷技术的推广应用。
发明内容:
本发明要解决的技术问题是,针对现有技术的不足,提供一种除磷净水剂及其制备方法;本发明采用制得的具有次级微球结构层的复合核壳纤维、污泥陶粒以及海藻酸钠凝胶改性金属复合物多孔材料、聚合硫酸铝、聚丙烯酰胺作为复合净水剂,其吸附能力大,对水体无二次污染,且制备简单,成本低。
为解决上述技术问题,本发明采用以下技术方案:
一种除磷净水剂,该净水剂包括具有次级微球结构层的复合核壳纤维、污泥陶粒、聚丙烯酰胺、聚合硫酸铝、海藻酸钠凝胶改性金属复合物多孔材料;所述具有次级微球结构层的复合核壳纤维是在核壳结构的C/SiC复合纤维表面沉积多孔纳米氧化钛颗粒涂层;所述海藻酸钠凝胶改性金属复合物多孔材料是海藻酸钠凝胶为载体,负载硝酸锰、氯化铁作为活性组分。
作为上述技术方案的优选,所述污泥陶粒是采用污泥、碳酸氢钠以质量比为5:(1-2)的比例混合造粒后干燥、预热处理之后进行烧结制得,其比表面积为 83.5-85.5m2/g。
作为上述技术方案的优选,所述预热处理的温度为120℃,所述预热处理的时间为30min。
作为上述技术方案的优选,所述烧结的条件采用分阶段烧结;首先以1℃/min的升温速率升温至280℃,保温处理10min,然后以4℃/min的升温速率升温至450℃,保温处理10min,最后以6℃/min的速率升温至600℃,保温处理40min。
作为上述技术方案的优选,所述各组分的用量以重量份计,分别为具有次级微球结构层的复合核壳纤维5-10份、污泥陶粒10-20份、聚丙烯酰胺7-15份、聚合硫酸铝8-13份、海藻酸钠凝胶改性金属复合物多孔材料3-7份。
为更好的解决上述技术问题,本发明采用以下技术方案:
一种除磷净水剂的制备方法,包括以下步骤:
(1)将十八烷胺溶于二甲基乙酰胺中,搅拌混合后加入均苯四甲酸二酐和苯酐后,在80-90℃下搅拌处理2-4h,制得纺丝溶液A;将聚苯乙烯颗粒、聚碳硅烷溶于 N,N-二甲基甲酰胺中制得溶液B;
(2)以溶液A作为壳层纺丝溶液,以溶液B作为芯层纺丝溶液,采用同轴静电纺丝法制得复合纤维;将1mol钛酸四丁酯溶于50ml无水乙醇中,并滴加0.35mol浓度为1mol/L的盐酸溶液和2mol去离子水,强烈搅拌处理制得钛溶胶;将4-5g上述制得的复合纤维加入到钛溶胶中,500W下超声处理10-30min后,然后升温至60-80℃继续超声处理1-2h,冷却至室温,过滤,将固体进行干燥后置于马弗炉内烧结处理,制得具有次级微球结构层的复合核壳纤维;
(3)将1g海藻酸钠溶于80ml去离子水中,然后加入(0.1-0.3)g硝酸锰和(0.1-0.15) g氯化铁,搅拌分散制得混合溶液;将上述制得的混合溶液缓慢滴加到质量浓度为10%的氯化钙溶液中,40℃下搅拌处理1-2h,之后进行喷雾干燥,制得海藻酸钠凝胶改性金属复合物多孔材料;喷雾干燥时,保持进风口温度为150-180℃,出风口温度为 70-90℃;
(4)将聚丙烯酰胺、聚合硫酸铝和100ml去离子水混合搅拌处理,然后加入污泥陶粒,具有次级微球结构层的复合核壳纤维、海藻酸钠凝胶改性金属复合物多孔材料,继续搅拌混合,之后干燥,制得除磷净水剂。
作为上述技术方案的优选,步骤(1)中,所述十八烷胺、二甲基乙酰胺、均苯四甲酸二酐和苯酐的用量比为10g:(80-100)ml:(10-12)g:(15-20)g。
作为上述技术方案的优选,步骤(1)中,所述聚苯乙烯颗粒、聚碳硅烷、N,N- 二甲基甲酰胺的用量比为1g:(0.8-1)g:50ml。
作为上述技术方案的优选,步骤(2)中,所述同轴静电纺丝工艺具体为:纺丝电压为10-20kV,喷头与收集器的距离为10-20cm,溶液A和溶液B的流量比为(1-5): 1。
作为上述技术方案的优选,步骤(2)中,所述烧结处理的具体过程为:首先以5℃ /min的升温速率升温至500℃保温1h,然后以10℃/min的升温速率升温至800℃,保温处理1h,最后以5℃/min的升温速率升温1200℃,保温处理2h。
由于采用上述技术方案,本发明具有以下有益效果:
本发明提供的除磷净水剂包括具有次级微球结构层的复合核壳纤维、污泥陶粒、聚丙烯酰胺、聚合硫酸铝、海藻酸钠凝胶改性金属复合物多孔材料;所述具有次级微球结构层的复合核壳纤维是在核壳结构的C/SiC复合纤维表面沉积多孔纳米氧化钛颗粒涂层;C/SiC复合纤维不仅力学性能好,且具有很好的孔隙结构,多孔纳米氧化钛在其表面分散性好,纳米氧化钛的孔洞与复合纤维壳层与核层的孔洞不连通,能够提供更大的吸附空间;所述海藻酸钠凝胶改性金属复合物多孔材料是海藻酸钠凝胶为载体,负载硝酸锰、氯化铁作为活性组分;硝酸锰、氯化铁稳定分散在海藻酸钠凝胶的三维网络结构中,具有较多的吸附位点,且海藻酸钠中的羟基、羧基等反应性官能团可有效除去废水中的磷;污泥陶粒中含有大量的Si、Al活性点,对废水中的磷具有很好的吸附凝聚作用。本发明提供的除磷净水剂吸附能力强,具有较多的孔隙,对水体二次污染。
具体实施方式:
下面通过实施例对本发明进一步说明,实施例只用于解释本发明,不会对本发明构成任何的限定。
实施例1
(1)将10g十八烷胺溶于80ml二甲基乙酰胺中,搅拌混合后加入10g均苯四甲酸二酐和15g苯酐后,在80℃下搅拌处理2h,制得纺丝溶液A;将1g聚苯乙烯颗粒、 0.8g聚碳硅烷溶于50mlN,N-二甲基甲酰胺中制得溶液B;
(2)以溶液A作为壳层纺丝溶液,以溶液B作为芯层纺丝溶液,采用同轴静电纺丝法制得复合纤维;纺丝过程中保持纺丝电压为10kV,喷头与收集器的距离为10cm,溶液A和溶液B的流量比为1:1;将1mol钛酸四丁酯溶于50ml无水乙醇中,并滴加0.35mol浓度为1mol/L的盐酸溶液和2mol去离子水,强烈搅拌处理制得钛溶胶;将4g上述制得的复合纤维加入到钛溶胶中,500W下超声处理10min后,然后升温至 60℃继续超声处理1h,冷却至室温,过滤,将固体进行干燥后置于马弗炉内,首先以 5℃/min的升温速率升温至500℃保温1h,然后以10℃/min的升温速率升温至800℃,保温处理1h,最后以5℃/min的升温速率升温1200℃,保温处理2h,制得具有次级微球结构层的复合核壳纤维;
(3)将1g海藻酸钠溶于80ml去离子水中,然后加入0.1g硝酸锰和0.1g氯化铁,搅拌分散制得混合溶液;将上述制得的混合溶液缓慢滴加到质量浓度为10%的氯化钙溶液中,40℃下搅拌处理1h,之后进行喷雾干燥,制得海藻酸钠凝胶改性金属复合物多孔材料;喷雾干燥时,保持进风口温度为150℃,出风口温度为70℃;
(4)污泥、碳酸氢钠以质量比为5:1的比例混合造粒后干燥,在120℃下预热处理之后30min,然后置于电阻炉内,首先以1℃/min的升温速率升温至280℃,保温处理10min,然后以4℃/min的升温速率升温至450℃,保温处理10min,最后以6℃ /min的速率升温至600℃,保温处理40min,制得污泥陶粒;
(5)以重量份计,将7份聚丙烯酰胺、8份聚合硫酸铝和100ml去离子水混合搅拌处理,然后加入10份污泥陶粒,5份具有次级微球结构层的复合核壳纤维、3份海藻酸钠凝胶改性金属复合物多孔材料,继续搅拌混合,之后干燥,制得除磷净水剂。
实施例2
(1)将10g十八烷胺溶于100ml二甲基乙酰胺中,搅拌混合后加入12g均苯四甲酸二酐和20g苯酐后,在90℃下搅拌处理4h,制得纺丝溶液A;将1g聚苯乙烯颗粒、1g聚碳硅烷溶于50ml N,N-二甲基甲酰胺中制得溶液B;
(2)以溶液A作为壳层纺丝溶液,以溶液B作为芯层纺丝溶液,采用同轴静电纺丝法制得复合纤维;纺丝过程中保持纺丝电压为20kV,喷头与收集器的距离为20cm,溶液A和溶液B的流量比为5:1;将1mol钛酸四丁酯溶于50ml无水乙醇中,并滴加0.35mol浓度为1mol/L的盐酸溶液和2mol去离子水,强烈搅拌处理制得钛溶胶;将5g上述制得的复合纤维加入到钛溶胶中,500W下超声处理30min后,然后升温至 80℃继续超声处理2h,冷却至室温,过滤,将固体进行干燥后置于马弗炉内,首先以5℃/min的升温速率升温至500℃保温1h,然后以10℃/min的升温速率升温至800℃,保温处理1h,最后以5℃/min的升温速率升温1200℃,保温处理2h,制得具有次级微球结构层的复合核壳纤维;
(3)将1g海藻酸钠溶于80ml去离子水中,然后加入0.15g硝酸锰和0.15g氯化铁,搅拌分散制得混合溶液;将上述制得的混合溶液缓慢滴加到质量浓度为10%的氯化钙溶液中,40℃下搅拌处理2h,之后进行喷雾干燥,制得海藻酸钠凝胶改性金属复合物多孔材料;喷雾干燥时,保持进风口温度为180℃,出风口温度为90℃;
(4)污泥、碳酸氢钠以质量比为5:2的比例混合造粒后干燥,在120℃下预热处理之后30min,然后置于电阻炉内,首先以1℃/min的升温速率升温至280℃,保温处理10min,然后以4℃/min的升温速率升温至450℃,保温处理10min,最后以6℃ /min的速率升温至600℃,保温处理40min,制得污泥陶粒;
(5)以重量份计,将15份聚丙烯酰胺、13份聚合硫酸铝和100ml去离子水混合搅拌处理,然后加入20份污泥陶粒,10份具有次级微球结构层的复合核壳纤维、7 份海藻酸钠凝胶改性金属复合物多孔材料,继续搅拌混合,之后干燥,制得除磷净水剂。
实施例3
(1)将10g十八烷胺溶于85ml二甲基乙酰胺中,搅拌混合后加入10g均苯四甲酸二酐和20g苯酐后,在85℃下搅拌处理3h,制得纺丝溶液A;将1g聚苯乙烯颗粒、 0.8g聚碳硅烷溶于50ml N,N-二甲基甲酰胺中制得溶液B;
(2)以溶液A作为壳层纺丝溶液,以溶液B作为芯层纺丝溶液,采用同轴静电纺丝法制得复合纤维;纺丝过程中保持纺丝电压为15kV,喷头与收集器的距离为10m,溶液A和溶液B的流量比为2:1;将1mol钛酸四丁酯溶于50ml无水乙醇中,并滴加0.35mol浓度为1mol/L的盐酸溶液和2mol去离子水,强烈搅拌处理制得钛溶胶;将4.5g上述制得的复合纤维加入到钛溶胶中,500W下超声处理15min后,然后升温至65℃继续超声处理1h,冷却至室温,过滤,将固体进行干燥后置于马弗炉内,首先以5℃/min的升温速率升温至500℃保温1h,然后以10℃/min的升温速率升温至 800℃,保温处理1h,最后以5℃/min的升温速率升温1200℃,保温处理2h,制得具有次级微球结构层的复合核壳纤维;
(3)将1g海藻酸钠溶于80ml去离子水中,然后加入0.3g硝酸锰和0.15g氯化铁,搅拌分散制得混合溶液;将上述制得的混合溶液缓慢滴加到质量浓度为10%的氯化钙溶液中,40℃下搅拌处理1.5h,之后进行喷雾干燥,制得海藻酸钠凝胶改性金属复合物多孔材料;喷雾干燥时,保持进风口温度为160℃,出风口温度为75℃;
(4)污泥、碳酸氢钠以质量比为5:1.5的比例混合造粒后干燥,在120℃下预热处理之后30min,然后置于电阻炉内,首先以1℃/min的升温速率升温至280℃,保温处理10min,然后以4℃/min的升温速率升温至450℃,保温处理10min,最后以 6℃/min的速率升温至600℃,保温处理40min,制得污泥陶粒;
(5)以重量份计,将8份聚丙烯酰胺、10份聚合硫酸铝和100ml去离子水混合搅拌处理,然后加入15份污泥陶粒,5份具有次级微球结构层的复合核壳纤维、6份海藻酸钠凝胶改性金属复合物多孔材料,继续搅拌混合,之后干燥,制得除磷净水剂。
实施例4
(1)将10g十八烷胺溶于90ml二甲基乙酰胺中,搅拌混合后加入11g均苯四甲酸二酐和18g苯酐后,在90℃下搅拌处理3h,制得纺丝溶液A;将1g聚苯乙烯颗粒、 0.9g聚碳硅烷溶于50ml N,N-二甲基甲酰胺中制得溶液B;
(2)以溶液A作为壳层纺丝溶液,以溶液B作为芯层纺丝溶液,采用同轴静电纺丝法制得复合纤维;纺丝过程中保持纺丝电压为15kV,喷头与收集器的距离为15m,溶液A和溶液B的流量比为2:1;将1mol钛酸四丁酯溶于50ml无水乙醇中,并滴加0.35mol浓度为1mol/L的盐酸溶液和2mol去离子水,强烈搅拌处理制得钛溶胶;将4-5g上述制得的复合纤维加入到钛溶胶中,500W下超声处理20min后,然后升温至70℃继续超声处理2h,冷却至室温,过滤,将固体进行干燥后置于马弗炉内,首先以5℃/min的升温速率升温至500℃保温1h,然后以10℃/min的升温速率升温至 800℃,保温处理1h,最后以5℃/min的升温速率升温1200℃,保温处理2h,制得具有次级微球结构层的复合核壳纤维;
(3)将1g海藻酸钠溶于80ml去离子水中,然后加入0.2g硝酸锰和0.15g氯化铁,搅拌分散制得混合溶液;将上述制得的混合溶液缓慢滴加到质量浓度为10%的氯化钙溶液中,40℃下搅拌处理2h,之后进行喷雾干燥,制得海藻酸钠凝胶改性金属复合物多孔材料;喷雾干燥时,保持进风口温度为170℃,出风口温度为80℃;
(4)污泥、碳酸氢钠以质量比为5:1的比例混合造粒后干燥,在120℃下预热处理之后30min,然后置于电阻炉内,首先以1℃/min的升温速率升温至280℃,保温处理10min,然后以4℃/min的升温速率升温至450℃,保温处理10min,最后以6℃ /min的速率升温至600℃,保温处理40min,制得污泥陶粒;
(5)以重量份计,将13份聚丙烯酰胺、10份聚合硫酸铝和100ml去离子水混合搅拌处理,然后加入15份污泥陶粒,8份具有次级微球结构层的复合核壳纤维、4 份海藻酸钠凝胶改性金属复合物多孔材料,继续搅拌混合,之后干燥,制得除磷净水剂。
实施例5
(1)将10g十八烷胺溶于95ml二甲基乙酰胺中,搅拌混合后加入10g均苯四甲酸二酐和20g苯酐后,在90℃下搅拌处理3h,制得纺丝溶液A;将1g聚苯乙烯颗粒、 0.8g聚碳硅烷溶于50ml N,N-二甲基甲酰胺中制得溶液B;
(2)以溶液A作为壳层纺丝溶液,以溶液B作为芯层纺丝溶液,采用同轴静电纺丝法制得复合纤维;纺丝过程中保持纺丝电压为20kV,喷头与收集器的距离为15cm,溶液A和溶液B的流量比为4:1;将1mol钛酸四丁酯溶于50ml无水乙醇中,并滴加0.35mol浓度为1mol/L的盐酸溶液和2mol去离子水,强烈搅拌处理制得钛溶胶;将5g上述制得的复合纤维加入到钛溶胶中,500W下超声处理20min后,然后升温至 75℃继续超声处理2h,冷却至室温,过滤,将固体进行干燥后置于马弗炉内,首先以 5℃/min的升温速率升温至500℃保温1h,然后以10℃/min的升温速率升温至800℃,保温处理1h,最后以5℃/min的升温速率升温1200℃,保温处理2h,制得具有次级微球结构层的复合核壳纤维;
(3)将1g海藻酸钠溶于80ml去离子水中,然后加入0.25g硝酸锰和0.15g氯化铁,搅拌分散制得混合溶液;将上述制得的混合溶液缓慢滴加到质量浓度为10%的氯化钙溶液中,40℃下搅拌处理2h,之后进行喷雾干燥,制得海藻酸钠凝胶改性金属复合物多孔材料;喷雾干燥时,保持进风口温度为170℃,出风口温度为80℃;
(4)污泥、碳酸氢钠以质量比为5:2的比例混合造粒后干燥,在120℃下预热处理之后30min,然后置于电阻炉内,首先以1℃/min的升温速率升温至280℃,保温处理10min,然后以4℃/min的升温速率升温至450℃,保温处理10min,最后以6℃ /min的速率升温至600℃,保温处理40min,制得污泥陶粒;
(5)以重量份计,将14份聚丙烯酰胺、12份聚合硫酸铝和100ml去离子水混合搅拌处理,然后加入15份污泥陶粒,10份具有次级微球结构层的复合核壳纤维、6 份海藻酸钠凝胶改性金属复合物多孔材料,继续搅拌混合,之后干燥,制得除磷净水剂。
应用实施例
将模拟废水浓缩液稀释至初始磷浓度为100mg/L,取稀释后的模拟含磷废水150mL于250mL处理器中,调节废水pH至7.00,称取2g上述制得的除磷净水剂于处理器中,将含混合液的处理器置于摇床振荡120h至吸附平衡,控制转速180r/min、温度(25±0.3)℃,定时用注射器取样上清液并过O.45μm醋酸纤维素膜保存。采用钼锑抗分光光度法测定样品磷浓度。测试结果如下:
表1
初始浓度,mg/L | 100 | 除磷率,% |
实施例1 | 0.25 | 99.7 |
实施例2 | 0.20 | 99.8 |
实施例3 | 0.23 | 99.7 |
实施例4 | 0.25 | 99.7 |
实施例5 | 0.3 | 99.8 |
从上述测试结果可以看出,本发明制备的除磷净水剂用于废水处理时除磷效果好,且对水体无二次污染。
虽然已经对本发明的具体实施方案进行了描述,但是本发明的许多其他形式和改变对本领域技术人员而言是显而易见的。应理解所附权利要求和本发明通常涵盖本发明真实精神和范围内的所有这些明显的形式和改变。
Claims (10)
1.一种除磷净水剂,其特征在于,该净水剂包括具有次级微球结构层的复合核壳纤维、污泥陶粒、聚丙烯酰胺、聚合硫酸铝、海藻酸钠凝胶改性金属复合物多孔材料;所述具有次级微球结构层的复合核壳纤维是在核壳结构的C/SiC复合纤维表面沉积多孔纳米氧化钛颗粒涂层;所述海藻酸钠凝胶改性金属复合物多孔材料是海藻酸钠凝胶为载体,负载硝酸锰、氯化铁作为活性组分。
2.根据权利要求1所述的一种除磷净水剂,其特征在于:所述污泥陶粒是采用污泥、碳酸氢钠以质量比为5:(1-2)的比例混合造粒后干燥、预热处理之后进行烧结制得,其比表面积为83.5-85.5m2/g。
3.根据权利要求2所述的一种除磷净水剂,其特征在于:所述预热处理的温度为120℃,所述预热处理的时间为30min。
4.根据权利要求2所述的一种除磷净水剂,其特征在于:所述烧结的条件采用分阶段烧结;首先以1℃/min的升温速率升温至280℃,保温处理10min,然后以4℃/min的升温速率升温至450℃,保温处理10min,最后以6℃/min的速率升温至600℃,保温处理40min。
5.根据权利要求1所述的一种除磷净水剂,其特征在于:所述各组分的用量以重量份计,分别为具有次级微球结构层的复合核壳纤维5-10份、污泥陶粒10-20份、聚丙烯酰胺7-15份、聚合硫酸铝8-13份、海藻酸钠凝胶改性金属复合物多孔材料3-7份。
6.根据权利要求1至5任一所述的一种除磷净水剂的制备方法,其特征在于,包括以下步骤:
(1)将十八烷胺溶于二甲基乙酰胺中,搅拌混合后加入均苯四甲酸二酐和苯酐后,在80-90℃下搅拌处理2-4h,制得纺丝溶液A;将聚苯乙烯颗粒、聚碳硅烷溶于N,N-二甲基甲酰胺中制得溶液B;
(2)以溶液A作为壳层纺丝溶液,以溶液B作为芯层纺丝溶液,采用同轴静电纺丝法制得复合纤维;将1mol钛酸四丁酯溶于50ml无水乙醇中,并滴加0.35mol浓度为1mol/L的盐酸溶液和2mol去离子水,强烈搅拌处理制得钛溶胶;将4-5g上述制得的复合纤维加入到钛溶胶中,500W下超声处理10-30min后,然后升温至60-80℃继续超声处理1-2h,冷却至室温,过滤,将固体进行干燥后置于马弗炉内烧结处理,制得具有次级微球结构层的复合核壳纤维;
(3)将1g海藻酸钠溶于80ml去离子水中,然后加入(0.1-0.3)g硝酸锰和(0.1-0.15)g氯化铁,搅拌分散制得混合溶液;将上述制得的混合溶液缓慢滴加到质量浓度为10%的氯化钙溶液中,40℃下搅拌处理1-2h,之后进行喷雾干燥,制得海藻酸钠凝胶改性金属复合物多孔材料;喷雾干燥时,保持进风口温度为150-180℃,出风口温度为70-90℃;
(4)将聚丙烯酰胺、聚合硫酸铝和100ml去离子水混合搅拌处理,然后加入污泥陶粒,具有次级微球结构层的复合核壳纤维、海藻酸钠凝胶改性金属复合物多孔材料,继续搅拌混合,之后干燥,制得除磷净水剂。
7.根据权利要求6所述的一种除磷净水剂的制备方法,其特征在于,步骤(1)中,所述十八烷胺、二甲基乙酰胺、均苯四甲酸二酐和苯酐的用量比为10g:(80-100)ml:(10-12)g:(15-20)g。
8.根据权利要求6所述的一种除磷净水剂的制备方法,其特征在于,步骤(1)中,所述聚苯乙烯颗粒、聚碳硅烷、N,N-二甲基甲酰胺的用量比为1g:(0.8-1)g:50ml。
9.根据权利要求6所述的一种除磷净水剂的制备方法,其特征在于,步骤(2)中,所述同轴静电纺丝工艺具体为:纺丝电压为10-20kV,喷头与收集器的距离为10-20cm,溶液A和溶液B的流量比为(1-5):1。
10.根据权利要求6所述的一种除磷净水剂的制备方法,其特征在于,步骤(2)中,所述烧结处理的具体过程为:首先以5℃/min的升温速率升温至500℃保温1h,然后以10℃/min的升温速率升温至800℃,保温处理1h,最后以5℃/min的升温速率升温1200℃,保温处理2h。
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