CN111346601A - Ceramsite for adsorbing perfluorinated compounds in water and preparation method thereof - Google Patents

Ceramsite for adsorbing perfluorinated compounds in water and preparation method thereof Download PDF

Info

Publication number
CN111346601A
CN111346601A CN202010171897.XA CN202010171897A CN111346601A CN 111346601 A CN111346601 A CN 111346601A CN 202010171897 A CN202010171897 A CN 202010171897A CN 111346601 A CN111346601 A CN 111346601A
Authority
CN
China
Prior art keywords
ceramsite
perfluorinated compounds
water body
adsorbing
water
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202010171897.XA
Other languages
Chinese (zh)
Other versions
CN111346601B (en
Inventor
马小东
许卓奇
王淑荣
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nankai University
Hebei University of Technology
Original Assignee
Nankai University
Hebei University of Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Nankai University, Hebei University of Technology filed Critical Nankai University
Priority to CN202010171897.XA priority Critical patent/CN111346601B/en
Publication of CN111346601A publication Critical patent/CN111346601A/en
Application granted granted Critical
Publication of CN111346601B publication Critical patent/CN111346601B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/04Solid 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
    • B01J20/041Oxides or hydroxides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/103Solid 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/12Naturally occurring clays or bleaching earth
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/16Alumino-silicates
    • B01J20/165Natural alumino-silicates, e.g. zeolites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014Solid 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
    • B01J20/28016Particle form
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30Processes for preparing, regenerating, or reactivating
    • B01J20/3028Granulating, agglomerating or aggregating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30Processes for preparing, regenerating, or reactivating
    • B01J20/305Addition of material, later completely removed, e.g. as result of heat treatment, leaching or washing, e.g. for forming pores
    • B01J20/3064Addition of pore forming agents, e.g. pore inducing or porogenic agents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/288Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/36Organic compounds containing halogen

Landscapes

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

Abstract

The invention discloses a ceramsite for adsorbing perfluorinated compounds in a water body and a preparation method thereof, wherein the ceramsite comprises the following raw materials in parts by mass: 40-80% of iron-containing solid waste, 5-20% of clay, 5-40% of straw and 3-15% of pore-forming agent; the iron-containing solid waste comprises the following components: SiO 22:40‑55%;Fe2O3:5‑15%;TiO2:1 to 10 percent; MgO: 10 to 15 percent; organic matter: 1-5%, others: 5 to 15 percent. The raw materials are evenly mixed according to the proportion, then are granulated into balls, and are roasted under high temperature and without oxygen to obtain the ceramsite capable of adsorbing the perfluorinated compounds in the water body. The ceramsite prepared by the method has the advantages of simple and convenient preparation process, low cost, high adsorption efficiency on perfluorinated compounds in water and the like.

Description

Ceramsite for adsorbing perfluorinated compounds in water and preparation method thereof
The technical field is as follows:
the invention relates to the field of water pollution control, in particular to ceramsite for adsorbing perfluorinated compounds in a water body and a preparation method thereof.
Background art:
perfluoro compounds (PFCs) mainly include perfluorocarboxylic acids (PFCAs), perfluorosulfonic acid salts (PFSAs), Fluorotelomer alcohols (FTOHs), and the like. With the research, development, production, use and disposal of PFCs commodities, PFCs can enter the water environment through various ways, and threatens the safety of a water ecosystem and the human health. In view of the persistence and bioaccumulation of PFCs, pollution control of PFCs in water has become a research hotspot in the field of environmental engineering. The F atom in PFCs has strong electronegativity, and the C-F bond in PFCs has large bond energy, so the PFCs have stable properties and are difficult to degrade by the traditional chemical and biological methods. The adsorption method is an important method for removing perfluorinated compounds in water, and at present, PFCs adsorbents in water are mainly removed: inorganic minerals, iron oxides, activated carbon adsorbents, and the like. At present, the problem of high cost of the adsorbent generally exists in the adsorbent for adsorbing PFCs in a water body.
The retrieval shows that Chinese patent application No. CN201510894494.7 discloses a material for selectively adsorbing PFCs and a preparation method thereof, the material is fluorinated montmorillonite, the preparation process is complex, and the adsorption effect on PFCs is only about 60%. Chinese patent application No. CN201410639721.7 discloses a magnetic nano iron oxide composite material for adsorbing PFCs and a preparation method thereof, which has a good adsorption effect on PFCs, but has a high cost. Valeria et al use granular activated carbon to adsorb PFCs in water, and the adsorption efficiency can reach 80%, but the cost for preparing activated carbon is high. In recent years, no report on the preparation of the PFCs adsorbent in purified water by using solid waste as a main raw material has been found in research on PFCs adsorbents in water.
The invention content is as follows:
aiming at the problem of higher cost of the existing adsorbent for adsorbing perfluorinated compounds in water, the invention provides a preparation method and application of ceramsite for adsorbing perfluorinated compounds in water. The ceramsite prepared by the method has the advantages of low cost of raw materials, simple and convenient preparation process and higher adsorption efficiency on perfluorinated compounds in water.
The technical scheme adopted by the invention is as follows:
the ceramsite for adsorbing the perfluorinated compounds in the water body is provided, and the ceramsite comprises the following raw materials in parts by mass: 40-80% of iron-containing solid waste, 5-20% of clay, 5-40% of straw and 3-15% of pore-forming agent; the iron-containing solid waste comprises the following components (by mass fraction): SiO 22:40-55%;Fe2O3:5-15%;TiO2:1 to 10 percent; MgO: 10 to 15 percent; organic matter: 1-5%, others: 5 to 15 percent; the raw materials are roasted under the high-temperature oxygen-free condition to prepare the ceramsite.
Preferably, the ceramsite comprises the following raw materials in parts by mass: 50-70% of iron-containing solid waste, 10-15% of clay, 10-30% of straw and 5-10% of pore-forming agent.
The phase structures contained in the ceramsite comprise: illite, hematite, mica, quartz, calcite, orthoclase; possible phases include: amphibole, leek, hempseite, albite, diopside, actinolite, anatase.
The preparation method of the ceramsite comprises the steps of taking the iron-containing solid waste, the clay and the straws as raw materials, uniformly mixing the raw materials according to a proportion, granulating into balls, roasting at high temperature in an oxygen-free mode, and cooling to obtain the ceramsite capable of adsorbing the perfluorinated compounds in the water body.
The method comprises the following specific steps:
1) and (3) granulation: grinding the raw materials, sieving the ground raw materials by a sieve with 100-plus-300 meshes, uniformly mixing the ground raw materials according to the proportion, putting the mixture into a granulator to form balls, and spraying deionized water according to the solid-to-liquid ratio of 5:1-15:1 in the process of forming the balls to prepare the material balls with the particle size of 1-3 cm;
2) and (3) drying: putting the pellets prepared in the step 1) into an oven, and drying for 8-12 h at 50-80 ℃;
3) roasting: placing the dried pellets in a box-type resistance furnace, heating to 400-1300 ℃ for presintering for 20-40min by a program under the protection of nitrogen atmosphere, and then heating to 1000-1300 ℃ for roasting for 20-40 min;
4) and (3) cooling: after the baking and sintering, cooling for 6-12h to obtain the ceramsite for adsorbing the perfluorinated compounds in the water body.
The invention also provides an application of the ceramsite for adsorbing the perfluorinated compounds in the water body, which is characterized in that: treating the polluted water body by using the ceramsite for adsorbing the perfluorinated compounds in the water body, wherein the concentration of the perfluorinated compounds in the polluted water body is 0.5-10mg/L, the using amount of the polluted water body is 30-100mL, the using amount of the ceramsite is 1-3g, the adsorption time is 12-48h, and the stirring speed is 100 plus materials and 1000 rpm; the perfluorinated compounds contained in the polluted water body are: perfluorocarboxylic acids or perfluorosulphonates or telomeric alcohols. After stirring, centrifuging for 5-10min at 1500-; and taking 5-20mL of filtered water sample, and taking 1.5mL of the filtered water sample from the water sample, and determining the concentration of the perfluorinated compounds in the water body after adsorption by using a liquid chromatography-mass spectrometer.
Compared with the prior art, the invention has the beneficial effects that:
the ceramsite disclosed by the invention takes the iron-containing solid waste, the clay, the straws and the pore-making agent with specific component contents as raw materials, the added straws can generate carbon components through anaerobic heat treatment, and the carbon components and the inorganic minerals form a synergistic effect, so that the ceramsite has a higher adsorption effect on perfluorinated compounds in a water body. The ceramsite prepared by the method disclosed by the invention is high in mechanical strength and good in stability.
The ceramsite adsorbing the perfluorinated compounds in the water body, which is obtained by the preparation method, is prepared by high-temperature oxygen-free calcination, and all the ceramsite comprises carbonaceous components and phases such as illite, hematite, mica, quartz, calcite, orthoclase and the like. The carbonaceous component and the phase composition are combined with the magnesium amphibole, or leek amphibole, or hemlock, or albite, or diopside, or actinolite, or anatase and other phases, so that the ceramsite has good adsorption performance on the perfluorinated compounds in the water body.
The ceramsite prepared by the method has the advantages of low cost of raw materials, simple and convenient preparation process and high adsorption efficiency of perfluorinated compounds in water, and can reach 80-95% of perfluorinated compound removal efficiency under the adsorption conditions given by the application.
Description of the drawings:
FIG. 1 is an XRD analysis diagram of the ceramsite in examples 1, 2, 3, 6 and 7.
FIG. 2 is an XRD analysis pattern of the ceramsite described in example 4.
FIG. 3 is an XRD analysis of the ceramsite sample according to example 5.
The specific implementation mode is as follows:
in order to better understand the contents of the present invention, the following examples are further provided to illustrate the present invention, but the scope of the present invention is not limited by the examples.
The invention relates to a preparation method of ceramsite for adsorbing perfluorinated compounds in water, which takes iron-containing solid wastes, clay, straws and pore-making agents as raw materials and prepares the ceramsite for adsorbing the perfluorinated compounds in the water through the steps of granulation, drying, anaerobic roasting, cooling and the like. The phases contained in the different ceramsite obtained in the following examples are: illite, hematite, mica, quartz, calcite and orthoclase.
The pore-forming agent comprises limestone, perlite tailings and the like. The straw is roasted and decomposed in an oxygen-free environment to generate carbon components, so that the adsorption effect on the perfluorinated compounds is improved. The clay has the following functions: the mechanical strength of the ceramsite is improved, and the ceramsite is easier to form. In the following embodiments, the straws are corn straws, and the pore-forming agent is perlite tailings, and the types of the straws in the formula of the invention are not limited to the corn straws, and can also be biomass straws such as cotton straws, wheat straws and the like.
Example 1:
(1) a preparation method of ceramsite for adsorbing perfluorinated compounds in water. The method comprises the following specific steps:
1) the raw material ratio is as follows: 50% of iron-containing solid waste, 15% of clay, 30% of straw and 5% of pore-forming agent. The iron-containing solid waste comprises the following components (by mass fraction): SiO 22:40-55%;Fe2O3:5-15%;TiO2:1 to 10 percent; MgO: 10 to 15 percent; organic matter: 1-5%, others: 5 to 15 percent;
2) and (3) granulation: grinding the raw materials respectively, sieving with a 120-mesh sieve, mixing uniformly according to a proportion, placing in a granulator to form balls, and spraying deionized water according to a solid-to-liquid ratio of 10:1 in the process of forming balls to prepare material balls with the particle size of 1 cm;
3) and (3) drying: putting the material balls prepared in the step 2) into an oven to dry for 10 hours at 70 ℃;
4) roasting: placing the dried pellets in a box-type resistance furnace, heating to 500 ℃ by a program under the protection of nitrogen atmosphere, pre-burning for 30min, and then heating to 1200 ℃ and roasting for 30 min;
5) and (3) cooling: after the baking and sintering, cooling for 12h to obtain the ceramsite for adsorbing the perfluorinated compounds in the water body.
After XRD analysis, the prepared ceramsite has illite, hematite, mica, quartz, calcite, orthoclase and amphibole.
(2) Experiment for removing perfluorinated compounds in water by adsorption
The adsorption process is carried out in a 50mL beaker, the prepared ceramsite is ground and sieved by a 120-mesh sieve, then 2g of the ground ceramsite is accurately weighed and placed in the beaker, finally 100mL of 1mg/L perfluorooctane carboxylic acid aqueous solution is added into the beaker, and the adsorption temperature is controlled at 25 ℃. Placing the beaker in a constant-temperature magnetic stirrer, controlling the rotating speed to be 300rpm, stirring for 24 hours, then sampling, filtering the solution through a 0.22 mu m water phase filter head, and analyzing the concentration of the residual perfluorooctane carboxylic acid in the water by utilizing high performance liquid chromatography-mass spectrometry.
As a result of the adsorption, the removal efficiency of perfluorooctane carboxylic acid from water was 94.2%.
Example 2:
(1) a preparation method of ceramsite for adsorbing perfluorinated compounds in water. The method comprises the following specific steps:
1) the raw material ratio is as follows: 50% of iron-containing solid waste, 15% of clay, 30% of straw and 5% of pore-forming agent. The iron-containing solid waste comprises the following components (by mass fraction): SiO 22:40-55%;Fe2O3:5-15%;TiO2:1 to 10 percent; MgO: 10 to 15 percent; organic matter: 1-5%, others: 5 to 15 percent;
2) and (3) granulation: grinding the raw materials respectively, sieving with a 120-mesh sieve, mixing uniformly according to a proportion, placing in a granulator to form balls, and spraying deionized water according to a solid-to-liquid ratio of 10:1 in the process of forming balls to prepare material balls with the particle size of 1 cm;
3) and (3) drying: putting the material balls prepared in the step 2) into an oven to dry for 10 hours at 70 ℃;
4) roasting: placing the dried pellets in a box-type resistance furnace, heating to 500 ℃ by a program under the protection of nitrogen atmosphere, pre-burning for 30min, and then heating to 1200 ℃ and roasting for 30 min;
5) and (3) cooling: after the baking and sintering, cooling for 12h to obtain the ceramsite for adsorbing the perfluorinated compounds in the water body.
(2) Experiment for removing perfluorinated compounds in water by adsorption
The adsorption process is carried out in a 50mL beaker, the prepared ceramsite is ground and sieved by a 120-mesh sieve, then 2g of the ground ceramsite is accurately weighed and placed in the beaker, finally 100mL of 1mg/L potassium perfluorooctane sulfonate aqueous solution is added into the beaker, and the adsorption temperature is controlled at 25 ℃. Placing the beaker in a constant-temperature magnetic stirrer, controlling the rotating speed to be 300rpm, stirring for 24 hours, then sampling, filtering the solution through a 0.22 mu m water phase filter head, and analyzing the concentration of the residual potassium perfluorooctyl sulfonate in the water by utilizing high performance liquid chromatography-mass spectrometry.
As a result of adsorption, the removal efficiency of potassium perfluorooctyl sulfonate in water was 91.3%.
Example 3:
(1) a preparation method of ceramsite for adsorbing perfluorinated compounds in water. The method comprises the following specific steps:
1) the raw material ratio is as follows: 50% of iron-containing solid waste, 15% of clay, 30% of straw and 5% of pore-forming agent. The iron-containing solid waste comprises the following components (by mass fraction): SiO 22:40-55%;Fe2O3:5-15%;TiO2:1 to 10 percent; MgO: 10 to 15 percent; organic matter: 1-5%, others: 5 to 15 percent;
2) and (3) granulation: grinding the raw materials respectively, sieving with a 120-mesh sieve, mixing uniformly according to a proportion, placing in a granulator to form balls, and spraying deionized water according to a solid-to-liquid ratio of 10:1 in the process of forming balls to prepare material balls with the particle size of 1 cm;
3) and (3) drying: putting the material balls prepared in the step 2) into an oven to dry for 10 hours at 70 ℃;
4) roasting: placing the dried pellets in a box-type resistance furnace, heating to 500 ℃ by a program under the protection of nitrogen atmosphere, pre-burning for 30min, and then heating to 1200 ℃ and roasting for 30 min;
5) and (3) cooling: after the baking and sintering, cooling for 12h to obtain the ceramsite for adsorbing the perfluorinated compounds in the water body.
(2) Experiment for removing perfluorinated compounds in water by adsorption
The adsorption process is carried out in a 50mL beaker, the prepared ceramsite is firstly ground and sieved by a 120-mesh sieve, then 2g of the ground ceramsite is accurately weighed and placed in the beaker, finally 100mL of 1 mg/L6: 2 fluorotelomer alcohol aqueous solution is added into the beaker, and the adsorption temperature is controlled at 25 ℃. Placing the beaker in a constant-temperature magnetic stirrer, controlling the rotating speed to be 300rpm, stirring for 24 hours, then sampling, filtering the solution through a 0.22 mu m water phase filter head, and analyzing the concentration of the residual 6:2 fluorotelomeric alcohol in the water by utilizing high performance liquid chromatography-mass spectrometry.
As a result of the adsorption, the removal efficiency of 6:2 fluorotelomer alcohol in water was 90.7%.
Example 4:
(1) a preparation method of ceramsite for adsorbing perfluorinated compounds in water. The method comprises the following specific steps:
1) the raw material ratio is as follows: 70% of iron-containing solid waste, 15% of clay, 10% of straw and 5% of pore-forming agent. The iron-containing solid waste comprises the following components (by mass fraction): SiO 22:40-55%;Fe2O3:5-15%;TiO2:1 to 10 percent; MgO: 10 to 15 percent; organic matter: 1-5%, others: 5 to 15 percent;
2) and (3) granulation: grinding the raw materials, sieving with a 120-mesh sieve, mixing uniformly according to a proportion, placing in a granulator to form balls, and spraying deionized water according to a solid-liquid ratio of 10:1 in the process of forming balls to prepare material balls with the particle size of 1 cm;
3) and (3) drying: putting the material balls prepared in the step 2) into an oven to dry for 10 hours at 70 ℃;
4) roasting: placing the dried pellets in a box-type resistance furnace, heating to 500 ℃ by a program under the protection of nitrogen atmosphere, pre-burning for 30min, and then heating to 1200 ℃ and roasting for 30 min;
5) and (3) cooling: after the baking and sintering, cooling for 12h to obtain the ceramsite for adsorbing the perfluorinated compounds in the water body.
After XRD analysis, the prepared ceramsite has illite, hematite, mica, quartz, calcite, orthoclase, albite, leek amphibole and amphibole.
(2) Experiment for removing perfluorinated compounds in water by adsorption
The adsorption process is carried out in a 50mL beaker, the prepared ceramsite is ground and sieved by a 120-mesh sieve, then 2g of the ground ceramsite is accurately weighed and placed in the beaker, finally 100mL of 1mg/L perfluorooctane carboxylic acid aqueous solution is added into the beaker, and the adsorption temperature is controlled at 25 ℃. Placing the beaker in a constant-temperature magnetic stirrer, controlling the rotating speed to be 300rpm, stirring for 24 hours, then sampling, filtering the solution through a 0.22 mu m water phase filter head, and analyzing the concentration of the residual perfluorooctane carboxylic acid in the water by utilizing high performance liquid chromatography-mass spectrometry.
As a result of the adsorption, the removal efficiency of perfluorooctane carboxylic acid from water was 87.1%.
Example 5:
(1) a preparation method of ceramsite for adsorbing perfluorinated compounds in water. The method comprises the following specific steps:
1) the raw material ratio is as follows: 60% of iron-containing solid waste, 15% of clay, 20% of straw and 5% of pore-forming agent. The iron-containing solid waste comprises the following components (by mass fraction): SiO 22:40-55%;Fe2O3:5-15%;TiO2:1 to 10 percent; MgO: 10 to 15 percent; organic matter: 1-5%, others: 5 to 15 percent;
2) and (3) granulation: grinding the raw materials, sieving with a 120-mesh sieve, mixing uniformly according to a proportion, placing in a granulator to form balls, and spraying deionized water according to a solid-liquid ratio of 10:1 in the process of forming balls to prepare material balls with the particle size of 1 cm;
3) and (3) drying: putting the material balls prepared in the step 2) into an oven to dry for 10 hours at 70 ℃;
4) roasting: placing the dried pellets in a box-type resistance furnace, programming to 500 ℃ for presintering for 30min under the aerobic condition, and then heating to 1200 ℃ for roasting for 30 min;
5) and (3) cooling: after the baking and sintering, cooling for 12h to obtain the ceramsite for adsorbing the perfluorinated compounds in the water body.
After XRD analysis, illite, hematite, mica, quartz, calcite, orthoclase, amphibole, albite, diopside, actinolite and anatase are obtained.
(2) Experiment for removing perfluorinated compounds in water by adsorption
The adsorption process is carried out in a 50mL beaker, the prepared ceramsite is ground and sieved by a 120-mesh sieve, then 2g of the ground ceramsite is accurately weighed and placed in the beaker, finally 100mL of 1mg/L perfluorooctane carboxylic acid aqueous solution is added into the beaker, and the adsorption temperature is controlled at 25 ℃. Placing the beaker in a constant-temperature magnetic stirrer, controlling the rotating speed to be 300rpm, stirring for 24 hours, then sampling, filtering the solution through a 0.22 mu m water phase filter head, and analyzing the concentration of the residual perfluorooctane carboxylic acid in the water by utilizing high performance liquid chromatography-mass spectrometry.
As a result of the adsorption, the removal efficiency of perfluorooctane carboxylic acid from water was 84.2%.
Example 6:
(1) a preparation method of ceramsite for adsorbing perfluorinated compounds in water. The method comprises the following specific steps:
1) the raw material ratio is as follows: 50% of iron-containing solid waste, 15% of clay, 30% of straw and 5% of pore-forming agent. The iron-containing solid waste comprises the following components (by mass fraction): SiO 22:40-55%;Fe2O3:5-15%;TiO2:1 to 10 percent; MgO: 10 to 15 percent; organic matter: 1-5%, others: 5 to 15 percent;
2) and (3) granulation: grinding the raw materials, sieving with a 120-mesh sieve, mixing uniformly according to a proportion, placing in a granulator to form balls, and spraying deionized water according to a solid-liquid ratio of 10:1 in the process of forming balls to prepare material balls with the particle size of 1 cm;
3) and (3) drying: putting the material balls prepared in the step 2) into an oven to dry for 10 hours at 70 ℃;
4) roasting: placing the dried pellets in a box-type resistance furnace, heating to 500 ℃ by a program under the protection of nitrogen atmosphere, pre-burning for 30min, and then heating to 1200 ℃ and roasting for 30 min;
5) and (3) cooling: after the baking and sintering, cooling for 12h to obtain the ceramsite for adsorbing the perfluorinated compounds in the water body.
(2) Experiment for removing perfluorinated compounds in water by adsorption
The adsorption process is carried out in a 50mL beaker, the prepared ceramsite is ground and sieved by a 120-mesh sieve, then 2g of the ground ceramsite is accurately weighed and placed in the beaker, finally 100mL of 10mg/L perfluorooctane carboxylic acid aqueous solution is added into the beaker, and the adsorption temperature is controlled at 25 ℃. Placing the beaker in a constant-temperature magnetic stirrer, controlling the rotating speed to be 300rpm, stirring for 24 hours, then sampling, filtering the solution through a 0.22 mu m water phase filter head, and analyzing the concentration of the residual perfluorooctane carboxylic acid in the water by utilizing high performance liquid chromatography-mass spectrometry.
As a result of the adsorption, the removal efficiency of perfluorooctane carboxylic acid from water was 85.4%.
Example 7:
(1) a preparation method of ceramsite for adsorbing perfluorinated compounds in water. The method comprises the following specific steps:
1) the raw material ratio is as follows: 50% of iron-containing solid waste, 15% of clay, 30% of straw and 5% of pore-forming agent. The iron-containing solid waste comprises the following components (by mass fraction): SiO 22:40-55%;Fe2O3:5-15%;TiO2:1 to 10 percent; MgO: 10 to 15 percent; organic matter: 1-5%, others: 5 to 15 percent;
2) and (3) granulation: grinding the raw materials, sieving with a 120-mesh sieve, mixing uniformly according to a proportion, placing in a granulator to form balls, and spraying deionized water according to a solid-liquid ratio of 10:1 in the process of forming balls to prepare material balls with the particle size of 1 cm;
3) and (3) drying: putting the material balls prepared in the step 2) into an oven to dry for 10 hours at 70 ℃;
4) roasting: placing the dried pellets in a box-type resistance furnace, heating to 500 ℃ by a program under the protection of nitrogen atmosphere, pre-burning for 30min, and then heating to 1200 ℃ and roasting for 30 min;
5) and (3) cooling: after the baking and sintering, cooling for 12h to obtain the ceramsite for adsorbing the perfluorinated compounds in the water body.
(2) Experiment for removing perfluorinated compounds in water by adsorption
The adsorption process is carried out in a 50mL beaker, the prepared ceramsite is ground and sieved by a 120-mesh sieve, then 2g of the ground ceramsite is accurately weighed and placed in the beaker, finally 100mL of 1mg/L perfluorooctane carboxylic acid aqueous solution is added into the beaker, and the adsorption temperature is controlled at 25 ℃. Placing the beaker in a constant-temperature magnetic stirrer, controlling the rotating speed to be 300rpm, stirring for 12 hours, then sampling, filtering the solution through a 0.22 mu m water phase filter head, and analyzing the concentration of the residual perfluorooctane carboxylic acid in the water by utilizing high performance liquid chromatography-mass spectrometry.
As a result of the adsorption, the removal efficiency of perfluorooctane carboxylic acid from water was 82.1%.
Nothing in this specification is said to apply to the prior art.

Claims (9)

1. The ceramsite for adsorbing the perfluorinated compounds in the water body comprises the following raw materials in parts by mass: 40-80% of iron-containing solid waste, 5-20% of clay, 5-40% of straw and 3-15% of pore-forming agent; the iron-containing solid waste comprises the following components: SiO 22:40-55%;Fe2O3:5-15%;TiO2:1 to 10 percent; MgO: 10 to 15 percent; organic matter: 1-5%, others: 5 to 15 percent;
the raw materials are roasted under the high-temperature oxygen-free condition to prepare the ceramsite.
2. The ceramsite of claim 1, wherein the ceramsite comprises the following raw materials by mass: 50-70% of iron-containing solid waste, 5-10% of clay, 10-30% of straw and 5-10% of pore-forming agent.
3. The ceramsite according to claim 1, wherein the ceramsite comprises phases defined as: illite, hematite, mica, quartz, calcite, and orthoclase; possible phases include: amphibole, leek, hempseite, albite, diopside, actinolite, anatase.
4. The ceramsite according to any one of claims 1-3, wherein the pore-forming agent is limestone or perlite tailings.
5. A process for preparing haydite as claimed in any one of claims 1 to 4, which is prepared from iron-containing solid wastes, clay and straw through proportional mixing, granulating, high-temp oxygen-free calcining and cooling.
6. The method according to claim 5, characterized in that the method comprises the following specific steps:
1) and (3) granulation: grinding the raw materials, sieving the ground raw materials by a sieve with 100-plus-300 meshes, uniformly mixing the ground raw materials according to the proportion, putting the mixture into a granulator to form balls, and spraying deionized water according to the solid-to-liquid ratio of 5:1-15:1 in the process of forming the balls to prepare the material balls with the particle size of 1-3 cm;
2) and (3) drying: putting the pellets prepared in the step 1) into an oven, and drying for 8-12 h at 50-80 ℃;
3) roasting: placing the dried pellets in a box-type resistance furnace, heating to 400-1300 ℃ for presintering for 20-40min by a program under the protection of nitrogen atmosphere, and then heating to 1000-1300 ℃ for roasting for 20-40 min;
4) and (3) cooling: after the baking and sintering, cooling for 6-12h to obtain the ceramsite for adsorbing the perfluorinated compounds in the water body.
7. The preparation method of claim 6, wherein the rotation speed of the granulator in the step 1) is 40-100 rpm.
8. The preparation method according to claim 6, wherein the temperature programming speed of the box-type resistance furnace in the step 3) is 10-25 ℃/min.
9. The application of the ceramsite for adsorbing the perfluorinated compounds in the water body is characterized in that: treating the polluted water body by using the ceramsite as defined in any one of claims 1 to 4 or the ceramsite for adsorbing the perfluorinated compounds in the water body prepared by the preparation method as defined in any one of claims 5 to 8, wherein the concentration of the perfluorinated compounds in the polluted water body is 0.5 to 10mg/L, the dosage of the polluted water body is 30 to 100mL, the dosage of the ceramsite is 1 to 3g, the adsorption time is 12 to 48h, and the stirring speed is 100-1000 rpm; the perfluorinated compounds contained in the polluted water body are: perfluorocarboxylic acids, perfluorosulfonates or telomer alcohols.
CN202010171897.XA 2020-03-12 2020-03-12 Ceramsite for adsorbing perfluorinated compounds in water and preparation method thereof Active CN111346601B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010171897.XA CN111346601B (en) 2020-03-12 2020-03-12 Ceramsite for adsorbing perfluorinated compounds in water and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010171897.XA CN111346601B (en) 2020-03-12 2020-03-12 Ceramsite for adsorbing perfluorinated compounds in water and preparation method thereof

Publications (2)

Publication Number Publication Date
CN111346601A true CN111346601A (en) 2020-06-30
CN111346601B CN111346601B (en) 2020-12-29

Family

ID=71189807

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010171897.XA Active CN111346601B (en) 2020-03-12 2020-03-12 Ceramsite for adsorbing perfluorinated compounds in water and preparation method thereof

Country Status (1)

Country Link
CN (1) CN111346601B (en)

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102451662A (en) * 2011-09-26 2012-05-16 郭华明 High-efficiency fluorine-removing adsorbent and preparation method thereof
CN102815965A (en) * 2012-08-30 2012-12-12 武汉钢铁(集团)公司 Porous ceramsite made of low-silicon iron tailings and preparation method of porous ceramsite
CN103801556A (en) * 2014-02-18 2014-05-21 广州中国科学院先进技术研究所 Method for repairing soil containing novel organic pollutant by using sludge biological carbon
CN103962137A (en) * 2014-05-15 2014-08-06 同济大学 Preparation method of titanium dioxide doped carbon-iron composite material for photo-degrading perfluorinated organic acid
CN104098488A (en) * 2013-04-03 2014-10-15 中国科学院生态环境研究中心 Process for harmless treatment of PFOS containing waste by solvothermal technique
JP2014231056A (en) * 2013-04-30 2014-12-11 国立大学法人京都大学 Capture material for polyfluoro compound containing hydrophilic star polymer and capturing method using the same
CN106732379A (en) * 2017-02-23 2017-05-31 华南理工大学 A kind of sludge-based activated carbon with efficient absorption PFOS and PFOA efficiency and preparation method and application

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102451662A (en) * 2011-09-26 2012-05-16 郭华明 High-efficiency fluorine-removing adsorbent and preparation method thereof
CN102815965A (en) * 2012-08-30 2012-12-12 武汉钢铁(集团)公司 Porous ceramsite made of low-silicon iron tailings and preparation method of porous ceramsite
CN104098488A (en) * 2013-04-03 2014-10-15 中国科学院生态环境研究中心 Process for harmless treatment of PFOS containing waste by solvothermal technique
JP2014231056A (en) * 2013-04-30 2014-12-11 国立大学法人京都大学 Capture material for polyfluoro compound containing hydrophilic star polymer and capturing method using the same
CN103801556A (en) * 2014-02-18 2014-05-21 广州中国科学院先进技术研究所 Method for repairing soil containing novel organic pollutant by using sludge biological carbon
CN103962137A (en) * 2014-05-15 2014-08-06 同济大学 Preparation method of titanium dioxide doped carbon-iron composite material for photo-degrading perfluorinated organic acid
CN106732379A (en) * 2017-02-23 2017-05-31 华南理工大学 A kind of sludge-based activated carbon with efficient absorption PFOS and PFOA efficiency and preparation method and application

Also Published As

Publication number Publication date
CN111346601B (en) 2020-12-29

Similar Documents

Publication Publication Date Title
CN107262037B (en) A kind of preparation and application of sepiolite FeOOH active carbon compound adsorbent
CN106423051A (en) Preparation method and application of magnetic activated hydrothermal biochar microspheres
CN103316628B (en) A kind of preparation method and application of adsorbent
CN106732358B (en) A kind of biomass carbonization microballoon loading iron oxide and its preparation and application
CN116474720B (en) Preparation method and application of red mud-based enhanced magnetic straw biochar material
CN107057705B (en) Heavy metal contaminated soil remediation material, preparation method and application
CN109569525A (en) Preparation of amino-modified magnetic rice hull biochar and method for adsorbing uranium in water body by using amino-modified magnetic rice hull biochar
CN114797779A (en) Ferrihydrite modified biochar capable of simultaneously repairing arsenic-lead-cadmium heavy metal polluted soil and preparation method thereof
CN104492372A (en) Preparation method and application of material for adsorbing heavy metals in wastewater
CN111330542B (en) Adsorbing material for adsorbing perfluorinated compounds in water body
CN103586011B (en) Sintering-free forming and coating method of MIL-101 material with ultrahigh specific surface area
CN105709689A (en) Carbon-based functional material and preparation method thereof
CN105396551A (en) Iron-containing biochar prepared from rice roots and application thereof in adsorption and solidification of heavy metal ions
US20160067672A1 (en) Method for preparing granulated inorganic adsorbent for radionuclides
CN106179215A (en) The preparation method of water plant charcoal carbon nano tube compound material and application
CN112680232B (en) Preparation method of ecological-friendly soil composite repairing agent
CN113231005B (en) Method for preparing porous adsorption material without sintering
CN111346601B (en) Ceramsite for adsorbing perfluorinated compounds in water and preparation method thereof
CN109967032A (en) A kind of method of flyash and stalk joint preparation industrial wastewater adsorbent
CN113750961A (en) Carbon dioxide adsorbent and preparation method thereof
CN101837279A (en) Dry-type CO2 adsorbent using lake sediment and fly ash together as carrier and preparation thereof
KR100275586B1 (en) Soil conditioner using natural mineral and method for producing the same
CN101816928A (en) Method for preparing coke-powder-based carbon adsorbing material by using waste coke powder
CN112774625A (en) Zirconium oxide doped magnetic high-surface active carbon composite material, preparation method and application
CN104353411B (en) The preparation method of the strong sorbent material of a kind of water treatment

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant