CN103386231B - Filter core material of household filter and preparation method thereof - Google Patents
Filter core material of household filter and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a filter core material of a household filter and a preparation method thereof. The filter core material is composed of porous ceramic substrate and nano zero valence iron particles in-situ formed in the porous ceramic substrate, the sizes of the micro-pores are in the range of 2 to 10 micrometers, furthermore, villiform amorphous silicon-iron-carbon structures are formed in the micro-pores, and the villiform amorphous silicon-iron-carbon structures in the micro-pores can form an absorbing membrane after absorbing water. The porous ceramic substrate is composed of following components in parts by weight: 75 to 85 parts of diatomite, 8 to 10 parts of carbon powder, 1 to 3 parts of bentonite and 3 to 5 parts of kaolin. The filter core material has nasal-analog, porous and villiform filtering structures in micro-structure, the structures can form an absorbing membrane, so the absorption efficiency is largely improved, and the filter core material can adapt to the chemical environment change of water body. The filter core material is safe in use because no heavy metal will fall off or separate out from the used filter material.
Description
Technical field
The present invention relates to a kind of can effectively except the filter core material of household filter and preparation method thereof of anhydrate middle trivalent arsenic and pentavalent arsenic.
Background technology
Arsenic is one of element that toxicity is very strong, the main inorganic toxins removed in Ye Shi various countries drinking water standard.Exist mainly with trivalent and pentavalent state in nature water body.But it is as a kind of metallic element, not exist with the state of common cation, and mainly exist with arsenous anion and arsenate form.Even if the technology in modern times is only about 50% as reverse osmosis membrane (RO) to arsenious clearance, the filtration needs to arsenic can not be met.In addition, filtering material filters arsenic and the great heavy metal of toxicity, must take into account the fixation problem after absorption.
Conventional porous pottery and ceramic element utilize diatomaceous natural porous structure can remove bacterium and larger molecular organics, but can not remove arsenic and the heavy metal of ionic condition.On the other hand, Zero-valent Iron/nano zero valence iron is less than 6 at low pH() in water, slowly corrode and contribute two free charges, arsenic and heavy metal are reduced and symbiosis precipitation (co-precipitation), thus reach the object of removal heavy metal.But the independent application of Zero-valent Iron, brings following problem: one, corrosion reaction must could occur under pH is less than the environment of 7, regulation and control pH is the application restriction of Drinking Water Filtration; Two, certain dissolved oxygen (being greater than 2 mg/litre) ability sustained response must be had in water; Three, form harmful mud in course of reaction, can not heavy metal be fixed, need further harmless treatment; Four, produce ferric iron or the ferrous ion of great quantities of spare in use procedure, water is presented red or orange, must process further.
In order to solve these application restricted problems of Zero-valent Iron, some researchs take Zero-valent Iron or nano zero valence iron to be formed on porous ceramic particles prepared by active carbon, natural diatomaceous earth, kaolin and kaolin in the mode of coating.But the way of coating still exists some problems, the coating prepared as active carbon mixing method easily comes off when pH change or change of water quality, and this can cause acute poisoning in drinking water; In addition, filtering material easily produces zeroth order iron powder and comes off and the problem of surface oxidation, thus reduces its adsorption capacity.
Chinese invention patent ZL200680052402.X discloses a kind of method and composition removing arsenic and heavy metal from water, kaolin ceramic particle is wherein used to carry out the method for Zero-valent Iron coating, can effectively remove arsenic and heavy metal, and realize heavy metal at ceramic surface and fix, but the method also only can utilize ceramic surface structure, adsorption efficiency also needs further raising.
Sum up, in the removal of arsenic, the major defect of prior art is: one, traditional ceramics oxidizing roasting only can provide loose structure filter bacteria and macromolecular substances to carry out physical filtering; Two, zeroth order iron powder applies voluminous pig iron ion and harmful waste; Three, there is the problem that comes off in active carbon iron powder coating; Four, ceramic grain surface coating only can utilize surface texture.
Summary of the invention
Technical problem to be solved by this invention overcomes the deficiencies in the prior art, provides a kind of novel filter material that can be used as filter core material of household filter and preparation method thereof.
For solving the problems of the technologies described above, a kind of technical scheme that the present invention takes is:
A kind of filter core material of household filter, this material for core is the porous ceramic matrices suitable of 35% ~ 85% by porosity and forms at the nanometer nulvalent iron particle that the internal in-situ of porous ceramic matrices suitable generates, the micropore size of porous ceramic matrices suitable is 2 ~ 10 microns, and in described micropore, be formed with velvet-like unformed silicon-iron-carbon structure, velvet-like unformed silicon-iron-carbon structure in described micropore can form adsorbed film after absorbing water, with parts by weight, the material of porous ceramic matrices suitable consists of: 75 ~ 85 parts, diatomite, powdered carbon 8 ~ 10 parts, bentonite 1 ~ 3 part, kaolin 3 ~ 5 parts.
According to the present invention, the surface of described material for core is iron cyan or cinerous, and fresh section is blue, and material for core becomes black after water suction or immersion; Below 0.1mm Y25 ferromagnetic powder can adsorb by described material for core; Described material for core is after scraping off top layer powder, and the pH measured by NY/T1377-2007 Soil standard is 8.0 ~ 8.5.
Preferably, the porosity of described porous ceramic matrices suitable is 55% ~ 70%.
Preferably, described material for core obtains by carrying out Nanoscale Iron modification to porous ceramic matrices suitable, the method of Nanoscale Iron modification is first by upper for porous ceramic matrices suitable absorption ferrous ion, recycling reducing agent carries out in-situ reducing to the ferrous ion be adsorbed on porous ceramic matrices suitable, finally porous ceramic matrices suitable is carried out anaerobic sintering at 400 DEG C ~ 500 DEG C.
Preferably, the shape of material for core is the spheric granules of 1 ~ 2mm or the cylindrical particle of long 5 ~ 20mm.
The another technical scheme that the present invention takes is: a kind of preparation method of above-mentioned filter core material of household filter, it comprises the steps:
(1) diatomite, bentonite, kaolin, powdered carbon, starch, liquid wax, iron powder are pressed formula rate mixing, at temperature 700 DEG C ~ 900 DEG C, carry out anaerobic sintering, obtain described porous ceramic matrices suitable;
(2), porous ceramic matrices suitable is dipped into pH7.0 ~ 8.0, containing in the aqueous phase mixed liquor of ferrous ion and tackifier, after porous ceramic matrices suitable complete wetting, take out porous ceramic matrices suitable, dry for subsequent use, wherein: tackifier are one or more the combination in glucose, sucrose and soluble starch, the content of tackifier in aqueous phase mixed liquor is 0.2wt% ~ 15wt%, and the content of described ferrous ion in aqueous phase mixed liquor is 1wt% ~ 2wt%;
(3) porous ceramic matrices suitable through step (2) is immersed in pH8.5 ~ 9.5, the aqueous solution containing sodium borohydride 2wt% ~ 3wt%, takes out after 2 ~ 8 minutes, dry for subsequent use;
(4) porous ceramic matrices suitable through step (3) is put in anaerobic stove, under nitrogen or hydrogen shield carry out anaerobic sintering; programming rate is 80 ~ 100 DEG C/h; be warming up to 300 DEG C ~ 500 DEG C, be incubated 0.5 ~ 3 hour, obtain described filter core material of household filter.
Further, in step (1), preferably sinter at temperature 750 ~ 850 DEG C.In step (2), ferrous ion can the form of such as frerrous chloride or ferrous sulfate be incorporated in solution.
According to a concrete and preferred aspect of the present invention: in step (2), regulate pH with natrium citricum.
According to another concrete and preferred aspect of the present invention: in step (3), use winestone acid for adjusting pH.
Preferably, in step (4), sintering temperature is 380 DEG C ~ 420 DEG C.More preferably, sintering temperature is 400 DEG C.
Filter core material of household filter provided by the present invention effectively can remove arsenic in drinking water and the plumbous chromium of heavy metal cadmium mercury.
Due to the enforcement of above technical scheme, the present invention compared with prior art tool has the following advantages:
1, material for core of the present invention has high absorption fixed function to trivalent arsenic and pentavalent arsenic, and the filter core be made up of the present invention, when 15 seconds times of contact of waterpower, can be removed arsenic plumbous mercury chromium ion clearance and reach more than 90%;
2, the glassware for drinking water after material for core of the present invention filters has stable alkalescent;
3, zeroth order nanometer iron powder is in the formation of microstructure, and have reproducibility environment C to protect, heavy metal cation has metathesis fast: Fe
0+ X
+→ Fe
++ X; Fe
+the form that can form (FeOOH) at silica surface is fixed, and wherein X can be lead, cadmium, mercury ion, but is not limited to these heavy metal ion, and after fixing, material for core is under simulation landfill yard condition, does not separate out heavy metal.Used civilian filter core material, does not come off or separates out heavy metal, ensure that its safety in utilization;
4, material for core of the present invention has strong reducing property to hexavalent chromium.Due to the existence of Zero-valent Iron, to poisonous Cr VI, nontoxic and useful trivalent chromium can be reduced to;
5, the silicon-iron-carbon structure of material for core of the present invention and hole active surface thereof are to the chlorine residue gas in water and chemical disinfection byproducts, also have removal effect.At 1.2 liters/min, the clearance of 90% when 12 seconds times of contact, can be reached;
6, material for core of the present invention is mainly used in water filtration, but also has filtration for the gas containing arsenic mercury and radiocesium;
7, material for core of the present invention after a procedure, can smash as soil conditioner, realize material circulation;
8, preparation method's reaction condition provided by the invention is gentle, and simple to operate, cost is low.
Accompanying drawing explanation
Fig. 1 shows the scanning electron microscope (SEM) photograph of material for core in embodiment, and wherein (1A) is filtering material finished product; (1B) be filtering material finished product (after water suction);
Fig. 2 is resolution chart when testing the strainability of filtering material.
Detailed description of the invention
Known common porous ceramic filter element, such as ordinary white Diatomite ceramic filter core, because micropore is flourishing, have good permeability, can for physically to bacteriological filter.But heavy metal ion can not filter.Although the existing method in ceramic surface formation coating can make pottery obtain the function of arsenic-adsorbing and heavy metal ion, there is coating and easily come off, generate harmful waste and the dissatisfactory problem of adsorption effect.Invention thinking of the present invention is mainly to provide a kind of internal in-situ at porous ceramic filter element to generate the method for nano-iron particle, the filtering material obtained not only has very high removal effect to arsenic and heavy metal ion, and absorption arsenic and heavy metal ion highly stable, do not come off, meanwhile, also there is not coating shedding problem in this filtering material.The present invention is also used for the application of drink water purifying simultaneously for filtering material, be optimized design to the composition of porous ceramic matrices suitable and the preparation condition of filtering material.
In the present invention, the material of porous ceramic matrices suitable is by after diatomite, bentonite, kaolin, powdered carbon mixing, and at temperature 700 DEG C ~ 900 DEG C, carry out anaerobic sintering obtain, porosity is preferably 55% ~ 70%, and shape is preferably hollow filter core shape.
Provided by the inventionly can be specifically implemented as follows the method that porous ceramic matrices suitable carries out Nanoscale Iron modification:
The first step: the sugar solution (such as glucose, sucrose) of preparation 0.2% ~ 15% or soluble starch solution, preferred alkalescent pH7.5 ~ 8.0 of pH7.0 ~ 8.0(are adjusted to) with natrium citricum, add sulfurous acid iron or frerrous chloride (consumption such as 2% ~ 6%), dissolve completely;
Second step: porous ceramic matrices suitable (such as common Diatomite ceramic filter core) is fully immersed in solution prepared by the first step, makes it completely moistening, more than 15 minutes, pull out dry stand-by;
3rd step: preparation sodium borohydride aqueous solution (sodium borohydride content 2% ~ 3%), dissolves completely, preferably regulates pH to 8.5 ~ 9.5 with such as tartaric acid solution, stand-by;
4th step: in the sodium borohydride aqueous solution that the porous ceramic matrices suitable rapid soaking dried by second step is prepared in the 3rd step, ceramic element generation surface chemical reaction, taking-up in 2 to 5 minutes is dried.
5th step: the porous ceramic matrices suitable that the 4th step is dried is placed in the anaerobic stove of nitrogen protection or hydrogen shield and is heated to 300 DEG C ~ 500 DEG C; optimum temperature about 400 DEG C; 80 ~ 120 DEG C per hour of heating rate (such as 100 DEG C); be incubated 0.5 ~ 3 hour; obtain filtering material; be cooled to less than 120 DEG C, take out.
The filtering material physics generated according to the method described above and structure as follows:
1) color: be cinerous or iron cyan, fresh section is blue, meets water (absorb water or soak rear) and becomes black;
2) pH: scrape off top layer powder, is determined as 8.0-8.5 by NY/T1377-2007 Soil standard.
3) material section structure: show under 5000 times of electron microscopes is 2 ~ 10 micrometer Millipore, inside has Si-Fe-C unformed (amorphous, amorphous) migrated first dopant, Nanoscale Iron structure, forms infiltrative type interlayer film after absorbing water.
4) magnetic testing: to Y25 (3800GS) magnet, can be less than the powder particle absorption of 0.1 millimeter.
Known, the nose of human or animal is perfect filter, because it has a unique structure: 1, electrostatic vibrissa absorption bulky grain and dust; 2, the adsorbable bacterium in nasal cavity built-in fine fleece surface; 3, the strong adsorption of chemical species of bronchia mucosal constantly generated and fixing.In microstructure, the porous ceramic matrices suitable (kaolin, diatomite, bentonite etc.) that the present invention adopts loses the crystallization water and forms loose structure after high-temperature calcination, but under certain controlled condition, water can be absorbed again and be reduced into membranaceous interlayer structure containing the crystallization water.Therefore, gained filtering material of the present invention, in microstructure, forms the porous of similar nose, fine hair filtration generate adsorbed film, thus will increase substantially adsorption efficiency, adapts to hydrochemistry environmental change.
Below in conjunction with specific embodiment, the present invention will be further described in detail, but the invention is not restricted to following examples.Content involved below, without when defining especially, refers to mass content.
The present embodiment provides a kind of filter core material of household filter, and its preparation method is as follows:
The first step: normal temperature preparation soluble starch solution, adds ferrous chloride aqueous solution, adjusts pH to 7.5 ~ 8.0 with natrium citricum, obtain the aqueous solution of content of starch 5%, ferrous ion content 2%;
Second step: porous ceramic matrices suitable is fully immersed in solution prepared by the first step, makes it completely moistening, more than 15 minutes, pull out dry stand-by;
3rd step: preparation 2wt% sodium borohydride aqueous solution, regulates pH to 8.5 ~ 9.5 with 0.1% tartaric acid solution, stand-by;
4th step: in the sodium borohydride aqueous solution that the porous ceramic matrices suitable rapid soaking dried by second step is prepared in the 3rd step, ceramic element generation surface chemical reaction, taking-up in 5 minutes is dried.
5th step: be placed in the kiln of nitrogen protection or hydrogen shield by the porous ceramic matrices suitable that the 4th step is dried, is heated to about 400 DEG C with the heating rate of 90 DEG C/h, is incubated 2 hours, and sintering obtains filtering material, is cooled to less than 120 DEG C, takes out.
In this example, with parts by weight, porous ceramic matrices suitable used is formed with anaerobic side's sintering by 80 parts, diatomite, calcium-base bentonite 2 parts, kaolin 5 parts, powdered carbon 10 parts, sintering temperature 800 DEG C, porosity 65%, pH8.5, color is cinerous, and one-tenth base shape is the single radial cut tubulose of long 200mm, overall diameter 40mm, interior diameter 33mm.
physical property and the structure of this routine gained filtering material are as follows:
1) color: be cinerous or iron cyan, fresh section is blue, meets water (absorb water or soak rear) and becomes black; Shape: the filter core of external diameter 40mm, internal diameter 35mm, length 200mm.
2) pH: scrape off top layer powder, is determined as 8.3 ~ 8.5 by NY/T1377-2007 Soil standard.
3) material section structure: show under 5000 times of electron microscopes is 2 ~ 10 micrometer Millipore, inside has Si-Fe-C unformed (amorphous, amorphous) migrated first dopant, Nanoscale Iron structure, forms infiltrative type interlayer film (see Fig. 1) after absorbing water.
4) magnetic testing: to Y25 (3800GS) magnet, can be less than the powder particle absorption of 0.1 millimeter.
this routine gained filtering material is to the filter effect of drinking water
1. method of testing:
Arsenic, chromium clearance: with reference to MOH " Drinking Water water quality treater safe and sanitary and functional evaluation specification-general water quality treater " & EPA200.8ICP/MS;
Mercury clearance: with reference to MOH " Drinking Water water quality treater safe and sanitary and functional evaluation specification-general water quality treater " & GB/T5750.6-2006 drinking water standard method of inspection metal index atomic fluorescence method;
Resolution chart is see Fig. 2.
2. test result: see table 1.
Table 1
stability test after this routine gained filtering material uses
According to international standard: EPA TCLP CD-ROM1311-1July1992
METHOD1311TOXICITY CHARACTERISTIC LEACHING PROCEDURE carries out simulated test.The heavy metals such as the plumbous cadmium of arsenic cadmium mercury that testing result absorption is fixing do not exceed standard or do not detect.
Above to invention has been detailed description; its object is to allow the personage being familiar with this art can understand content of the present invention and be implemented; can not limit the scope of the invention with this; the equivalence change that all Spirit Essences according to the present invention are done or modification, all should be encompassed in protection scope of the present invention.
Claims (10)
1. a filter core material of household filter, it is characterized in that: described material for core is the porous ceramic matrices suitable of 35% ~ 85% by porosity and forms at the nanometer nulvalent iron particle that the internal in-situ of described porous ceramic matrices suitable generates, the micropore size of described porous ceramic matrices suitable is 2 ~ 10 microns, and in described micropore, be formed with velvet-like unformed silicon-iron-carbon structure, velvet-like unformed silicon-iron-carbon structure in described micropore can form adsorbed film after absorbing water, with parts by weight, the material of described porous ceramic matrices suitable consists of 75 ~ 85 parts, diatomite, powdered carbon 8 ~ 10 parts, bentonite 1 ~ 3 part, kaolin 3 ~ 5 parts.
2. filter core material of household filter according to claim 1, is characterized in that: the surface of described material for core is iron cyan or cinerous, and fresh section is blue, and material for core becomes black after water suction or immersion; Below 0.1mm Y25 ferromagnetic powder can adsorb by described material for core; Described material for core is after scraping off top layer powder, and the pH measured by NY/T 1377-2007 Soil standard is 8.0 ~ 8.5.
3. filter core material of household filter according to claim 1, is characterized in that: the porosity of described porous ceramic matrices suitable is 55% ~ 70%.
4. filter core material of household filter according to claim 1, it is characterized in that: described material for core obtains by carrying out Nanoscale Iron modification to porous ceramic matrices suitable, the method of Nanoscale Iron modification is first by upper for porous ceramic matrices suitable absorption ferrous ion, recycling reducing agent carries out in-situ reducing to the ferrous ion be adsorbed on porous ceramic matrices suitable, finally porous ceramic matrices suitable is carried out anaerobic sintering at 400 DEG C ~ 500 DEG C.
5. filter core material of household filter according to claim 1, is characterized in that: described material for core is of a size of: external diameter 30 ~ 50mm, internal diameter 25 ~ 45mm, length 100 ~ 250mm.
6. a preparation method for the filter core material of household filter any one of claim 1,2,3 and 5 as described in claim, is characterized in that: comprise the steps:
(1) diatomite, bentonite, kaolin, powdered carbon are pressed formula rate mixing, at temperature 700 DEG C ~ 900 DEG C, carry out anaerobic sintering, obtain described porous ceramic matrices suitable;
(2), porous ceramic matrices suitable is dipped into pH 7.0 ~ 8.0, containing in the aqueous phase mixed liquor of ferrous ion and tackifier, after porous ceramic matrices suitable complete wetting, take out porous ceramic matrices suitable, dry for subsequent use, wherein: tackifier are one or more the combination in glucose, sucrose and soluble starch, the content of tackifier in aqueous phase mixed liquor is 0.2wt% ~ 15wt%, and the content of described ferrous ion in aqueous phase mixed liquor is 1wt% ~ 2wt%;
(3) porous ceramic matrices suitable through step (2) is immersed in pH 8.5 ~ 9.5, the aqueous solution containing sodium borohydride 2wt% ~ 3wt%, takes out after 2 ~ 8 minutes, dry for subsequent use;
(4) porous ceramic matrices suitable through step (3) is put in anaerobic stove, under nitrogen or hydrogen shield carry out anaerobic sintering; programming rate is 80 ~ 100 DEG C/h; be warming up to 300 DEG C ~ 500 DEG C, be incubated 0.5 ~ 3 hour, obtain described filter core material of household filter.
7. preparation method according to claim 6, is characterized in that: in step (2), regulate pH with natrium citricum.
8. the preparation method of filter core material of household filter according to claim 6, is characterized in that: in step (3), use winestone acid for adjusting pH.
9. preparation method according to claim 6, is characterized in that: in step (4), and sintering temperature is 380 DEG C ~ 420 DEG C.
10. preparation method according to claim 6, is characterized in that: in step (1), at temperature 750 DEG C ~ 850 DEG C, carry out anaerobic sintering.
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| WO2018058110A1 (en) * | 2016-09-26 | 2018-03-29 | Mesofilter Inc. | Filtration medium for removal or inactivation of microorganisms from water |
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| CN109476512B (en) * | 2016-06-12 | 2021-11-09 | 美索过滤公司 | Composition and method for removing arsenic and heavy metals from water |
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| CN101347717B (en) * | 2007-07-18 | 2010-05-19 | 中国科学院沈阳应用生态研究所 | Method for preparing load type nano arsenic-removing sorbent for drinking water |
| CN101486506B (en) * | 2008-01-18 | 2011-04-06 | 中国科学院沈阳应用生态研究所 | Arsenic removing apparatus for drinking water |
| CN101314496A (en) * | 2008-07-04 | 2008-12-03 | 绍兴文理学院 | Modified alta-mud loaded nano- hot metal treating agent and preparation thereof |
| CN102344194B (en) * | 2011-06-14 | 2013-01-02 | 中国科学院新疆理化技术研究所 | Method for preparing montmorillonite in situ intercalation type nanoscale zero-valent iron |
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