CN102500162B - Iron carbonyl-coated filtering material and preparation method and application thereof - Google Patents
Iron carbonyl-coated filtering material and preparation method and application thereof Download PDFInfo
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- CN102500162B CN102500162B CN201110361422.8A CN201110361422A CN102500162B CN 102500162 B CN102500162 B CN 102500162B CN 201110361422 A CN201110361422 A CN 201110361422A CN 102500162 B CN102500162 B CN 102500162B
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Abstract
The invention discloses an iron carbonyl-coated filtering material and a preparation method and application thereof. The filtering material has a core-shell structure, wherein the core refers to a ceramic filtering material substrate which is formed by pelleting and sintering a ceramic filtering material and the ceramic filtering material is at least one of kaolin, quartz and white mica; and the shell refers to an iron carbonyl active substance coating layer coating the surface of the core. The iron carbonyl-coated filtering material provided by the invention has strong absorption, high physical strength, good chemical stability, excellent absorption and interception effect on dissolved pollutants in water and good physical filtering effect superior to that of the traditional ceramic filtering material; therefore, the iron carbonyl-coated filtering material can generate good economic and social benefits and has a very good application prospect.
Description
Technical field
The present invention relates to a kind of material for water treatment, particularly, relate to a kind of iron carbonyl-coated filtering material, its preparation method and for removing the application of water arsenic, fluorine, wet goods pollutant.
Background technology
Along with the plant-scale rapid growth of China, the water pollution problem being caused by industrial wastewater, waste residue also becomes increasingly conspicuous.In 28 important water contamination accidents that 2001 ~ 2008 years occur in China, have 3 to originate from arsenic pollution in water, 2 originate from fluoride pollution.Because industrial wastewater pollution causes people's arsenic poisoning more than 100, there is the symptoms such as vomiting, numbness in hands and feet, eye mask hyperemia in Hengyang, Hunan Province in 2002.Guizhou in 2007 all Liujiang makes 17 people's arsenic poisonings because of the illegal blowdown of enterprise, and causes the domestic water of people more than 20,000 difficulty along the river.The nearly 200,000 people's fluorine poisonings in Weichang county in 2005, within 2007, Guyuan of Ningxia has again the fluorine poisoning of people more than 70,000.
In recent years, arsenic in water body contamination accident is growing on and on.According to Chinese Academy of Geological Sciences's hydrological environment Institute of Geology testing result to Yunnan bavin rock patch reservoir, domestic waters, Nanpanjiang River Yiliang arsenic content between in April, 2011, find that arsenic content reaches respectively 0.215mg/L and 0.226mg/L, belongs to severe contamination.In September, 2010, in the running water example inspection in yueyang, hunan county, also find 10 times of arsenic content overproofs, pollute and come from the discharge in violation of regulations of enterprise's high concentration containing arsenic sewage.
In some areas of China East China, North China, northwest, comprise the areas such as Henan, Hebei, Tianjin, Anhui, Shanxi, Inner Mongol, Gansu, Ningxia, Qinghai, Xinjiang, groundwater resources are all to some extent by fluoride pollution, particularly North China drinks the absolute number of high-fluorine water and ratio all ranks first in the country, and is secondly East China.Have statistics to show, China has at least 5,000 ten thousand people drinking high-fluorine water, occurs that because long-term drinking high-fluorine water causes large area the provinces，municipalities and autonomous regions of the fluorine illnesss such as fluorine dental plaque, fluorosis of bone have accounted for national half.
China is the country of a water resource wretched insufficiency, and the freshwater resources that have are per capita less than 25% of world average level.The day by day serious pollution problem causing to China's water resource for harmful elements such as arsenic, fluorine in China's industrial wastewater; develop a kind of can efficient adsorption the filtering material of the objectionable impurities such as arsenic, fluorine in water, healthy all tools of China's water resource purification, ecological environmental protection and the people are of great significance.
Summary of the invention
The object of this invention is to provide a kind of novel filter material that integrates physical filtering and chemisorbed--iron carbonyl-coated filtering material, this filtering material adopts the coated traditional ceramics filtering material of FeOOH active component, can realize suspended state particle and filter and synchronize the function of removal with dissolved pollutant absorption, industrial wastewater and drinking water be there is to the effect of the objectionable impurities such as good filtration and removal arsenic, fluorine.
In order to achieve the above object, the invention provides a kind of iron carbonyl-coated filtering material, this filtering material has core-shell structure, this core refers to ceramic filter material matrix, this ceramic filter material matrix is to adopt ceramic filter material to form through granulation, sintering, more than this ceramic filter material refers to any one of kaolin, quartz and muscovite; This shell refers to the surface coated FeOOH active material clad at described core.
Above-mentioned iron carbonyl-coated filtering material, wherein, the material that described ceramic filter material comprises the following meter of percentage by weight:
SiO
2 68~70%;
Al
2O
3 18~24%;
CaO 1~2%;
K
2O/Na
2O 3~3.8%;
CaMg(CO
3)
2 5%。
Above-mentioned iron carbonyl-coated filtering material, wherein, described FeOOH active material comprises FeO (OH), and this FeO (OH) is that ferric hydroxide precipitate obtains through calcining and activating processing.
Above-mentioned iron carbonyl-coated filtering material, wherein, described FeOOH active material layer also comprises: percentage is counted 18 ~ 20% magnesia sintering aid by weight, more than this magnesia sintering aid comprises any one of dolomite, talcum and clinochlore.
Above-mentioned iron carbonyl-coated filtering material, wherein, described magnesia sintering aid is by percentage meter 30-50% dolomite, 30-50% talcum and 10-30% clinochlore form by weight; The magnesia sintering aid that more preferably percentage meter 40% dolomite, 40% talcum and 20% clinochlore form by weight.Described clinochlore is as binding agent.
Above-mentioned iron carbonyl-coated filtering material, wherein, described coating thickness is 0.5 ~ 1.0mm.
The present invention also provides a kind of preparation method of above-mentioned iron carbonyl-coated filtering material, and the method comprises following concrete steps:
Step 1, prepare filtrate matrix: take ceramic filter material, add percentage by weight and mix after counting 10 ~ 14% water, after shelving homogenizing, be configured as the green compact ball of diameter 1 ~ 3mm with group's ball machine, after dry in shuttle kiln in 1250 ~ 1280 ℃ of sintering, be incubated naturally cooling after 2 ~ 4 hours;
Step 3, coated: the group's of employing ball machine is coated the filtrate matrix that FeOOH active material prepared by step 2 is prepared step 1, coating thickness is controlled at 0.5 ~ 1.0mm, then activates 1 ~ 1.3 hour at 400 ~ 800 ℃, and qualified product can be packed and dispatch from the factory after testing.
The preparation method of above-mentioned iron carbonyl-coated filtering material, wherein, in step 2, also comprises: the step that the FeOOH of activation is mixed with magnesia sintering aid.
The preparation method of above-mentioned iron carbonyl-coated filtering material, wherein, described magnesia sintering aid adds water and converts into liquid, joins in the FeOOH of activation with the form of spraying.
The present invention also provides the application of a kind of above-mentioned iron carbonyl-coated filtering material in water treatment.
Existing ceramic filter material is widely used in water treatment field, but does not possess the arsenic in adsorbed water pollution, the ability of fluorine harmful element; And iron carbonyl-coated filtrate of the present invention can be widely used in water treatment field, and possess the arsenic in adsorbed water pollution, the ability of fluorine harmful element, the adsorbable arsenic >9mg/g of iron carbonyl-coated filtering material, fluorine ~ 8mg/g.
Product high adsorption capacity provided by the invention, physical strength is high, chemical stability good, not only dissolved pollutant in water body is had to good absorption rejection effect, and its physical filtering effect is also better than traditional ceramic filter material, can produce good economic benefit and social benefit, there is extraordinary application prospect.
Accompanying drawing explanation
Fig. 1 is the structural representation of a kind of iron carbonyl-coated filtering material of the present invention.
Fig. 2 is the process chart that the present invention prepares iron carbonyl-coated filtering material.
Fig. 3 is mineral composition X-ray diffraction (XRD) analysis chart of embodiments of the invention Raw china clay; The expression quartz that wherein marks Δ, O represents muscovite.
Fig. 4 is thermogravimetric-differential thermal (TG-DSC) analysis chart of FeOOH of the present invention.
Fig. 5 is X-ray diffraction (XRD) analysis chart of the FeOOH product after 600 ℃ of calcining and activatings of the present invention, wherein
.
Fig. 6 is X-ray diffraction (XRD) analysis chart of magnesia sintering aid of the present invention,
Wherein
.
Fig. 7 is X-ray diffraction (XRD) analysis chart of ceramic filter material matrix after sintering of the present invention,
Wherein:
.
Fig. 8 is microstructure (SEM, × 3000) schematic diagram of ceramic filter material matrix after sintering of the present invention.
Fig. 9 is X-ray diffraction (XRD) analysis chart of iron carbonyl-coated filter material surface of the present invention
Wherein:
.
Figure 10 is the combination situation schematic diagram between cover surface of the present invention and ceramic filter material matrix.
The specific embodiment
Below in conjunction with accompanying drawing, technical scheme of the present invention is described further.
In order to make the existing certain intensity of iron carbonyl-coated filtrate, there are again good filtration and absorption property, as shown in Figure 1, iron carbonyl-coated filtering material provided by the invention has core-shell structure: take traditional ceramic filter material as matrix 10(, core), at the coated FeOOH active material clad 20(in its surface, shell).This ceramic filter material matrix 10 is to adopt ceramic filter material to form through granulation, sintering, more than this ceramic filter material refers to any one of kaolin, quartz and muscovite.
As shown in Figure 2, for the present invention prepares the technological process of iron carbonyl-coated filtering material: ceramic filter material is through being uniformly mixed, granulation, sintering, obtains ceramic filter material matrix; Ferric trichloride and NaOH obtain iron hydroxide through chemical deposition step, and this iron hydroxide obtains FeOOH through calcining and activating, after this FeOOH mixes with magnesia sintering aid, be coated on ceramic filter material matrix outside, activated again, after the assay was approved, packing.
Embodiment 1
Preparing FeOOH, coated filtering material is raw materials used comprises: china clay, ferric trichloride, NaOH, magnesia sintering aid.
The china clay that ceramic filter material matrix is produced take Pingxiang is primary raw material, and its mineral composition is mainly kaolin, quartz and a small amount of muscovite, as shown in Figure 3.
Clad FeOOH is in the iron chloride (FeCl of percentage 20% by weight
3), 15% caustic soda (NaOH) and 65% water is raw material reaction, adopts chemical deposition preparation; Wherein, the chemical reaction of formation FeOOH is as follows:
FeCl
3 + 3NaOH ─→ Fe(OH)
3↓+ 3NaCl
Fe(OH)
3 ─→ FeO(OH) + H
2O。
As shown in Figure 4,, there is a Weight lose slowly from room temperature to 900 ℃ in thermogravimetric-differential thermal (TG-DSC) analysis result demonstration of FeOOH, total weight loss is 3.29% always, illustrate that removing of hydroxyl is a progressive process, before 900 ℃, FeOOH all has higher activity.As shown in Figure 5, principal crystalline phase is Fe to the XRD analysis result of the FeOOH product after 600 ℃ of calcining and activatings
2o
3and FeO (OH), separately there is a small amount of SiO
2, may in sample process, bring into.
In order to improve the bond strength between FeOOH clad and ceramic filter material matrix, in hydroxyl oxidize iron powder, add the magnesia sintering aid of percentage meter 18% by weight, its thing phase composition as shown in Figure 6, by 40%(percentage by weight) dolomite, 40% talcum and 20% oblique green mud mix and form, stirring adds water, convert into liquid mixture, add with the form of spraying.
Step 1, prepare filtrate matrix: take ceramic filter material, add percentage by weight and mix after counting 10% water, after shelving homogenizing, be configured as the green compact ball of diameter 1 ~ 3mm with group's ball machine, after dry in shuttle kiln in 1250 ℃ of left and right sintering, be incubated naturally cooling after 2 ~ 4 hours; After sintering, as shown in Figure 7, its principal crystalline phase is mullite and quartz (SiO to the X-ray diffraction analysis result of ceramic filter material matrix
2), separately there is a small amount of ferrosilite (FeSiO
3).In order to obtain higher-strength, ceramic matrix is realized densification sintering substantially, surface is rough structure, be conducive to iron carbonyl-coated on its surface, be illustrated in figure 8 the microstructure (× 3000) of ceramic filter material matrix after sintering, inner visible average grain size is below 10 μ m, and aperture is many between 2 ~ 5 μ m.
Step 3, coated: the group's of employing ball machine is coated the filtrate matrix that FeOOH active material prepared by step 2 is prepared step 1, coating thickness is controlled at 0.5 ~ 1.0mm, then activates at 400 ~ 800 ℃, and qualified product can be packed and dispatch from the factory after testing.As shown in Figure 9, main crystalline phase is iron oxide, silica and FeOOH to the XRD analysis result of the iron carbonyl-coated filter material surface of gained.Combination situation between cover surface and ceramic filter material matrix as shown in figure 10, be combined with clad closely, without sharp interface by matrix.
The Performance Detection of iron carbonyl-coated filtering material
Iron carbonyl-coated filtering material product prepared by the present invention is through the Jiangxi Province's industrial ceramics quality monitoring testing station check of test center of industrial ceramics country, and result is as follows:
Bulk density: 1.78 g/cm
3
Bulk density: 1.62 g/cm
3
Percentage of damage: 0.75 %
Mohs' hardness: 6 grades
Pile up porosity: 28.60 %
Water absorption rate: 2.16 %
Thermal conductivity factor: 4.41 W/m.K
Specific heat: 735 J/kg.K
Arsenic maximal absorptive capacity: 9.48 mg/g
Fluorine maximal absorptive capacity: 8.0 mg/g
Oil maximal absorptive capacity: 3.0 mg/g.
Product of the present invention shows at the result on trial of the normal flat Second Waterworks in Dongguan, Guangdong Province, uses after product of the present invention, and in water, arsenide content is reduced to 0.03mg/L by original 0.2mg/L; Content of fluoride is reduced to 0.8mg/L by 1.3mg/L, and through repeatedly check, property indices all reaches national drinking water standard.
Product of the present invention is for the treatment process of oily waste water, electroplating wastewater, comprehensive wastewater, through repeated detection, show that this product can separate the pollutant in water body by efficient adsorption, especially arsenic, fluorine, wet goods pollutant are had to efficient adsorption and hold back effect, meet designing requirement and the discharge standard to wastewater treatment completely.
Because high adsorption capacity, the physical strength of product of the present invention is high, chemical stability good, not only dissolved pollutant in water body had to good absorption rejection effect, and its physical filtering effect is also better than traditional ceramic filter material, has huge market prospects.
Except magnesia sintering aid composition, prepare that the coated filtering material of FeOOH is raw materials used and percentage by weight composition is identical with embodiment 1.The present embodiment magnesia sintering aid used is made up of talcum.
Adopt the method identical with embodiment 1, prepare iron carbonyl-coated filtering material 2, its main performance index is as shown in table 1.
Embodiment 3
Except magnesia sintering aid composition, prepare that the coated filtering material of FeOOH is raw materials used and percentage by weight composition is identical with embodiment 1.The present embodiment magnesia sintering aid used is made up of 80% talcum and 20% oblique green mud.
Adopt the method identical with embodiment 1, prepare iron carbonyl-coated filtering material 3, its main performance index is as shown in table 1.
Table 3 iron carbonyl-coated filtrate 2 and 3 main performance index
Although content of the present invention has been done detailed introduction by above preferred embodiment, will be appreciated that above-mentioned description should not be considered to limitation of the present invention.Read after foregoing those skilled in the art, for multiple modification of the present invention and substitute will be all apparent.Therefore, protection scope of the present invention should be limited to the appended claims.
Claims (7)
1. an iron carbonyl-coated filtering material, it is characterized in that, this filtering material has core-shell structure, this core refers to ceramic filter material matrix (10), this ceramic filter material matrix (10) is to adopt ceramic filter material to form through granulation, sintering, more than this ceramic filter material refers to any one of kaolin, quartz and muscovite; This shell refers to the surface coated FeOOH active material clad (20) at described core, and described clad (20) thickness is 0.5～1.0mm; Described FeOOH active material comprises FeO (OH), and this FeO (OH) is that ferric hydroxide precipitate obtains through calcining and activating processing; Described FeOOH active material also comprises: percentage is counted 18～20% magnesia sintering aid by weight, more than this magnesia sintering aid comprises any one of dolomite, talcum and clinochlore;
This iron carbonyl-coated filtering material is prepared by the following method:
Step 1, prepare ceramic filter material matrix: take ceramic filter material, add percentage by weight and mix after counting 10～14% water, after shelving homogenizing, be configured as the green compact ball of diameter 1～3mm with group's ball machine, after dry in shuttle kiln in 1250～1280 ℃ of sintering, be incubated naturally cooling after 2～4 hours;
Step 2, prepare FeOOH active material: the iron hydroxide obtaining with ferric trichloride and sodium hydroxide solution chemical deposition, this iron hydroxide is 600～900 ℃ of calcining bondings, obtain the FeOOH of activation, the FeOOH of activation is mixed to i.e. FeOOH active material with magnesia sintering aid;
Step 3, coated: the group's of employing ball machine is coated the ceramic filter material matrix that FeOOH active material prepared by step 2 is prepared step 1, coating thickness is controlled at 0.5～1.0mm, then activates 1～1.3 hour at 400～800 ℃, and qualified product can be packed and dispatch from the factory after testing.
2. iron carbonyl-coated filtering material as claimed in claim 1, is characterized in that, the material that described ceramic filter material comprises the following meter of percentage by weight:
The percetage by weight summation of described material is 100%.
3. iron carbonyl-coated filtering material as claimed in claim 1, is characterized in that, described magnesia sintering aid is by percentage meter 30-50% dolomite, 30-50% talcum and 10-30% clinochlore form by weight.
4. iron carbonyl-coated filtering material as claimed in claim 3, is characterized in that, described magnesia sintering aid is by percentage meter 40% dolomite, 40% talcum and 20% clinochlore form by weight.
5. according to a preparation method for the iron carbonyl-coated filtering material described in claim 1-4 any one, it is characterized in that, the method comprises following concrete steps:
Step 1, prepare ceramic filter material matrix: take ceramic filter material, add percentage by weight and mix after counting 10～14% water, after shelving homogenizing, be configured as the green compact ball of diameter 1～3mm with group's ball machine, after dry in shuttle kiln in 1250～1280 ℃ of sintering, be incubated naturally cooling after 2～4 hours;
Step 2, prepare FeOOH active material: the iron hydroxide obtaining with ferric trichloride and sodium hydroxide solution chemical deposition, this iron hydroxide is 600～900 ℃ of calcining bondings, obtain the FeOOH of activation, the FeOOH of activation is mixed to i.e. FeOOH active material with magnesia sintering aid;
Step 3, coated: the group's of employing ball machine is coated the filtrate matrix that FeOOH active material prepared by step 2 is prepared step 1, coating thickness is controlled at 0.5～1.0mm, then activates 1～1.3 hour at 400～800 ℃, and qualified product can be packed and dispatch from the factory after testing.
6. the preparation method of iron carbonyl-coated filtering material as claimed in claim 5, is characterized in that, described magnesia sintering aid adds water and converts into liquid, joins in the FeOOH of activation with the form of spraying.
7. the application in water treatment according to the iron carbonyl-coated filtering material described in claim 1-4 any one.
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| CN103316626B (en) * | 2013-07-12 | 2015-01-21 | 苏州微陶重金属过滤科技有限公司 | Filtering material having arsenic and heavy metal adsorbing and fixing functions, and use thereof |
| CN103880109B (en) * | 2014-03-20 | 2016-02-03 | 苏州腾纳环保科技有限公司 | A kind of manufacture method of forced purifying water-based filtrate |
| CN105289549A (en) * | 2015-12-01 | 2016-02-03 | 佛山市农业总公司 | Filtering medium and filter core for removing hexavalent chromium from drinking water and preparation method of filtering medium |
| CN105344160B (en) * | 2015-12-16 | 2017-12-22 | 安徽兴安电气设备股份有限公司 | A kind of water process composite filtering material |
| CN106179193A (en) * | 2016-08-30 | 2016-12-07 | 内蒙古师范大学 | A kind of polymerization iron carbonyl modified kaolin composite and its preparation method and application |
| CN107233884B (en) * | 2017-06-05 | 2020-06-30 | 云南驰宏锌锗股份有限公司 | Ferromagnetic catalyst for catalyzing hydrolysis and precipitation of trivalent iron, and preparation method and application thereof |
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| JP2579177B2 (en) * | 1987-12-26 | 1997-02-05 | 戸田工業株式会社 | Composite iron oxide particle powder and method for producing the same |
| CN101696037A (en) * | 2009-11-05 | 2010-04-21 | 中国烟草总公司郑州烟草研究院 | Beta-FeOOH particles, preparation method and application thereof |
| CN101982237A (en) * | 2010-09-20 | 2011-03-02 | 中国海洋石油总公司 | Preparation method of ozone catalytic oxidation catalyst used for treating oil refining waste water |
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Patent Citations (3)
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|---|---|---|---|---|
| JP2579177B2 (en) * | 1987-12-26 | 1997-02-05 | 戸田工業株式会社 | Composite iron oxide particle powder and method for producing the same |
| CN101696037A (en) * | 2009-11-05 | 2010-04-21 | 中国烟草总公司郑州烟草研究院 | Beta-FeOOH particles, preparation method and application thereof |
| CN101982237A (en) * | 2010-09-20 | 2011-03-02 | 中国海洋石油总公司 | Preparation method of ozone catalytic oxidation catalyst used for treating oil refining waste water |
Non-Patent Citations (1)
| Title |
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