CN105251371A - Method for treating heavy metal sludge and preparing membranes - Google Patents
Method for treating heavy metal sludge and preparing membranes Download PDFInfo
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- CN105251371A CN105251371A CN201510705710.9A CN201510705710A CN105251371A CN 105251371 A CN105251371 A CN 105251371A CN 201510705710 A CN201510705710 A CN 201510705710A CN 105251371 A CN105251371 A CN 105251371A
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Abstract
The invention discloses a method for treating heavy metal sludge and preparing membranes. The method comprises the steps that the heavy metal sludge is mixed with bauxite clinker to obtain a mixture, after additives are added to the mixture, additives are added according to the configuration of a prepared ceramic membrane, a plate-type membrane is prepared from the prepared membrane through a tablet machine, a tubular membrane is prepared through an extruding machine, and a hollow fibrous tubular membrane is prepared through home-made wet-spinning jetting equipment; all types of prepared blank bodies are calcined at certain temperature to obtain the ceramic membranes with various types, wherein the molar ratio of heavy metal contained in the heavy metal sludge to aluminum in the bauxite clinker ranges from 1:2 to 1:8, the heavy metal sludge is taken from electroplating industry, circuit board industry, metal surface treatment industry and battery manufacturing industry. According to the method for treating the heavy metal sludge and preparing the membranes, heavy metal pollutants are prepared into functional ceramic separation membranes with a porous structure, pollution is treated in a scientific and environmentally friendly way, waste is utilized, and promotional value is achieved.
Description
Technical field
The present invention relates to heavy metal sewage sludge process field, particularly relate to and process heavy metal sewage sludge and the method preparing film.
Background technology
In recent years, along with the quick growth of China's economy and the obvious quickening of urbanization process, the ecological environment faced worsens increasingly, and the environmental problem how tackling severe contamination has been the significant challenge that Chinese society sustainable development and Ecological Civilization Construction face.Can plurality of heavy metal be produced in the industrial production, as lead, copper, magnesium, nickel, zinc etc., if these heavy metals are directly discharged in environment, the health that food chain affects the mankind and other biology can be entered, cause many diseases.In order to reduce the harm that heavy metal brings, generally adopt the way that cement solidification is buried at present, but this needs to consume a large amount of cement, takies a large amount of land resource.Comprehensive domestic and foreign literature, it is immobilization of heavy metals that scientific worker is devoted to by the form of metal hydroxides, carbonate, phosphate, sulfide and organometallic complex.These methods all achieve certain effect, but immobilized heavy metal (especially under acid condition) instability under field conditions (factors), easily again discharged, caused secondary pollution.The heavy metals such as lead, copper, zinc are successfully fixed in rich aluminium mineral such as Alpha-alumina, gama-alumina and kaolin, mullite etc. by ceramic high temperature inversion of phases by professor KaiminShih of Hong Kong University, generate more stable spinelle, there is the stability (very low leaching ability of heavy metal rate) of very high sour environment, thus realize its immobilization.But the spinelle for this generation does not have subsequent treatment and functionalized application.Simultaneously for its raw material, pure alumina price is higher, and for kaolin and mullite, owing to containing a large amount of silica in its raw material, is difficult to prepare porous ceramic film.
Summary of the invention
The object of the present invention is to provide one effectively to process heavy metal sewage sludge, and be prepared into the method for the function ceramics diffusion barrier with loose structure.
For achieving the above object, the invention provides and a kind ofly process heavy metal sewage sludge and prepare the method for film, it is characterized in that, step is mixture heavy metal sewage sludge and bauxite being mixed to get both, and this mixture prepares film after adding additive.
Further, the mol ratio of the heavy metal contained by described heavy metal sewage sludge and the aluminium in bauxite is 1:2-1:8.
Further, described heavy metal sewage sludge from electroplating industry, wiring board industry and metal finishing industry and battery manufacture industry.
Further, described film is board-like film, tubular film or doughnut tubulose film.
Further, also comprise the steps,
Shaping: mixture heavy metal sewage sludge and bauxite being mixed to get both, under gauge pressure 6MPa pressure, prepares diameter 20mm, thickness is about the round ceramic film idiosome of 1-2mm;
Calcining: the ceramic membrane idiosome prepared is placed in Muffle furnace and calcines under target temperature, heating schedule is as follows: with the speed of 3 DEG C/min from room temperature to 700-1300 DEG C; Optional, then be warming up to 1300 DEG C-1500 DEG C with the speed of 2 DEG C/min; Cooling process is, is cooled to 500-700 DEG C with the speed of 5 DEG C/min; Namely Temperature fall obtains board-like film to room temperature again.
Further, also comprise the steps,
Mixture heavy metal sewage sludge and bauxite being mixed to get both adds the iron ball that polyurethane wraps up, and dry ball milling mixing 12h, obtains mixed powder; Preferably, the mixture of described heavy metal sewage sludge and bauxite and the volume ratio of iron ball are 4:1;
Add the tung oil of 5wt%PVA as binding agent and 5wt% as plasticizer, then in powder, add 5wt% warm water mud, clay kneading machine is refined into the plastic mud material of the moisture content of 22%; Preferably, the addition of described binding agent is 5wt%PVA; The addition of described plasticizer is the tung oil of 5wt%; The addition of described warm water is 5wt% warm water;
Under high humidity environment old 3 days, guarantee that organic matter and moisture are uniformly distributed in pug, vacuum mud refining 4 times, old 2 days again, be adjusted to the size of mould, on extruder, obtained external diameter * internal diameter is respectively 14*10mm respectively, the ceramic-film tube green compact of 20*16mm, 30*24mm, 40*34mm tetra-kinds of specifications, after dry 72h, in Muffle furnace, rise to 900 DEG C of insulation 1h with 2 DEG C/min from room temperature, and then rise to target temperature 1400 DEG C with 5 DEG C/min, insulation 2h, naturally cool to room temperature, obtain earthenware supporter; Suspended particles dip coating is utilized to prepare one deck TiO at described earthenware supporter inner surface
2wet film is 80 in relative humidity, and under room temperature, drying rises to target temperature 500 DEG C for 3 days, and insulation 2h, namely cooling obtains tubular film naturally subsequently.
Further, also comprise the steps,
First PESf and NMP is mixed into solution according to the ratio of mass ratio 1:4, then adds 1-2wt.%PVP and mix, then add the mixture that heavy metal sewage sludge and bauxite are mixed to get both, planetary ball mill mixes 48 hours;
Shaping: by above-mentioned gained degassed 1 hour under vacuum, 10cm air clearance is passed through again under 0.03-0.07MPa nitrogen pressure, simultaneously using water or alcohol, NMP as inside and outside body lotion, inside and outside body lotion can be same or different, obtained hollow-fibre membrane idiosome, this idiosome soaks 24 hours in body lotion outside;
Dry: described hollow-fibre membrane idiosome is taken out rear tap water several times from solution, then dry under field conditions (factors);
Calcining: the hollow-fibre membrane idiosome of drying is placed in Muffle furnace and calcines at target temperature 1100-1500 DEG C, heating schedule is from room temperature to 700-1300 DEG C with the speed of 3 DEG C/min; Optional, then be warming up to 1300 DEG C-1500 DEG C with the speed of 2 DEG C/min, be incubated 2 hours; Cooling process is, is cooled to 500 DEG C with the speed of 5 DEG C/min; Namely Temperature fall to room temperature obtains doughnut tubulose film again.
PVA: polyvinyl alcohol; PESf: polyethersulfone resin; NMP:N-methyl pyrrolidone; PVP: polyethylene pyrrole network alkane ketone.
Porous ceramic film (as Figure 1A, Figure 1B and Fig. 1 C) can be prepared containing the heavy metal sewage sludge of nickel oxide and bauxite.In the process preparing ceramic membrane, reacted by high-temperature-phase, fixation in situ nickel oxide, generate the Ni-Al spinelle with high chemical stability completely at 1300 DEG C, obtain porous ceramic film simultaneously.This ceramic membrane materials, relative to nickel oxide, has higher acid-resistant corrosion (as Fig. 7).Meanwhile, because bauxite is except main reaction phase alumina, only have a small amount of mullite, be suitable for preparing high porosity perforated membrane.
The present invention prepares in the raw material of different film, and the amount of heavy metal sewage sludge and bauxite presses the mol ratio 1:2-1:8 of aluminium element in heavy metal ion and bauxite in heavy metal sewage sludge.Within the scope of this, to form the porosity of film high, effective.
Its pyroreaction is embedded in the crystalline phase of the ceramic membrane with environment separation function by the present invention, to reduce the environmental hazard of heavy metal.
The present invention is to reduce the environmental hazard of heavy metal for starting point, its pyroreaction is embedded in the crystalline phase of the ceramic membrane with environment separation function, to prepare low cost functional porous ceramic film, and apply it to the process (as Figure 1A, Figure 1B and Fig. 1 C) of oil-containing water quality.Carry out the research of the high-temperature phase-change mechanism of heavy metal and solid waste/mineral on the one hand, while realizing the Efficient Conversion of metal pollutant, prepare the porous ceramic film with separation function.On the other hand, in the oily waste water treatment process of inorganic ceramic membrane, pay close attention to emphatically the Process Law of membrane mass transfer process and the microcosmic effect mechanism of pollutant and ceramic membrane.The physical chemistry at research on utilization institute's instrument and equipment center and structural characterization technology, the Preparation of inorganic membrane that Binding experiment room is built and test platform, disclose Changing Pattern and the related mechanism of the main technologic parameters of ceramic membrane technology process pollutant.This project, to opening up new research direction in environmental contaminants control technology field, i.e. enviroment protective ceramic membrane technology, is applied for the environmental project realizing inorganic ceramic membrane technology and is provided Science and Technology reference.
The invention provides a kind of novel heavy metal contaminants transformation technology, heavy metal contaminants is efficiently fixed in stable ceramic junction crystalline phase, and be prepared into the function ceramics diffusion barrier with loose structure; Porous ceramics membrane separation technique is incorporated into the process of oily waste water, development " fenestra and profit system " surface physics chemistry, and explores the microcosmic effect mechanism with oil droplet in mass transport process.
Accompanying drawing explanation
Figure 1A is the board-like film pictorial diagram of nickel oxide that embodiment 1 prepares;
Figure 1B is the tubular film pictorial diagram that embodiment 2 prepares;
Fig. 1 C is the doughnut tubulose film pictorial diagram that embodiment 3 prepares;
Fig. 2 A is the porosity variation with temperature curve of the board-like film adopting containing metal nickel oxide to prepare;
Fig. 2 B is the shrinkage factor variation with temperature curve of the board-like film adopting containing metal nickel oxide to prepare;
Fig. 3 A is that embodiment 1 adopts the mol ratio of Ni:Al to be the board-like film strength of 1:4 gained heavy metal nickel and temperature results figure;
Fig. 3 B is that embodiment 3 adopts the mol ratio of Ni:Al to be 1:4 gained heavy metal nickel doughnut tubulose film strength and temperature results figure;
Fig. 4 A adopts heavy metal sewage sludge (containing NiO) and bauxite according to the pore size distribution curve of the board-like film of mol ratio Ni:Al=1:4 gained;
Fig. 4 B adopts heavy metal sewage sludge (containing NiO) and the average pore size of bauxite according to the board-like film of mol ratio Ni:Al=1:4 gained and the curve of temperature;
Fig. 5 is the XRD result figure of each phase composition of bauxite used in embodiment;
Fig. 6 A is the XRD result of the phase composition of the board-like film of embodiment 1 gained heavy metal nickel when mol ratio Ni:Al=1:2;
Fig. 6 B is that each phase content of the board-like film of embodiment 1 gained heavy metal nickel when mol ratio Ni:Al=1:2 varies with temperature result;
Fig. 7 is the nickel oxide powder under 1400 degree after calcining, and bauxite and heavy metal sewage sludge (containing NiO) are according to mol ratio Ni:Al=1:2; The powder that tabular film ball milling prepared by 1:4 becomes is at the leaching concentration figure of pH value 2.9 times copper ions;
Fig. 8 is the scanning electron microscope (SEM) photograph of board-like film prepared by 1200 DEG C-1500 DEG C fixing nickel oxide.
Detailed description of the invention
Be described below in detail embodiments of the invention, the example of described embodiment is shown in the drawings, and wherein same or similar label represents same or similar element or has element that is identical or similar functions from start to finish.Be exemplary below by the embodiment be described with reference to the drawings, be intended to for explaining the present invention, and can not limitation of the present invention be interpreted as.Unreceipted concrete technology or condition person in embodiment, according to the technology described by the document in this area or condition or carry out according to product description.Agents useful for same or the unreceipted production firm person of instrument, being can by the conventional products of commercial acquisition.
embodiment 1: the preparation of board-like film
Mixing: by heavy metal sewage sludge (containing NiO) and bauxite according to mol ratio Ni:Al=1:2; 1:4; 1:8; 0(0 represents fine aluminium bauxite clinker) ratio mixing, and add the amount interpolation 5wt%PVA aqueous solution of the 20ml5wt%PVA aqueous solution according to 100 grams of powders after, mix, at 60 DEG C of dry 2h;
Shaping: by the above-mentioned powder mixed under gauge pressure 6MPa pressure, to prepare diameter 20mm, thickness is about the round ceramic film idiosome of 1-2mm;
Calcining: the ceramic membrane idiosome prepared is placed in Muffle furnace and calcines under target temperature, heating schedule is as follows: with the speed of 3 DEG C/min from room temperature to 1300 DEG C; 1500 DEG C are warming up to from 1300 DEG C with 2 DEG C/min; Cooling process is, is cooled to target temperature 500 DEG C with 5 DEG C/min; Freely be cooled to room temperature again.When most high sintering temperature is lower than 1300 DEG C time, as 1200 DEG C, heat up with the speed of 3 DEG C/min from room temperature to 1200 DEG C, then 5 DEG C/min is down to 500 DEG C, more freely cools to room temperature.
Heavy metal sewage sludge (containing NiO) and bauxite are according to mol ratio Ni:Al=1:2; 1:4; 1:8 the results are shown in Figure 1A and Fig. 8, wherein Fig. 8 be the board-like film of nickel oxide spinelle at 1200 to 1500 DEG C, electromicroscopic photograph during multiplication factor 10,000 times, wherein (a) 1200 DEG C, (b) 1300 DEG C, (c) 1400 DEG C, (d) 1500 DEG C.Can find out, nickel aluminate starts to be formed low temperature 1200 DEG C, and the process raising with temperature and constantly grow up.
embodiment 2: the preparation of tubular film
The mixture of heavy metal sewage sludge and bauxite is added the iron ball that polyurethane wraps up, dry ball milling mixing 12h, obtains mixed powder; The amount of described heavy metal sewage sludge (containing NiO) and bauxite presses the mol ratio 1:2 of aluminium element in heavy metal ion and bauxite in heavy metal sewage sludge; The mixture of described heavy metal sewage sludge and bauxite and the volume ratio of iron ball are 4:1.
The PVA adding 5wt% as the tung oil of binding agent and 5wt% as plasticizer, then in powder, 5wt.% warm water mud is added, clay kneading machine is refined into the plastic mud material of the moisture content of 22%, within old 3 days under high humidity environment, (after water injection mix the water few evaporation as far as possible making the inside under air-proof condition afterwards, keep its humidity higher), guarantee that organic matter and moisture are uniformly distributed in pug, vacuum (0.02-0.06MPa) mud refining 4 times, under natural room temperature condition old 2 days again, be adjusted to the size of mould, on extruder, obtained size (external diameter * internal diameter) is 14*10mm respectively, 20*16mm, 30*24mm, the ceramic-film tube green compact of 40*34mm tetra-kinds of specifications, after dry 72h, in Muffle furnace, rise to 900 ° of C with 2 DEG C/min from room temperature be incubated 1h, and then rise to target temperature 1400 DEG C with 5 DEG C/min, insulation 2h, naturally cool to room temperature, obtain earthenware supporter, suspended particles dip coating is utilized to prepare one deck TiO at described earthenware supporter inner surface
2wet film is 80 in relative humidity, and under room temperature, drying rises to target temperature 500 DEG C for 3 days, and insulation 2h, namely cooling obtains tubular film naturally subsequently, sees the pictorial diagram of Figure 1B.
embodiment 3: doughnut tubulose film
Mixing: first PESf and NMP is mixed into solution according to the mass ratio of 1:4, then adds 1-2wt.%PVP, and mix, then add the heavy metallic oxide of 40-65wt.% and the mixture of bauxite, planetary ball mill mixes 48 hours; The amount of described heavy metal sewage sludge (containing NiO) and bauxite presses mol ratio 1:2 or the 1:4 of aluminium element in heavy metal ion and bauxite in heavy metal sewage sludge;
Shaping: by under above-mentioned slurry vacuum condition degassed 1 hour, then under 0.03-0.07MPa nitrogen pressure, by 10cm air clearance, simultaneously using water or other solvents as inside and outside body lotion, the hollow-fibre membrane idiosome of system, this idiosome soaks 24 hours in body lotion outside;
Dry: hollow-fibre membrane idiosome is taken out rear tap water several times from solution, then dry under field conditions (factors);
Calcining: the hollow-fibre membrane idiosome of drying is placed in Muffle furnace and calcine at target temperature 1100-1300 DEG C, heating schedule is, with the speed of 3 DEG C/min from room temperature to target temperature after be incubated 2 hours; Cooling process is, is cooled to 500 DEG C with the speed of 5 DEG C/min; Namely Temperature fall obtains hollow-fibre membrane to room temperature again, sees the pictorial diagram of Fig. 1 C.
embodiment 4: compliance test result
Porosity detects: Archimedes method, and instrument is precision electronic balance; Under different mol ratio, (metal ion and aluminium element mol ratio are 2,4,8 to the board-like film of embodiment 1 gained heavy metal nickel.Wherein 0 represent fine aluminium bauxite clinker) the results are shown in Figure 2A and Fig. 2 B.Wherein Fig. 2 A is porosity variation with temperature curve, and Fig. 2 B is shrinkage factor variation with temperature curve, and as can be seen from the figure, porosity reduces with the rising of temperature, and shrinkage factor raises with temperature and increases.Adopt heavy metal sewage sludge (containing NiO) and bauxite all higher in whole temperature range according to the porosity of the board-like film of mol ratio Ni:Al=1:4 gained, wherein 1400 degree time porosity the highest, spinelle simultaneously at this temperature generates (Fig. 6 A and Fig. 6 B) completely, intensity higher (Fig. 3 A), therefore, the board-like film of heavy metal nickel made under 1400 degree is applicable to the application in later stage.
Intensity: Biaxial flexturefirings (board-like film), three-point bending strength (hollow-fibre membrane), instrument is universal testing machine; (heavy metal sewage sludge (containing NiO) and bauxite are according to mol ratio Ni:Al=1:4 for the board-like film of embodiment 1 gained heavy metal nickel, with 0 i.e. fine aluminium alumina) the results are shown in Figure 3A, as can be seen from the figure, when low temperature 1200-1300 spends, the mol ratio of Ni:Al is that the board-like film-strength of heavy metal nickel of 1:4 is better than fine aluminium alumina, when high temperature 1400-1500 spends, its intensity declines to some extent relative to fine aluminium alumina, and both intensity all raises with temperature and increases.Embodiment 3 gained heavy metal nickel doughnut tubulose film the mol ratio of Ni:Al be 1:4 the results are shown in Figure 3B, can find out, with temperature raise, its intensity also sharply raises.
Aperture: Vesicular protein, Porosimetry; The board-like film of embodiment 1 gained heavy metal nickel (heavy metal sewage sludge (containing NiO) and bauxite according to mol ratio Ni:Al=1:4, and 0 i.e. fine aluminium alumina) the results are shown in Figure 4A and Fig. 4 B.Wherein Fig. 4 A adopts heavy metal sewage sludge (containing NiO) and bauxite according to the pore size distribution curve of the board-like film of mol ratio Ni:Al=1:4 gained, and Fig. 4 B is employing heavy metal sewage sludge (containing NiO) and the average pore size of bauxite according to the board-like film of mol ratio Ni:Al=1:4 gained and the curve of temperature.As can be seen from the figure, the average pore size of the board-like film of heavy metal nickel is all higher than the board-like film of fine aluminium alumina at different temperatures.
The crystalline phase composition of raw material and membrane material: XRD diffractometer detects; The phase composition of the bauxite used in embodiment the results are shown in Figure 5, and as can be seen from the figure, bauxite based on alumina phase, and contains a small amount of mullite phase.The phase composition of the board-like film of embodiment 1 gained heavy metal nickel when mol ratio Ni:Al=1:2 and content results are shown in Fig. 6 A and Fig. 6 B.Wherein Fig. 6 A is XRD result (S represents nickel aluminate, and M represents mullite, and A represents corundum, and N represents nickel oxide), and Fig. 6 B is that the content of each phase varies with temperature result.As can be seen from the figure, the content of nickel aluminate constantly increases with the rising of temperature, and other each phase contents all raise with temperature as aluminium oxide, nickel oxide and mullite and reduce.This illustrates that nickel aluminate is more stable than copper aluminate between high-temperature region, can not decompose again.
The leaching behavior of harmful substance Ni: harmful substance leaches standard (USEPAMethod1311).Fig. 7 is the cupric oxide powder under 1400 degree after calcining, and bauxite and heavy metal sewage sludge (containing NiO) are according to mol ratio Ni:Al=1:2; The powder that tabular film ball milling prepared by 1:4 becomes is at the leaching concentration figure of pH value 2.9 times copper ions.As can be seen from the figure, nickel aluminate stability in acid condition will be better than far away its heavy metallic oxide, illustrates that the film that the present invention prepares has higher acid-resistant corrosion.Wherein, the nickel ion leaching content of tabular film that bauxite and heavy metal sewage sludge (containing NiO) are prepared according to mol ratio Ni:Al=1:4 is less than the tabular film prepared according to mol ratio Ni:Al=1:2.Consider that the pore-forming of bauxite is effective, in preparation process, the proportioning of Ni:Al=1:4 is preferentially applicable to preparing membrane material.Therefore, with ceramic membrane prepared by the method, there is certain feasibility.
Although illustrate and describe embodiments of the invention above, be understandable that, above-described embodiment is exemplary, can not be interpreted as limitation of the present invention, those of ordinary skill in the art can change above-described embodiment within the scope of the invention when not departing from principle of the present invention and aim, revising, replacing and modification.
Claims (7)
1. process heavy metal sewage sludge and prepare the method for film, it is characterized in that, step is mixture heavy metal sewage sludge and bauxite being mixed to get both, and this mixture prepares film after adding additive.
2. process heavy metal sewage sludge described in claim 1 and prepare the method for film, it is characterized in that, the mol ratio of the aluminium in heavy metal contained in described heavy metal sewage sludge and bauxite is 1:2-1:8.
3. process heavy metal sewage sludge described in claim 1 and prepare the method for film, it is characterized in that, described heavy metal sewage sludge from electroplating industry, wiring board industry and metal finishing industry and battery manufacture industry.
4. process heavy metal sewage sludge described in claim 1 and prepare the method for film, it is characterized in that, described film is board-like film, tubular film or doughnut tubulose film.
5. process heavy metal sewage sludge described in claim 1 and prepare the method for film, it is characterized in that, also comprise the steps,
Shaping: mixture heavy metal sewage sludge and bauxite being mixed to get both, under gauge pressure 6MPa pressure, prepares diameter 20mm, thickness is about the round ceramic film idiosome of 1-2mm;
Calcining: the ceramic membrane idiosome prepared is placed in Muffle furnace and calcines under target temperature, heating schedule is as follows: with the speed of 3 DEG C/min from room temperature to 700-1300 DEG C; Optional, then be warming up to 1300 DEG C-1500 DEG C with the speed of 2 DEG C/min; Cooling process is, is cooled to 500-700 DEG C with the speed of 5 DEG C/min; Namely Temperature fall obtains board-like film to room temperature again.
6. process heavy metal sewage sludge described in claim 1 and prepare the method for film, it is characterized in that, also comprise the steps,
Mixture heavy metal sewage sludge and bauxite being mixed to get both adds the iron ball that polyurethane wraps up, and dry ball milling mixing 12h, obtains mixed powder; Preferably, the mixture of described heavy metal sewage sludge and bauxite and the volume ratio of iron ball are 4:1;
Add the tung oil of 5wt%PVA as binding agent and 5wt% as plasticizer, then in powder, add 5wt% warm water mud, clay kneading machine is refined into the plastic mud material of the moisture content of 22%; Preferably, the addition of described binding agent is 5wt%PVA; The addition of described plasticizer is the tung oil of 5wt%; The addition of described warm water is 5wt% warm water;
Under high humidity environment old 3 days, guarantee that organic matter and moisture are uniformly distributed in pug, vacuum mud refining 4 times, old 2 days again, be adjusted to the size of mould, on extruder, obtained external diameter * internal diameter is respectively 14*10mm respectively, the ceramic-film tube green compact of 20*16mm, 30*24mm, 40*34mm tetra-kinds of specifications, after dry 72h, in Muffle furnace, rise to 900 DEG C of insulation 1h with 2 DEG C/min from room temperature, and then rise to target temperature 1400 DEG C with 5 DEG C/min, insulation 2h, naturally cool to room temperature, obtain earthenware supporter; Suspended particles dip coating is utilized to prepare one deck TiO at described earthenware supporter inner surface
2wet film is 80 in relative humidity, and under room temperature, drying rises to target temperature 500 DEG C for 3 days, and insulation 2h, namely cooling obtains tubular film naturally subsequently.
7. process heavy metal sewage sludge described in claim 1 and prepare the method for film, it is characterized in that, also comprise the steps,
First PESf and NMP is mixed into solution according to the ratio of mass ratio 1:4, then adds 1-2wt.%PVP and mix, then add the mixture that heavy metal sewage sludge and bauxite are mixed to get both, planetary ball mill mixes 48 hours;
Shaping: by above-mentioned gained degassed 1 hour under vacuum, 10cm air clearance is passed through again under 0.03-0.07MPa nitrogen pressure, simultaneously using water or alcohol, NMP as inside and outside body lotion, inside and outside body lotion can be same or different, obtained hollow-fibre membrane idiosome, this idiosome soaks 24 hours in body lotion outside;
Dry: described hollow-fibre membrane idiosome is taken out rear tap water several times from solution, then dry under field conditions (factors);
Calcining: the hollow-fibre membrane idiosome of drying is placed in Muffle furnace and calcines at target temperature 1100-1500 DEG C, heating schedule is from room temperature to 700-1300 DEG C with the speed of 3 DEG C/min; Optional, then be warming up to 1300 DEG C-1500 DEG C with the speed of 2 DEG C/min, be incubated 2 hours; Cooling process is, is cooled to 500 DEG C with the speed of 5 DEG C/min; Namely Temperature fall to room temperature obtains doughnut tubulose film again.
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| CN106316359A (en) * | 2016-08-09 | 2017-01-11 | 北京市自来水集团有限责任公司技术研究院 | Method for preparing ceramic membrane supporting body from water purification plant sludge and prepared ceramic membrane supporting body |
| CN111747774A (en) * | 2020-07-10 | 2020-10-09 | 武汉理工大学 | Red mud ceramic membrane support and preparation method and application thereof |
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