CN116116378A - 一种利用磷矿尾矿制作磷吸附材料的制备方法 - Google Patents
一种利用磷矿尾矿制作磷吸附材料的制备方法 Download PDFInfo
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 89
- 239000011574 phosphorus Substances 0.000 title claims abstract description 89
- 229910052698 phosphorus Inorganic materials 0.000 title claims abstract description 89
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 58
- 239000000463 material Substances 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000002367 phosphate rock Substances 0.000 title claims description 7
- 239000002994 raw material Substances 0.000 claims abstract description 27
- 239000002351 wastewater Substances 0.000 claims abstract description 25
- 239000002002 slurry Substances 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 16
- 239000010452 phosphate Substances 0.000 claims abstract description 16
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 16
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000011575 calcium Substances 0.000 claims abstract description 12
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 12
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 12
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- 239000002131 composite material Substances 0.000 claims abstract description 11
- 230000035484 reaction time Effects 0.000 claims abstract description 9
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- 239000010881 fly ash Substances 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 13
- 239000002893 slag Substances 0.000 claims description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 11
- 239000010440 gypsum Substances 0.000 claims description 11
- 229910052602 gypsum Inorganic materials 0.000 claims description 11
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 10
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 8
- 239000000920 calcium hydroxide Substances 0.000 claims description 8
- 235000011116 calcium hydroxide Nutrition 0.000 claims description 8
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 8
- PASHVRUKOFIRIK-UHFFFAOYSA-L calcium sulfate dihydrate Chemical compound O.O.[Ca+2].[O-]S([O-])(=O)=O PASHVRUKOFIRIK-UHFFFAOYSA-L 0.000 claims description 8
- OBSZRRSYVTXPNB-UHFFFAOYSA-N tetraphosphorus Chemical compound P12P3P1P32 OBSZRRSYVTXPNB-UHFFFAOYSA-N 0.000 claims description 8
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- 229910000831 Steel Inorganic materials 0.000 claims description 5
- 239000000292 calcium oxide Substances 0.000 claims description 5
- 235000012255 calcium oxide Nutrition 0.000 claims description 5
- 239000010959 steel Substances 0.000 claims description 5
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 claims description 3
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 3
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 claims description 3
- 235000019738 Limestone Nutrition 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 239000006028 limestone Substances 0.000 claims description 2
- 239000010865 sewage Substances 0.000 abstract description 4
- 238000005187 foaming Methods 0.000 abstract description 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 7
- 235000011941 Tilia x europaea Nutrition 0.000 description 7
- 239000004571 lime Substances 0.000 description 7
- 239000000203 mixture Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 2
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 2
- 241000195493 Cryptophyta Species 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000012851 eutrophication Methods 0.000 description 1
- 229910052588 hydroxylapatite Inorganic materials 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
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Abstract
本发明公开一种利用磷矿尾矿制作磷吸附材料的制备方法，其特征在于按以下步骤进行：(1)、将所需含硅原料、含钙原料先进行破碎、粉碎、筛分处理，筛分后制得粒径在200目～600目的粉末原料；(2)、将步骤(1)中含硅原料、含钙原料按照一定比例混合，添加定的改性剂，用水调制成改性料浆；(3)、将步骤(2)中的改性料浆放于反应槽中，反应槽置入密闭的容器中，向容器中通入蒸汽，控制压力于0.2～1.6MPa，控制温度于120～200℃，控制反应时间于2～16h，制得多孔结构复合的磷吸附材料。本发明的磷吸附材料发泡制作而成，具备高比表面积、高孔隙率，应用于污水处理领域，尤其是含磷废水吸附磷；且去除率不受含磷废水pH值的限制。
Description
技术领域
本发明涉及一种利用磷矿尾矿制作磷吸附材料的制备方法，此吸附材料用于含磷废水的处理，属环保领域废水处理板块。
背景技术
磷矿资源在自然界储量极其有限，据估算，地球上的磷矿大概仅够人类使用200年左右。磷是地球一切生命体的重要营养元素，没有磷，地球上就不可能有生命。磷矿的形成需要1000万年以上的时间，但若按照中国目前的开采速度，最多只能开采几十年。
磷资源的有限性对人类而言是一场巨大的危机。与此同时，人类还面对着另一场磷污染危机：废水中磷污染会加速藻类生长，消耗水中溶解氧，造成水体富营养化，造成水资源的严重污染。最新数据显示，我国超过一半的河流湖泊和水库富营养化。
传统石灰法除磷，pH值是影响除磷效果大的因素，随着pH值的升高，羟基磷灰石的溶解度急剧下降，即磷的去除率迅速增加，pH值大于9.5后，水中所有磷酸盐都转为不溶性的沉淀。一般控制pH值在9.5～10之间，除磷效果最好。废水中金属离子对石灰用量影响较大，对于不同废水的石灰投加量不一。如欲使处理水中磷的含量在1mg/L以下时，对二级处理水，pH值应在9.5以上，对原废水则应在11以上。
石灰法处理磷废水存在的弊端：石灰用于前置除磷后污水pH值较高，进生物处理系统前需调节pH值；石灰用于后置除磷时，处理后的出水必须调节pH值才能满足排放要求。
发明内容
本发明的目的为了克服上述现有石灰法处理磷废水技术存在的弊端，提供一种利用磷矿尾矿制作磷吸附材料的制备方法，利用磷矿尾矿制作磷吸附材料用于处理磷废水，将改性复合吸附剂按照设定的投加量，添加至低浓度含磷废水中，对水中的磷和重金属离子进行吸附去除。
本发明采用了如下技术方案：
一种利用磷矿尾矿制作磷吸附材料的制备方法，其特征在于按以下步骤进行：
(1)、将所需含硅原料、含钙原料先进行破碎、粉碎、筛分处理，筛分后制得粒径在200目～600目的粉末原料；
(2)、将步骤(1)中含硅原料、含钙原料按照一定比例混合，再添加一定的改性剂，用水调制成改性料浆；
(3)、将步骤(2)中的改性料浆放于反应槽中，反应槽置入密闭的容器中，向容器中通入蒸汽，控制压力于0.2～1.6MPa，控制温度于120～200℃，控制反应时间于2～16h，制得多孔结构复合的磷吸附材料。
步骤(1)所述的含硅原料为硅藻土、粉煤灰、钢渣的一种或两种以上组成。
步骤(1)所述的含钙原料为生石灰、熟石灰、石灰石、石膏、磷石膏或黄磷渣中的一种或两种以上组成。
步骤(2)所述的改性剂为十二烷基苯磺酸钠、铝粉、碳酸钠、碳酸氢钠、松香热聚物、聚乙二醇中的一种或者两种以上组成。
步骤(2)所述的含硅原料、含钙原料、改性剂的质量份数为：含硅原料20-70，含钙原料20-70，改性剂0.5-10。
将制得多孔结构复合的磷吸附材料用于含磷废水的处理。
与现有技术相比，本发明制备的磷吸附材料具备以下优点：该磷吸附材料发泡制作而成，具备高比表面积、高孔隙率，应用于污水处理领域，尤其是含磷废水吸附磷；且去除率不受含磷废水pH值的限制。
具体实施方式
结合实施例对本发明作进一步描述。
实施例1
一种利用磷矿尾矿制作磷吸附材料的制备方法，按以下步骤进行：
(1)将硅藻土、黄磷渣先进行粉碎、筛分处理，制得硅藻土325目、黄磷渣200目；
(2)将40份硅藻土、50份黄磷渣、添加10份碳酸钠，充分混合，用水调制成改性料浆；
(3)将步骤(2)中的改性料浆放于反应槽中，反应槽置入密闭的容器中，向容器中通入蒸汽，控制压力于1.5MPa，控制温度于198℃，控制反应时间于3h，制得一种多孔结构复合的磷吸附材料。
将制得的磷吸附材料，进行破碎成5mm小块，将100g磷吸附材料放入1L配制20mg/L含磷废水中，充分搅拌1h后，检测废水中磷浓度为3.88mg/L。折算此磷吸附材料的磷吸附量为161.2g/t。
实施例2
一种利用磷矿尾矿制作磷吸附材料的制备方法，按以下步骤进行：
(1)将硅藻土、熟石灰、磷石膏先进行粉碎、筛分处理，制得硅藻土325目、熟石灰600目、磷石膏200目；
(2)将25份硅藻土、40份熟石灰、30份磷石膏，添加5份聚乙二醇，充分混合，用水调制成改性料浆；
(3)将步骤(2)中的改性料浆放于反应槽中，反应槽置入密闭的容器中，向容器中通入蒸汽，控制压力于0.2MPa，控制温度于120℃，控制反应时间于16h，制得一种多孔结构复合的磷吸附材料。
将制得的磷吸附材料，进行破碎成5mm小块，将100g磷吸附材料放入1L配制20mg/L含磷废水中，充分搅拌1h后，检测废水中磷浓度为5.69mg/L。折算此磷吸附材料的磷吸附量为143.1g/t。
实施例3
一种利用磷矿尾矿制作磷吸附材料的制备方法，按以下步骤进行：
(1)将粉煤灰、石膏、黄磷渣先进行粉碎、筛分处理，制得粉煤灰400目、石膏600目、黄磷渣300目；
(2)将50粉煤灰、20份石膏、28份黄磷渣,添加2份铝粉，充分混合，用水调制成改性料浆
(3)将步骤(2)中的改性料浆放于反应槽中，反应槽置入密闭的容器中，向容器中通入蒸汽，控制压力于1.0MPa，控制温度于180℃，控制反应时间于10h，制得一种多孔结构复合的磷吸附材料。
将制得的磷吸附材料，进行破碎成5mm小块，将100g磷吸附材料放入1L配制20mg/L含磷废水中，充分搅拌1h后，检测废水中磷浓度为4.23mg/L。折算此磷吸附材料的磷吸附量为157.7g/t。
实施例4
一种利用磷矿尾矿制作磷吸附材料的制备方法，按以下步骤进行：
(1)将粉煤灰、钢渣、熟石灰、磷石膏先进行粉碎、筛分处理，制得粉煤灰300目、钢渣300目、熟石灰600目、磷石膏200目；
(2)将10份粉煤灰、10份钢渣、40份熟石灰、30份磷石膏，添加10份碳酸氢钠，充分混合，用水调制成改性料浆；
(3)将步骤(2)中的改性料浆放于反应槽中，反应槽置入密闭的容器中，向容器中通入蒸汽，控制压力于0.2MPa，控制温度于120℃，控制反应时间于12h，制得一种多孔结构复合的磷吸附材料。
将制得的磷吸附材料，进行破碎成5mm小块，将100g磷吸附材料放入1L配制20mg/L含磷废水中，充分搅拌1h后，检测废水中磷浓度为6.22mg/L。折算此磷吸附材料的磷吸附量为137.8g/t。
实施例5
一种利用磷矿尾矿制作磷吸附材料的制备方法，按以下步骤进行：
(1)将粉煤灰、石膏先进行粉碎、筛分处理，制得粉煤灰400目、石膏600目；
(2)将70份粉煤灰、29.5份石膏,添加0.5份松香热聚物，充分混合，用水调制成改性料浆
(3)将步骤(2)中的改性料浆放于反应槽中，反应槽置入密闭的容器中，向容器中通入蒸汽，控制压力于1.6MPa，控制温度于200℃，控制反应时间于4h，制得一种多孔结构复合的磷吸附材料。
将制得的磷吸附材料，进行破碎成5mm小块，将100g磷吸附材料放入1L配制20mg/L含磷废水中，充分搅拌1h后，检测废水中磷浓度为2.99mg/L。折算此磷吸附材料的磷吸附量为170.1g/t。
实施例6
一种利用磷矿尾矿制作磷吸附材料的制备方法，按以下步骤进行：
(1)将硅藻土、粉煤灰、石膏、生石灰先进行粉碎、筛分处理，制得硅藻土400目、粉煤灰400目、石膏500目、生石灰500目；
(2)将40份硅藻土、30份粉煤灰、10份石膏、10份生石灰,添加10份十二烷基苯磺酸钠，充分混合，用水调制成改性料浆
(3)将步骤(2)中的改性料浆放于反应槽中，反应槽置入密闭的容器中，向容器中通入蒸汽，控制压力于0.8MPa，控制温度于170℃，控制反应时间于10h，制得一种多孔结构复合的磷吸附材料。
将制得的磷吸附材料，进行破碎成5mm小块，将100g磷吸附材料放入1L配制20mg/L含磷废水中，充分搅拌1h后，检测废水中磷浓度为5.07mg/L。折算此磷吸附材料的磷吸附量为149.3g/t。
Claims (6)
1.一种利用磷矿尾矿制作磷吸附材料的制备方法，其特征在于按以下步骤进行：
(1)、将所需含硅原料、含钙原料先进行破碎、粉碎、筛分处理，筛分后制得粒径在200目～600目的粉末原料；
(2)、将步骤(1)中含硅原料、含钙原料按照一定比例混合，再添加一定的改性剂，用水调制成改性料浆；
(3)、将步骤(2)中的改性料浆放于反应槽中，反应槽置入密闭的容器中，向容器中通入蒸汽，控制压力于0.2～1.6MPa，控制温度于120～200℃，控制反应时间于2～16h，制得多孔结构复合的磷吸附材料。
2.如权利要求1所述的利用磷矿尾矿制作磷吸附材料的制备方法，其特征在于：步骤(1)所述的含硅原料为硅藻土、粉煤灰、钢渣或的一种或两种以上组成。
3.如权利要求1所述的利用磷矿尾矿制作磷吸附材料的制备方法，其特征在于：步骤(1)所述的含钙原料为生石灰、熟石灰、石灰石、石膏、磷石膏或黄磷渣中的一种或两种以上组成。
4.如权利要求1所述的利用磷矿尾矿制作磷吸附材料的制备方法，其特征在于：步骤(2)所述的改性剂为十二烷基苯磺酸钠、铝粉、碳酸钠、碳酸氢钠、松香热聚物、聚乙二醇中的一种或者两种以上组成。
5.如权利要求1所述的利用磷矿尾矿制作磷吸附材料的制备方法，其特征在于：步骤(2)所述的含硅原料、含钙原料、改性剂的质量份数为：含硅原料20-70，含钙原料20-70，改性剂0.5-10。
6.如权利要求1-5之一所述的利用磷矿尾矿制作磷吸附材料的制备方法，其特征在于：将制得多孔结构复合的磷吸附材料用于含磷废水的处理。
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| CN114602421A (zh) * | 2022-03-01 | 2022-06-10 | 湖北富邦科技股份有限公司 | 一种制备低磷多孔结构材料的方法 |
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| CN101973599A (zh) * | 2010-10-25 | 2011-02-16 | 武汉理工大学 | 一种利用钢铁工业废渣吸附水中磷污染物的方法 |
| JP2018126683A (ja) * | 2017-02-08 | 2018-08-16 | 国立大学法人鳥取大学 | リン吸着材及びその製造方法 |
| CN114602421A (zh) * | 2022-03-01 | 2022-06-10 | 湖北富邦科技股份有限公司 | 一种制备低磷多孔结构材料的方法 |
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| CN117427618B (zh) * | 2023-12-20 | 2024-03-05 | 中国农业大学 | 壳聚糖改性黄磷渣-膨润土复合材料及其制备方法和应用 |
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