CN105418145A - Method of preparing porous phosphor absorbing ceramic particle from sludge in water supply plant - Google Patents

Method of preparing porous phosphor absorbing ceramic particle from sludge in water supply plant Download PDF

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Publication number
CN105418145A
CN105418145A CN201511023099.8A CN201511023099A CN105418145A CN 105418145 A CN105418145 A CN 105418145A CN 201511023099 A CN201511023099 A CN 201511023099A CN 105418145 A CN105418145 A CN 105418145A
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China
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haydite
sludge
balling
raw
waterworks sludge
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CN201511023099.8A
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裴海燕
陈洋
胡文容
孟盼盼
邵媛媛
李政
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Shandong University
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Shandong University
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/009Porous or hollow ceramic granular materials, e.g. microballoons
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B33/00Clay-wares
    • C04B33/02Preparing or treating the raw materials individually or as batches
    • C04B33/13Compounding ingredients
    • C04B33/131Inorganic additives
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B33/00Clay-wares
    • C04B33/02Preparing or treating the raw materials individually or as batches
    • C04B33/13Compounding ingredients
    • C04B33/132Waste materials; Refuse; Residues
    • C04B33/1321Waste slurries, e.g. harbour sludge, industrial muds
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605Treating the starting powders individually or as mixtures
    • C04B35/62695Granulation or pelletising
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/6303Inorganic additives
    • C04B35/6316Binders based on silicon compounds
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74Physical characteristics
    • C04B2235/77Density
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/94Products characterised by their shape
    • C04B2235/945Products containing grooves, cuts, recesses or protusions
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00Technologies relating to the processing of minerals
    • Y02P40/60Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes

Abstract

The invention relates to a method of preparing porous phosphor absorbing ceramic particle from sludge in water supply plant. The preparation method comprises four phases: raw material preprocessing, balling, sintering, and cooling. The preparation method specifically comprises the following steps: picking raw material balls with a particle size of 6 to 8 mm, drying the raw material balls at a temperature of 105 DEG C for two hours, preheating the raw material balls at a temperature of 300 to 400 DEG C for 20 to 30 minutes, burning the raw material balls at a temperature of 1150 DEG C for 8 to 10 minutes, and cooling to obtain the finished product of ceramic particles. Through controlling the material ratio, rotation speed of granulator, the spraying mode of adhesive, burning time, and burning temperature, ceramic particles with a large specific surface area and strong phosphor absorbing performance can be obtained. The ceramic particles can be used as the filling material of a sewage processing system, and the sludge in a water supply plant is converted into valuable resource.

Description

A kind of waterworks sludge prepares the method that multi-hole type inhales phosphorus haydite
One, technical field
The present invention relates to a kind of multi-hole type and inhale phosphorus haydite, belong to sludge ceramsite technical field.
Two, technical background
The water supply plant of current China, mainly through series of process purified water source such as coagulation, precipitation, filtration and sterilizations, removes the impurity such as the suspended matter in former water, colloidalmaterial, and the form of distributing with pipe network is by the water supply user after purification.A large amount of mud can be produced, mainly from the spoil disposal water of settling tank and the flushing waste water of back-purge system in drinking water producing procedure.2014, National urban water factory dewatered sludge (water ratio 70%) annual production is close to 2,200 ten thousand tons, along with the continuous increase of China's population and the quickening day by day of urbanization process, quantity and the scale of water supply plant constantly expand, the sludge quantity that water supply plant produces also will increase day by day, and therefore rationally disposing waterworks sludge becomes the current problem needing solution badly.
Waterworks sludge is a kind of resource of potential recoverable, and there is huge commercial value.Current, the disposal of waterworks sludge mainly concentrate on the direct discharge of spoil disposal water, dehydrated sludge cake ocean dumping, land bury abandon, sanitary landfill, the regeneration of aluminium salt molysite, the aspect such as Land_use change and building materials utilization, but exist and cause the problems such as secondary pollution, subsequent disposal expense are high.The major ingredient of waterworks sludge is the coagulating agent that a large amount of silts, impurity and the water factory brought in source water adds, and its major ingredient is with SiO 2, Al 2o 3, Fe 2o 3be main, the basic satisfied compositional ranges requirement preparing haydite materials, therefore be main raw material with waterworks sludge, a certain amount of auxiliary material, additive, through the swollen light ceramic with some strength of making of burning, can consume dewatered sludge in a large number in addition, the problem of sludge ultimate disposal can be solved, can solve again the problem of haydite materials shortage, especially meeting innoxious, minimizing and the resource utilization principle of China's fixed-end forces, is the new road of a Sustainable development.
Be used as in sewage disposal at waterworks sludge, the core theory of its dephosphorization is that these noncrystal aluminum ions have adsorption to the phosphorus in sewage, and the phosphorus of solubility can be solidified owing to containing noncrystal aluminum ion in mud.Conventional drinking water treatment technology generally adopts coagulation process, and novel coagulant polymerize aluminum chloride etc. instead of Tai-Ace S 150 and iron(ic) chloride gradually, a large amount of aluminum ion is finally deposited in waterworks sludge, has stronger adsorptive power to phosphorus.
In current patent or research, waterworks sludge is utilized to prepare the research of inhaling phosphorus haydite less, be in 201010130425.6, disclose " a kind of be method that major ingredient fire light ceramic with alum sludge " at application number, in this patent, obtained haydite be used for building material industry; Be disclose in 201410334856.2 " application of a kind of haydite production method and haydite and haydite " at application number, in this patent, waterworks sludge addition is less, is only 10 ~ 30%.There is the problems such as copper water-supply pipe addition is less, specific surface area is not high in the haydite prepared in these patent applications.This industrial by-products of the present invention's waterworks sludge prepares haydite, and the production technique of waterworks sludge haydite is optimized for current Problems existing, have studied performance and the P adsorption characteristics of waterworks sludge haydite, inquire into the feasibility of waterworks sludge haydite for Sewage treatment systems dephosphorization, achieve the recycling to waterworks sludge.
Three, summary of the invention
The object of the invention is to: provide a kind of waterworks sludge and prepare the method that multi-hole type inhales phosphorus haydite.Described multi-hole type is inhaled phosphorus haydite and is had stronger phosphorus absorption property.
For achieving the above object, the present invention adopt the preparation process of technical scheme to be:
(1) by waterworks sludge natural air drying, put into pulverizer and grind, sieve with 100 ~ 120 object standard sieves;
(2) waterworks sludge and clay Homogeneous phase mixing are obtained balling-up material, join in nodulizer and prepare raw material ball, spray sodium silicate solution in globulation as tackiness agent;
(3) filter out the raw material ball that particle diameter is 6 ~ 8mm after balling-up, put into baking oven dry 2h under 105 DEG C of conditions and slough moisture, move into retort furnace preheating 20 ~ 30min under 300 ~ 400 DEG C of conditions, continue to be warming up to 1150 DEG C of roasting 8 ~ 10min;
(4) close retort furnace heating power supply, after temperature drops to 400 DEG C, open fire door, naturally cool to room temperature, namely obtain haydite finished product.
In the present invention, in described step (2), waterworks sludge and clay are by (3 ~ 4): the quality of 1 compares Homogeneous phase mixing.
In the present invention, control nodulizer rotating speed in described step (3) at 30 ~ 40r/min.
In the present invention, in described step (3), globulation alternately adds (sprinkling) balling-up material and sodium silicate solution, and the massfraction of sodium silicate solution is 0.5 ~ 2.0%, and sodium silicate solution consumption is balling-up quality of material 10% ~ 15%.
The beneficial effect that the present invention has:
Haydite surface irregularity prepared by the present invention, is evenly covered with the granular projection that diameter is 1 ~ 2mm, and has abundant microvoid structure, and micropore gap comparatively large (1 ~ 5 μm), has stronger physical adsorption ability; It is high that haydite prepared by the present invention has physical strength, and porosity is high, the feature that specific surface area is large, and these features are suitable as the filler of Sewage treatment systems; Waterworks sludge is used as cheap, efficient, novel Sewage treatment systems dephosphorization material and has larger application prospect for control body eutrophication by the present invention.The present invention produces haydite with waterworks sludge and is used for Sewage treatment systems; achieve innoxious, resource utilization and the industrialization process of waterworks sludge; be conducive to protection land resources and water resources; reduce construction investment, working cost, in economic society and environment etc., all there is higher use value.
Four, accompanying drawing explanation
Fig. 1 is the apparent structure figure of sludge ceramsite of the present invention;
Fig. 2 is 3000 times of Electronic Speculum microscopic surface texture figure of sludge ceramsite of the present invention;
Fig. 3 is that multi-hole type of the present invention inhales phosphorus haydite to the adsorption isothermal curve figure of phosphorus.
Five, embodiment
Below in conjunction with embodiment, the present invention is further illustrated.
Embodiment 1
Waterworks sludge prepares the method that multi-hole type inhales phosphorus haydite, and concrete grammar is as follows:
The production technique of waterworks sludge haydite mainly comprises raw-material pre-treatment, balling-up, fires and cool four-stage.
(1) pre-treatment
By waterworks sludge natural air drying, put into pulverizer and grind, sieve with 100 object standard sieves (size of mesh 0.15mm).
(2) balling-up
Waterworks sludge and clay are compared Homogeneous phase mixing by the quality of 3:1, join nodulizer and prepare raw material ball, spray in globulation massfraction be the solution of 0.5% water glass as tackiness agent, sodium silicate solution consumption is balling-up quality of material 10%, and controlling nodulizer rotating speed is 40r/min.
(3) dry
Filter out the raw material ball that particle diameter is 6 ~ 8mm after balling-up, put into baking oven dry 2h under 105 DEG C of conditions and slough moisture, move into retort furnace preheating 20min under 300 DEG C of conditions, continue to be warming up to 1150 DEG C of roasting 8min.
(4) cool
Close retort furnace heating power supply, after temperature drops to 400 DEG C, open fire door, naturally cool to room temperature, namely obtain haydite finished product.
The outward appearance of haydite finished product is the spherical solid that beige surface irregularity has granular projection, uneven COEFFICIENT K 80be 1.8, apparent density is 1.35 ~ 1.40g/cm 3, cylindrical compress strength is 4.2 ~ 4.5Mpa, and specific surface area is 4.7 ~ 4.9m 2/ g, 1h water-intake rate is 8% ~ 13%, and porosity is 43% ~ 47%, percentage of damage≤1.0%, and hydrochloric acid can capacity rate≤0.8%, burning decrement≤0.03%.
Embodiment 2
Waterworks sludge prepares the method that multi-hole type inhales phosphorus haydite, and concrete grammar is as follows:
The production technique of waterworks sludge haydite mainly comprises raw-material pre-treatment, balling-up, fires and cool four-stage.
(1) pre-treatment
By waterworks sludge natural air drying, put into pulverizer and grind, sieve with 120 object standard sieves (size of mesh 0.125mm).
(2) balling-up
Waterworks sludge and clay are compared Homogeneous phase mixing by the quality of 4:1, join nodulizer and prepare raw material ball, spray in globulation massfraction be the solution of 2.0% water glass as tackiness agent, sodium silicate solution consumption is balling-up quality of material 15%, and controlling nodulizer rotating speed is 30r/min.
(3) dry
Filter out the raw material ball that particle diameter is 6 ~ 8mm after balling-up, put into baking oven dry 2h under 105 DEG C of conditions and slough moisture, move into retort furnace preheating 30min under 400 DEG C of conditions, continue to be warming up to 1150 DEG C of roasting 10min.
(4) cool
Close retort furnace heating power supply, after temperature drops to 400 DEG C, open fire door, naturally cool to room temperature, namely obtain haydite finished product.
The apparent structure of haydite finished product as shown in Figure 1, as can be seen from Figure, sludge ceramsite surface irregularity, slickness is low, haydite surface uniform is covered with the granular projection that diameter is 1 ~ 2mm, significantly improves the surface-area that multi-hole type inhales phosphorus haydite, brings abundant microvoid structure.
As shown in Figure 2, as can be seen from Figure, haydite surface is filled with big and small hole to the microvoid structure of haydite finished product, and have a lot of gully, and have abundant microvoid structure, micropore size scope is 1 ~ 5 μm, has stronger physical adsorption ability.
Multi-hole type of the present invention inhales phosphorus haydite, and have stronger phosphorus absorption property, isothermal adsorption characteristics meets Langmuir equation, and concrete research trial method is as follows:
Main agents: 5% potassium persulfate solution, 10% xitix, molybdate solution, Phosphate stock liquid and reference liquid, phenolphthalein, sodium hydroxide solution (1mol/L), sulphuric acid soln (1mol/L)
Major experimental instrument: UV-2450 ultraviolet spectrophotometer; MLS-3750 autoclave sterilizer; Constant temperature oscillator (HZQ-R); Suction filter (GM-0.33II); FA1004 type electronic analytical balance; Moisture eliminator; Liquid-transfering gun.
By potassium primary phosphate (KH pure for top grade 2pO4) in 110 DEG C of dry 2h, let cool in moisture eliminator.Take 0.2197g water-soluble, move in 1000ml volumetric flask.Add (1+1) sulfuric acid 5ml, be diluted with water to graticule, this solution with water is diluted to graticule, and in this solution, every milliliter contains 50.0 μ g phosphorus (in P), as KH 2pO 4stock solution.
(1) take raw material 20g, be placed in 500mlKH 2pO 4in solution, 145r/min vibration under room temperature 25 DEG C of conditions, respectively 1,2,4,6,8,12,24,36,48,72h sampling, centrifugal under 4000r/min rotating speed, get its supernatant liquor, colorimetric estimation, calculate the prepared maximal absorptive capacity of haydite to phosphorus and reach 319mg/kg.
(2) take raw material 10g and be placed in 250ml Erlenmeyer flask, add the KH of 100mL different concns respectively 2pO 4solution (0,5.0,10,20,30,40,50mg/L), be placed in constant-temperature table, with 145r/min, after (25 ± 1) DEG C vibration 72h, 0.45 μm of membrane filtration, molybdenum antimony uvioresistant spectrophotometry is in the phosphorus concentration of 700nm place colorimetric estimation filtrate, and according to change in concentration, institute system is for the characterization of adsorption of haydite to phosphorus.
To the adsorption isothermal curve of phosphorus as shown in Figure 3, isothermal adsorption process can be divided into two stages to prepared haydite: the starting stage, and along with the increase of strength of solution, the adsorptive capacity of haydite to phosphorus increases rapidly, and adsorption isothermal line is steeper; When strength of solution increases to a certain degree, adsorption weakens gradually, increases strength of solution further, and phosphorus adsorptive capacity increasess slowly, and adsorption tends to balance.

Claims (4)

1. prepare with waterworks sludge the method that multi-hole type inhales phosphorus haydite, comprise raw-material pre-treatment, balling-up, fire and cool four-stage, it is characterized in that the preparation method of described haydite is:
(1) by waterworks sludge natural air drying, put into pulverizer and grind, sieve with 100 ~ 120 object standard sieves;
(2) waterworks sludge and clay Homogeneous phase mixing are obtained balling-up material, join in nodulizer and prepare raw material ball, spray sodium silicate solution in globulation as tackiness agent;
(3) filter out the raw material ball that particle diameter is 6 ~ 8mm after balling-up, put into baking oven dry 2h under 105 DEG C of conditions and slough moisture, move into retort furnace preheating 20 ~ 30min under 300 ~ 400 DEG C of conditions, continue to be warming up to 1150 DEG C of roasting 8 ~ 10min;
(4) close retort furnace heating power supply, after temperature drops to 400 DEG C, open fire door, naturally cool to room temperature, namely obtain haydite finished product.
2. a kind of waterworks sludge according to claim 1 prepares the method that multi-hole type inhales phosphorus haydite, it is characterized in that balling-up material by waterworks sludge and clay by (3 ~ 4): the quality of 1 forms than Homogeneous phase mixing.
3. a kind of waterworks sludge according to claim 1 prepares the method that multi-hole type inhales phosphorus haydite, it is characterized in that controlling nodulizer rotating speed in globulation at 30 ~ 40r/min.
4. a kind of waterworks sludge according to claim 1 prepares the method that multi-hole type inhales phosphorus haydite, it is characterized in that globulation alternately adds (sprinkling) balling-up material and sodium silicate solution, the massfraction of sodium silicate solution is 0.5 ~ 2.0%, and sodium silicate solution consumption is balling-up quality of material 10% ~ 15%.
CN201511023099.8A 2015-12-29 2015-12-29 Method of preparing porous phosphor absorbing ceramic particle from sludge in water supply plant Pending CN105418145A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106747299A (en) * 2016-11-28 2017-05-31 北京师范大学 A kind of waterworks sludge base haydite that activates strengthens its method for inhaling phosphorus effect
CN109603734A (en) * 2018-12-28 2019-04-12 博域环保技术研究院(南京)有限公司 Phosphorus adsorbent based on river bottom mud and its application for being back to river water body processing

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102503368A (en) * 2011-10-17 2012-06-20 西安建筑科技大学 Spherical haydite matrix for constructed wetland and its preparation method
CN104163617A (en) * 2014-07-14 2014-11-26 深圳市环境科学研究院 Ceramsite preparation method, ceramsite and ceramsite application

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Publication number Priority date Publication date Assignee Title
CN102503368A (en) * 2011-10-17 2012-06-20 西安建筑科技大学 Spherical haydite matrix for constructed wetland and its preparation method
CN104163617A (en) * 2014-07-14 2014-11-26 深圳市环境科学研究院 Ceramsite preparation method, ceramsite and ceramsite application

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106747299A (en) * 2016-11-28 2017-05-31 北京师范大学 A kind of waterworks sludge base haydite that activates strengthens its method for inhaling phosphorus effect
CN109603734A (en) * 2018-12-28 2019-04-12 博域环保技术研究院(南京)有限公司 Phosphorus adsorbent based on river bottom mud and its application for being back to river water body processing

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