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WO2024187607A1 - Procédé de préparation d'un matériau adsorbant le phosphore au moyen de résidus de roche phosphatée - Google Patents

Procédé de préparation d'un matériau adsorbant le phosphore au moyen de résidus de roche phosphatée Download PDF

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Publication number
WO2024187607A1
WO2024187607A1 PCT/CN2023/099580 CN2023099580W WO2024187607A1 WO 2024187607 A1 WO2024187607 A1 WO 2024187607A1 CN 2023099580 W CN2023099580 W CN 2023099580W WO 2024187607 A1 WO2024187607 A1 WO 2024187607A1
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phosphorus
containing raw
raw material
preparing
phosphorus adsorption
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English (en)
Chinese (zh)
Inventor
李江鹏
王仁宗
王钊
晏进军
龚江龙
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Hubei Forbon Technology Co Ltd
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Hubei Forbon Technology Co Ltd
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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
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/14—Diatomaceous earth
    • 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
    • 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
    • B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
    • 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
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
    • 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
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • 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
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
    • 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
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/26—Synthetic macromolecular compounds
    • B01J20/262—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon to carbon unsaturated bonds, e.g. obtained by polycondensation
    • 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
    • B01J20/28002—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 physical properties
    • B01J20/28004—Sorbent size or size distribution, e.g. particle size
    • 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
    • B01J20/28042—Shaped bodies; Monolithic structures
    • B01J20/28045—Honeycomb or cellular structures; Solid foams or sponges
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/105—Phosphorus compounds
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/91—Use of waste materials as fillers for mortars or concrete

Definitions

  • the invention relates to a preparation method of a phosphorus adsorption material using phosphate ore tailings.
  • the adsorption material is used for treating phosphorus-containing wastewater and belongs to the wastewater treatment sector in the environmental protection field.
  • Phosphate resources are extremely limited in nature. It is estimated that there is only enough phosphate on Earth for human use for about 200 years. Phosphorus is an important nutrient element for all life on Earth. Without phosphorus, there would be no life on Earth. The formation of phosphate requires more than 10 million years, but at the current mining rate in China, it can only be mined for a few decades at most.
  • pH value is the factor that has the greatest impact on phosphorus removal effect. As the pH value increases, the solubility of hydroxyapatite drops sharply, that is, the phosphorus removal rate increases rapidly. When the pH value is greater than 9.5, all phosphates in the water are converted into insoluble precipitates. Generally, the pH value is controlled between 9.5 and 10, and the phosphorus removal effect is best. Metal ions in wastewater have a great influence on the amount of lime used, and the amount of lime added for different wastewaters is different. If you want to keep the phosphorus content in the treated water below 1 mg/L, the pH value should be above 9.5 for secondary treated water and above 11 for raw wastewater.
  • the purpose of the present invention is to overcome the drawbacks of the above-mentioned existing lime method for treating phosphorus wastewater, and provide a preparation method for phosphorus adsorption material using phosphate ore tailings, and use phosphate ore tailings to make phosphorus adsorption material for treating phosphorus wastewater, and add the modified composite adsorbent to low-concentration phosphorus-containing wastewater according to a set dosage to adsorb and remove phosphorus and heavy metal ions in the water.
  • a method for preparing a phosphorus adsorption material using phosphate ore tailings characterized by the following steps:
  • the required silicon-containing raw materials and calcium-containing raw materials are first crushed, pulverized and sieved to obtain powder raw materials with a particle size of 200 mesh to 600 mesh;
  • step (1) Mix the silicon-containing raw material and the calcium-containing raw material in step (1) in a certain proportion, and then add a certain modifier. Prepare modified slurry with water;
  • step (3) Place the modified slurry in step (2) in a reaction tank, place the reaction tank in a sealed container, introduce steam into the container, control the pressure at 0.2-1.6 MPa, control the temperature at 120-200° C., and control the reaction time at 2-16 h to obtain a porous structure composite phosphorus adsorption material.
  • the silicon-containing raw material in step (1) is composed of one or more of diatomaceous earth, fly ash and steel slag.
  • the calcium-containing raw material in step (1) is one or more of quicklime, slaked lime, limestone, gypsum, phosphogypsum or yellow phosphorus slag.
  • the modifier described in step (2) is one or more of sodium dodecylbenzene sulfonate, aluminum powder, sodium carbonate, sodium bicarbonate, rosin thermal polymer, and polyethylene glycol.
  • the mass fractions of the silicon-containing raw material, calcium-containing raw material and modifier in step (2) are: 20-70 for silicon-containing raw material, 20-70 for calcium-containing raw material and 0.5-10 for modifier.
  • the prepared porous structure composite phosphorus adsorption material is used for treating phosphorus-containing wastewater.
  • the phosphorus adsorption material prepared by the present invention has the following advantages: the phosphorus adsorption material is made by foaming, has a high specific surface area and high porosity, and is used in the field of sewage treatment, especially for the adsorption of phosphorus in phosphorus-containing wastewater; and the removal rate is not limited by the pH value of the phosphorus-containing wastewater.
  • a method for preparing a phosphorus adsorption material using phosphate ore tailings is carried out in the following steps:
  • diatomaceous earth and yellow phosphorus slag are first crushed and sieved to obtain 325 mesh diatomaceous earth and 200 mesh yellow phosphorus slag;
  • step (3) The modified slurry in step (2) is placed in a reaction tank, the reaction tank is placed in a sealed container, steam is introduced into the container, the pressure is controlled at 1.5 MPa, the temperature is controlled at 198° C., and the reaction time is controlled at 3 h to obtain a porous structure composite phosphorus adsorption material.
  • the prepared phosphorus adsorption material was broken into 5 mm small pieces, and 100 g of the phosphorus adsorption material was put into 1 L of 20 mg/L phosphorus-containing wastewater. After fully stirring for 1 hour, the phosphorus concentration in the wastewater was detected to be 3.88 mg/L. The phosphorus adsorption capacity of this phosphorus adsorption material was converted to 161.2 g/t.
  • a method for preparing a phosphorus adsorption material using phosphate ore tailings is carried out in the following steps:
  • diatomite, slaked lime and phosphogypsum are first crushed and sieved to obtain 325 mesh diatomite, 600 mesh slaked lime and 200 mesh phosphogypsum;
  • step (3) The modified slurry in step (2) is placed in a reaction tank, the reaction tank is placed in a sealed container, steam is introduced into the container, the pressure is controlled at 0.2 MPa, the temperature is controlled at 120° C., and the reaction time is controlled at 16 h to obtain a porous structure composite phosphorus adsorption material.
  • the prepared phosphorus adsorption material was broken into 5 mm small pieces, and 100 g of the phosphorus adsorption material was put into 1 L of 20 mg/L phosphorus-containing wastewater. After fully stirring for 1 hour, the phosphorus concentration in the wastewater was detected to be 5.69 mg/L. The phosphorus adsorption capacity of this phosphorus adsorption material was converted to 143.1 g/t.
  • a method for preparing a phosphorus adsorption material using phosphate ore tailings is carried out in the following steps:
  • fly ash, gypsum and yellow phosphorus slag are first crushed and sieved to obtain fly ash of 400 mesh, gypsum of 600 mesh and yellow phosphorus slag of 300 mesh;
  • step (3) The modified slurry in step (2) is placed in a reaction tank, the reaction tank is placed in a sealed container, steam is introduced into the container, the pressure is controlled at 1.0 MPa, the temperature is controlled at 180° C., and the reaction time is controlled at 10 h to obtain a porous structure composite phosphorus adsorption material.
  • the prepared phosphorus adsorption material was broken into 5 mm small pieces, and 100 g of the phosphorus adsorption material was put into 1 L of 20 mg/L phosphorus-containing wastewater. After fully stirring for 1 hour, the phosphorus concentration in the wastewater was detected to be 4.23 mg/L. The phosphorus adsorption capacity of this phosphorus adsorption material was converted to 157.7 g/t.
  • a method for preparing a phosphorus adsorption material using phosphate ore tailings is carried out in the following steps:
  • fly ash, steel slag, slaked lime and phosphogypsum are first crushed and sieved to obtain fly ash of 300 mesh, steel slag of 300 mesh, slaked lime of 600 mesh and phosphogypsum of 200 mesh;
  • step (3) placing the modified slurry in step (2) in a reaction tank, placing the reaction tank in a sealed container, introducing steam into the container, controlling the pressure at 0.2 MPa, the temperature at 120° C., and the reaction time at 12 h to obtain a porous structure composite Phosphorus adsorbing materials.
  • the prepared phosphorus adsorption material was broken into 5 mm small pieces, and 100 g of the phosphorus adsorption material was put into 1 L of 20 mg/L phosphorus-containing wastewater. After fully stirring for 1 hour, the phosphorus concentration in the wastewater was detected to be 6.22 mg/L. The phosphorus adsorption capacity of this phosphorus adsorption material was converted to 137.8 g/t.
  • a method for preparing a phosphorus adsorption material using phosphate ore tailings is carried out in the following steps:
  • fly ash and gypsum are first crushed and sieved to obtain fly ash of 400 mesh and gypsum of 600 mesh;
  • step (3) The modified slurry in step (2) is placed in a reaction tank, the reaction tank is placed in a sealed container, steam is introduced into the container, the pressure is controlled at 1.6 MPa, the temperature is controlled at 200° C., and the reaction time is controlled at 4 h to obtain a porous structure composite phosphorus adsorption material.
  • the prepared phosphorus adsorption material was broken into 5 mm small pieces, and 100 g of the phosphorus adsorption material was put into 1 L of 20 mg/L phosphorus-containing wastewater. After fully stirring for 1 hour, the phosphorus concentration in the wastewater was detected to be 2.99 mg/L. The phosphorus adsorption capacity of this phosphorus adsorption material was converted to 170.1 g/t.
  • a method for preparing a phosphorus adsorption material using phosphate ore tailings is carried out in the following steps:
  • diatomaceous earth, fly ash, gypsum and quicklime are first crushed and sieved to obtain 400 mesh diatomaceous earth, 400 mesh fly ash, 500 mesh gypsum and 500 mesh quicklime;
  • step (3) The modified slurry in step (2) is placed in a reaction tank, the reaction tank is placed in a sealed container, steam is introduced into the container, the pressure is controlled at 0.8 MPa, the temperature is controlled at 170° C., and the reaction time is controlled at 10 h to obtain a porous structure composite phosphorus adsorption material.
  • the prepared phosphorus adsorption material was broken into 5 mm small pieces, and 100 g of the phosphorus adsorption material was put into 1 L of 20 mg/L phosphorus-containing wastewater. After fully stirring for 1 hour, the phosphorus concentration in the wastewater was detected to be 5.07 mg/L. The phosphorus adsorption capacity of this phosphorus adsorption material was converted to 149.3 g/t.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Analytical Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Water Supply & Treatment (AREA)
  • Environmental & Geological Engineering (AREA)
  • Engineering & Computer Science (AREA)
  • Hydrology & Water Resources (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Water Treatment By Sorption (AREA)

Abstract

Est divulgué dans la présente invention un procédé de préparation d'un matériau adsorbant le phosphore au moyen de résidus de roche phosphatée. Le procédé est caractérisé en ce qu'il est mis en œuvre selon les étapes suivantes : (1) concassage, écrasement et tamisage d'une matière première contenant du silicium et d'une matière première contenant du calcium requises pour obtenir des matières premières en poudre présentant une granularité de 200 à 600 mailles ; (2) mélange de la matière première contenant du silicium et de la matière première contenant du calcium dans l'étape (1) selon une certaine proportion, ajout d'un certain modificateur, et mélange de celles-ci avec de l'eau pour obtenir une suspension modifiée ; et (3) placement de la suspension modifiée dans l'étape (2) dans un réservoir de réaction, placement du réservoir de réaction dans un contenant fermé, introduction de la vapeur dans le contenant, contrôle de la pression à 0,2-1,6 MPa, contrôle de la température à 120-200°C, et contrôle du temps de réaction à 2-16 heures, ce qui permet d'obtenir un matériau adsorbant le phosphore composite à structure poreuse. Le matériau adsorbant le phosphore de la présente invention est préparé par moussage, présente une surface spécifique élevée et une porosité élevée, et est appliqué au champ de traitement des eaux usées, en particulier à l'adsorption de phosphore d'eaux usées contenant du phosphore ; et le taux d'élimination n'est pas limité par la valeur de pH des eaux usées contenant du phosphore.
PCT/CN2023/099580 2023-03-15 2023-06-12 Procédé de préparation d'un matériau adsorbant le phosphore au moyen de résidus de roche phosphatée Pending WO2024187607A1 (fr)

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CN202310251954.9 2023-03-15
CN202310251954.9A CN116116378A (zh) 2023-03-15 2023-03-15 一种利用磷矿尾矿制作磷吸附材料的制备方法

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Cited By (1)

* Cited by examiner, † Cited by third party
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CN119349988A (zh) * 2024-10-29 2025-01-24 武汉科技大学 一种高掺量磷石膏基超绝热多孔耐高温材料及其制备方法

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CN116116378A (zh) * 2023-03-15 2023-05-16 湖北富邦科技股份有限公司 一种利用磷矿尾矿制作磷吸附材料的制备方法
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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JP2010234280A (ja) * 2009-03-31 2010-10-21 Hokuriku Electric Power Co Inc:The リン吸着材およびこれを用いた肥料の製造方法
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
JP2013202463A (ja) * 2012-03-27 2013-10-07 Hokuriku Electric Power Co Inc:The リン回収材、リン回収方法及び肥料の製造方法
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CN116116378A (zh) * 2023-03-15 2023-05-16 湖北富邦科技股份有限公司 一种利用磷矿尾矿制作磷吸附材料的制备方法

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN119349988A (zh) * 2024-10-29 2025-01-24 武汉科技大学 一种高掺量磷石膏基超绝热多孔耐高温材料及其制备方法

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