CN103084072A - Method for preparing hollow fiber ceramic membrane from tantalum-niobium mine tailings - Google Patents
Method for preparing hollow fiber ceramic membrane from tantalum-niobium mine tailings Download PDFInfo
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Abstract
The invention belongs to the field of recycling comprehensive utilization of ore dressing solid waste and preparation of hollow fiber ceramic membrane, and provides a method for preparing a hollow fiber ceramic membrane from tantalum-niobium mine tailings. The hollow fiber ceramic membrane comprises the following components: 30-73 parts of tantalum-niobium mine tailings powder, 5-20 parts of polymer binder, 1.5-7 parts of structural control additive, 20-42 parts of solvent and 0.5-1 part of powder particle dispersant. A nascent-state hollow fiber ceramic membrane blank is prepared through material preparation, high-temperature dissolution, vacuum defoaming and dry spraying-wet spinning conversion, wherein the inner diameter of the membrane blank is 1.5-2mm, and the outer diameter is 2.5-3.4mm. The nascent-state hollow fiber ceramic membrane blank is subjected to a specific sintering technology in a muffle furnace to obtain a hollow fiber ceramic membrane. The inner diameter of the hollow fiber ceramic membrane is 1.0-1.5mm, the outer diameter is 1.9-3.0mm, the length is 200-500mm, the porosity is 50-65%, the pure water flux reaches 200-500L/m2.H@0.1MPa, and the pore diameter is 0.2-0.4 microns.
Description
Technical field
The present invention relates to a kind of method for preparing hollow fiber ceramic membrane, relate in particular to a kind of method of utilizing tantalum niobium CHARACTERISTICS OF TAILINGS SAND to prepare hollow fiber ceramic membrane.
Background technology
The lepidolite that the tantalum niobium concentrate association is a large amount of, feldspar and kaolin.After the ore-dressing techniques such as the fragmentation of ore process, screening, gravity treatment, flotation, magnetic separation; after sorting out the valuable minerals such as tantalum-niobium concentrate, lepidolite, feldspar and kaolin; also have a large amount of particulate feldspar powders, mica and kaolin to flow into Tailings Dam, through storing up in Tailings Dam after gravitational settling.Due to the Tailings Dam limited space, the new method of therefore seeking new tantalum niobium CHARACTERISTICS OF TAILINGS SAND comprehensive utilization of resources realizes minimizing, the resource and innoxious of solid waste having very important environmental benefit and economic benefit.
The Main Ingredients and Appearance of these CHARACTERISTICS OF TAILINGS SAND is common raw materials of preparation pottery, but wherein contains the heavy metal element of trace, and during as ceramic raw material, the product of firing can produce the black flaw, affects product quality, so this CHARACTERISTICS OF TAILINGS SAND is difficult to the application in ceramics factory.
It is high that ceramic membrane has intensity, and anti-exceedingly odious condition is widely used in wastewater treatment, and medicine separates, food separation and purifying, the fields such as molten steel filtration.Commodity ceramic membrane great majority are multichannel at present, and this ceramic membrane exists packing density low, see through runner long, are difficult to the shortcomings such as recovery after pollution.In recent years, utilize Al
2O
3The research that powder prepares similar polymer hollow tunica fibrosa extensively launches, due to Al
2O
3The powder price is more expensive, and the reasons such as sintering temperature height cause these ceramic membrane preparation costs higher, and therefore seeking cheap ceramic membrane raw material and reducing sintering temperature is to reduce the striving direction of ceramic membrane production cost.
Contain abundant lepidolite in tantalum niobium CHARACTERISTICS OF TAILINGS SAND, the application of lepidolite in a small amount of patent report comprehensive utilization tantalum niobium CHARACTERISTICS OF TAILINGS SAND is arranged in recent years.For example: FLOTATION SEPARATION lepidolite concentrate (201110025088.9) from tantalum niobium mine tailing; Utilize tantalum niobium tailings lepidolite to prepare aluminium cesium sulfate, aluminium rubidium sulfate (201110026383.6); Utilize tantalum niobium tailings lepidolite to prepare lithium carbonate defluorination (201110026401.0); Utilize tantalum niobium tailings lepidolite to prepare alum (201110026411.4) etc.And to the feldspar in tantalum niobium CHARACTERISTICS OF TAILINGS SAND, the comprehensive utilization of other nonmetallic ores such as kaolin has no relevant report.And Jiang Yuhua etc. have reported a kind of alumina-based ceramic doughnut preparation method (201010264781.7).Therefore the present invention is in conjunction with the preparation method of hollow-fibre membrane, and intending selecting tantalum niobium CHARACTERISTICS OF TAILINGS SAND is raw material, adopts dried wetting phase conversion-sintering process to prepare hollow fiber ceramic membrane.
Summary of the invention
The objective of the invention is a kind of tantalum niobium concentrate that fully utilizes and selected the CHARACTERISTICS OF TAILINGS SAND that produces after tantalum-niobium concentrate, lepidolite, feldspar and kaolin, prepare hollow fiber ceramic membrane with it as raw material.Have cost of material cheap, sintering temperature is low, and energy consumption is low; It is high that the hollow fiber ceramic membrane finished product that makes has porosity, and water flux is large, and mechanical strength is high, has pack completeness by the hollow fiber ceramic membrane assembly of its encapsulation high, and the film surface area is large, the advantages such as applicable exceedingly odious condition.
The present invention proposes a kind of new method that fully utilizes tantalum niobium CHARACTERISTICS OF TAILINGS SAND-preparation hollow fiber ceramic membrane, its concrete steps are as follows:
1, tantalum niobium CHARACTERISTICS OF TAILINGS SAND is first used the drying box drying after, then the sieve with different pore size carries out classification, more varigrained CHARACTERISTICS OF TAILINGS SAND powder is carried out grating, obtains the ceramic membrane powder material;
2, polymeric binder, structure control additive and solvent are added together in the dissolving tank of band stirring, obtained casting solution at 30-80 ℃ of stirring and dissolving 4-24 hour;
3, again the ceramic membrane powder material in step 1 and powder particle dispersant are joined in the prepared casting solution of step 2, mechanical agitation 10-24 hour, owing to having prevented the sedimentation of particle in casting solution adding of powder particle dispersant, obtain the nascent state film spinning solution of homogeneous, the spinning solution temperature range is 30～60 ℃; Nascent state film spinning solution after vacuum defoamation at N
2Under pressure-acting, extrude in the annular space by the lantern ring type spinneret, behind the air gap, enter in the running water gel media inversion of phases occurs, obtain nascent state hollow-fibre membrane ceramic membrane, spinneret pump seat temperature range is 20～50 ℃; The nascent state hollow fiber ceramic membrane soaks 10-24 hour in running water after, more natural drying in air, obtain nascent state hollow fiber ceramic membrane idiosome;
4, the prepared nascent state hollow fiber ceramic membrane of step 3 idiosome is put into Muffle furnace, carries out sintering according to following sintering process: first rise to 200 ℃ with 2～5 ℃/min programming rate, and be incubated 0.5～1 hour under 200 ℃; Be increased to 500 ℃ with 1～3 ℃/min programming rate again, and be incubated 1～2 hour; Be increased to 900 ℃ with 1～2 ℃/min programming rate again, be incubated 4～6 hours under 900 ℃; Be increased to 1400 ℃ with 2～5 ℃/min again, be incubated 2～4 hours; Be reduced to 10～35 ℃ with 1～5 ℃/min rate of temperature fall at last, obtain hollow fiber ceramic membrane.
Described CHARACTERISTICS OF TAILINGS SAND main component is: lepidolite, thick feldspar, elongated stone, ultra-fine feldspar powder and kaolin etc.
Described organic solvent is DMF, DMA, METHYLPYRROLIDONE, the mixture of any one or a few in dimethyl sulfoxide (DMSO) and chloroform.
Described polymeric binder is any one or a few the mixture in polysulfones, polyether sulfone, cellulose acetate, polyacrylonitrile or Kynoar.
Described structure control additive is polyvinyl alcohol, polyethylene glycol, poly, polyethylene glycol oxide, any one in polyvinylpyrrolidone, PLA or several mixtures.
Described powder particle dispersant is Span60, Span80, oligomeric phosphoric acid sodium, dodecyl sodium sulfate, one or more mixtures in dodecyl quaternary ammonium salt and bay ether.
In described polymer solution, to account for the mass fraction of gross weight be 5%～20% to polymeric binder.
In described spinning solution, to account for the scope of the mass percent of gross weight be 30%～73% to powder.
The mass fraction that described solvent accounts for gross weight is 20%～42%.
Described structure control additive account for gross weight mass fraction be 1.5%～7%.
Described powder particle dispersant account for gross weight mass fraction be 0.5%～1%.
Described nascent state film spinning solution makes the nascent state hollow fiber ceramic membrane through the inversion of phases technique of overdrying spray-wet spinning, and the outer gel media distance of spinneret distance is 0～20cm.
Described outer gel media is running water, and temperature range is 20～50 ℃.
In described spinneret, the inner gel medium is deionized water, and temperature range is 20～50 ℃.
The described nascent state hollow-fibre membrane of making soaked in the running water of 20～50 ℃ 10～24 hours.
Described nascent state hollow fiber ceramic membrane obtains nascent state hollow fiber ceramic membrane idiosome after super-dry, adopt following sintering process in Muffle furnace: first rise to 200 ℃ with 2～5 ℃/min programming rate, and be incubated 0.5～1 hour under 200 ℃; Be increased to 500 ℃ with 1～3 ℃/min programming rate again, and be incubated 1～2 hour; Be increased to 900 ℃ with 1～2 ℃/min programming rate again, be incubated 4～6 hours under 900 ℃; Be increased to 1400 ℃ with 2～5 ℃/min again, be incubated 2～4 hours; Be reduced to 10～35 ℃ with 1～5 ℃/min rate of temperature fall at last, obtain hollow fiber ceramic membrane.
Do spray-wet spinning inversion of phases and prepare nascent state hollow fiber ceramic membrane idiosome, film idiosome specification is internal diameter 1.5-2mm, external diameter 2.5-3.4mm.Nascent state hollow ceramic membranes idiosome Muffle furnace makes hollow fiber ceramic membrane through specific sintering process.This hollow fiber ceramic membrane internal diameter 1.0-1.5mm, external diameter is 1.9-3.0mm, long 200-500mm, porosity is 50～65%, pure water flux reaches 200-500L/m
2.H@0.1MPa, pore size is 0.2-0.4um.
Technique effect of the present invention is: the raw material that tantalum niobium CHARACTERISTICS OF TAILINGS SAND is prepared as hollow fiber ceramic membrane of the invention, and sintering temperature is low, and energy consumption is low, preparation cost is low.Can realize on the one hand the comprehensive recycling of discarded tailing sand resource-turn waste into wealth; The hollow fiber ceramic membrane of preparation has that high temperature resistant, resistance to chemical attack, mechanical strength are high on the other hand, the even narrowly distributing in aperture, microstructure are controlled, long service life, loading density is large, membranous wall is thin, the permeation flux advantages of higher.
Description of drawings
Fig. 1 is nascent state hollow fiber ceramic membrane idiosome cross section whole and part enlarged drawing (before sintering).
Fig. 2 is hollow fiber ceramic membrane cross section and outer surface shape appearance figure (after sintering).
The specific embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1
(1) with the 27.9g polyether sulfone, 0.837g sodium phosphate trimer, 4.022g polyvinylpyrrolidone (K90) and 1.003g polyethylene glycol add 94gN, in N-dimethylacetylamide and 10g chloroform mixed solvent, stirred 24 hours in the thermostat water bath of 60 ℃, obtain casting solution.
(2) the tantalum niobium CHARACTERISTICS OF TAILINGS SAND that 151.22g is prepared adds in above-mentioned casting solution, adds simultaneously 0.05gSpan60 and 1.042g dodecyl sodium sulfate, stirs 12 hours in the thermostat water bath of 60 ℃, obtains disperseing the film precursor solution of homogeneous.After vacuum defoamation 2 hours, at N
2Spinneret via special construction under pressure-acting is extruded, enter through 10cm air distance in the running water of 30 ℃, the deionized water that spinneret is inner logical 30 ℃, form the nascent state hollow fiber ceramic membrane under the acting in conjunction of inner deionized water and outside running water, soak after 24 hours in 30 ℃ of running water, taking-up is the natural drying nascent state hollow fiber ceramic membrane idiosome that obtains in air, and microstructure is seen accompanying drawing 1.
(3) the nascent state doughnut pottery idiosome that makes is put into Muffle furnace, carry out sintering according to following sintering circuit, first the heating rate with 2 ℃/min was increased to 200 ℃, 200 ℃ of insulations 0.5 hour; Be warming up to 500 ℃ with 1 ℃/min again, 500 ℃ of insulations 1 hour; Be warming up to and 900 ℃ with 2 ℃/min, insulation is 4 hours under 900 ℃ again; Be warming up to 1200 ℃ with 3 ℃/min at last, 1400 ℃ of insulations 2 hours; Be cooled to 10～35 ℃ with 5 ℃/min at last, obtain hollow fiber ceramic membrane.Porosity is 65%, and pure water flux reaches 480 L/m
2.H@0.1MPa, pore size is 0.35um.
Hollow fiber ceramic membrane cross section whole and part structure is seen accompanying drawing 2.
Embodiment 2
With the 35.3g polysulfones, 4.42g cetomacrogol 1000 and 1.003g PEG400 add in the 94g METHYLPYRROLIDONE, stir 24 hours in the thermostat water bath of 25 ℃, obtain casting solution.Then add 191.6g tantalum niobium CHARACTERISTICS OF TAILINGS SAND powder, after 0.25gSpan80 and 1.452g oligomeric phosphoric acid sodium, stirred 12 hours in the thermostat water bath of 50 ℃, vacuum defoamation is after 2 hours, at N
2Spinneret via special construction under pressure-acting is extruded, enter through 20cm air distance in the running water of 30 ℃, the deionized water that spinneret is inner logical 30 ℃, form the nascent state hollow fiber ceramic membrane under the acting in conjunction of inner deionized water and outside running water, soak in 30 ℃ of running water after 24 hours, take out the natural drying nascent state hollow fiber ceramic membrane idiosome that obtains in air.The hollow fiber ceramic membrane idiosome carries out sintering according to following sintering circuit: first the heating rate with 2 ℃/min was increased to 200 ℃, 200 ℃ of insulations 1 hour; Be warming up to 500 ℃ with 1 ℃/min again, 500 ℃ of insulations 1.5 hours; Be warming up to and 900 ℃ with 2 ℃/min, insulation is 5 hours under 900 ℃ again; Be warming up to 1200 ℃ with 3 ℃/min at last, 1400 ℃ of insulations 3 hours; Be cooled to 10～35 ℃ with 5 ℃/min at last, obtain hollow fiber ceramic membrane.Porosity is 50%, and pure water flux reaches 257 L/m
2.H@0.1MPa, pore size is 0.21um.
Embodiment 3
With the 40.3g polyacrylonitrile, 4.42g PEG400 and 1.003g polyvinylpyrrolidone (K30) add 100gN, in dinethylformamide, stir 24 hours in the thermostat water bath of 30 ℃, obtain casting solution.Then add 171.6g tantalum niobium CHARACTERISTICS OF TAILINGS SAND powder, the 1.126g dodecyl sodium sulfate after 0.33g bay ether, stirred 12 hours in the thermostat water bath of 30 ℃, and vacuum defoamation is after 2 hours, at N
2Spinneret via special construction under pressure-acting is extruded, enter through 0cm air distance in the running water of 30 ℃, the deionized water that spinneret is inner logical 30 ℃, form the nascent state hollow fiber ceramic membrane under the acting in conjunction of inner deionized water and outside running water, soak in 30 ℃ of running water after 24 hours, take out the natural drying nascent state hollow fiber ceramic membrane idiosome that obtains in air.The hollow fiber ceramic membrane idiosome carries out sintering according to following sintering circuit: first the heating rate with 2 ℃/min was increased to 200 ℃, 200 ℃ of insulations 1 hour; Be warming up to 500 ℃ with 1 ℃/min again, 500 ℃ of insulations 2 hours; Be warming up to and 900 ℃ with 2 ℃/min, insulation is 6 hours under 900 ℃ again; Be warming up to 1200 ℃ with 3 ℃/min at last, 1400 ℃ of insulations 4 hours; Be cooled to 10～35 ℃ with 5 ℃/min at last, obtain hollow fiber ceramic membrane.Porosity is 53%, and pure water flux reaches 355L/m
2.H@0.1MPa, pore size is 0.28um.
Claims (9)
1. method of utilizing tantalum niobium CHARACTERISTICS OF TAILINGS SAND to prepare hollow fiber ceramic membrane is characterized in that the preparation method is as follows:
1) tantalum niobium CHARACTERISTICS OF TAILINGS SAND is first used the drying box drying after, then the sieve with different pore size carries out classification, more varigrained CHARACTERISTICS OF TAILINGS SAND powder is carried out grating, obtains the ceramic membrane powder material;
2) polymeric binder, structure control additive and solvent are added together in the dissolving tank of band stirring, obtained casting solution at 30-80 ℃ of stirring and dissolving 4-24 hour;
3) again the ceramic membrane powder material in step 1 and powder particle dispersant are joined in the prepared casting solution of step 2, mechanical agitation 10-24 hour, owing to having prevented the sedimentation of particle in casting solution adding of powder particle dispersant, obtain the nascent state film spinning solution of homogeneous, the spinning solution temperature range is 30～60 ℃; Nascent state film spinning solution after vacuum defoamation at N
2Under pressure-acting, extrude in the annular space by the lantern ring type spinneret, behind the air gap, enter in the running water gel media inversion of phases occurs, obtain nascent state hollow-fibre membrane ceramic membrane, spinneret pump seat temperature range is 20～50 ℃; The nascent state hollow fiber ceramic membrane soaks 10-24 hour in running water after, more natural drying in air, obtain nascent state hollow fiber ceramic membrane idiosome;
4) the prepared nascent state hollow fiber ceramic membrane of step 3 idiosome is put into Muffle furnace, carries out sintering according to following sintering process: first rise to 200 ℃ with 2～5 ℃/min programming rate, and be incubated 0.5～1 hour under 200 ℃; Be increased to 500 ℃ with 1～3 ℃/min programming rate again, and be incubated 1～2 hour; Be increased to 900 ℃ with 1～2 ℃/min programming rate again, be incubated 4～6 hours under 900 ℃; Be increased to 1400 ℃ with 2～5 ℃/min again, be incubated 2～4 hours; Be reduced to 10～35 ℃ with 1～5 ℃/min rate of temperature fall at last, obtain hollow fiber ceramic membrane.
2. a kind of method of utilizing tantalum niobium CHARACTERISTICS OF TAILINGS SAND to prepare hollow fiber ceramic membrane according to claim 1, is characterized in that described CHARACTERISTICS OF TAILINGS SAND main component is: lepidolite, thick feldspar, elongated stone, ultra-fine feldspar powder and kaolin etc.
3. a kind of method of utilizing tantalum niobium CHARACTERISTICS OF TAILINGS SAND to prepare hollow fiber ceramic membrane according to claim 1, it is characterized in that described organic solvent is N, dinethylformamide, N, the N-dimethylacetylamide, METHYLPYRROLIDONE, the mixture of any one or a few in dimethyl sulfoxide (DMSO) and chloroform.
4. a kind of method of utilizing tantalum niobium CHARACTERISTICS OF TAILINGS SAND to prepare hollow fiber ceramic membrane according to claim 1 is characterized in that described polymeric binder is any one or a few the mixture in polysulfones, polyether sulfone, cellulose acetate, polyacrylonitrile or Kynoar.
5. a kind of method of utilizing tantalum niobium CHARACTERISTICS OF TAILINGS SAND to prepare hollow fiber ceramic membrane according to claim 1, it is characterized in that described structure control additive is polyvinyl alcohol, polyethylene glycol, poly, polyethylene glycol oxide, any one in polyvinylpyrrolidone, PLA or several mixtures.
6. a kind of method of utilizing tantalum niobium CHARACTERISTICS OF TAILINGS SAND to prepare hollow fiber ceramic membrane according to claim 1, it is characterized in that described powder particle dispersant is Span60, Span80, oligomeric phosphoric acid sodium, dodecyl sodium sulfate, one or more mixtures in dodecyl quaternary ammonium salt and bay ether.
7. a kind of method of utilizing tantalum niobium CHARACTERISTICS OF TAILINGS SAND to prepare hollow fiber ceramic membrane according to claim 1 is characterized in that the mass fraction that polymeric binder in described polymer solution accounts for gross weight is 5%～20%; The scope that powder accounts for the mass percent of gross weight is 30%～73%; The mass fraction that solvent accounts for gross weight is 20%～42%; The structure control additive account for gross weight mass fraction be 1.5%～7%; The powder particle dispersant account for gross weight mass fraction be 0.5%～1%.
8. a kind of method of utilizing tantalum niobium CHARACTERISTICS OF TAILINGS SAND to prepare hollow fiber ceramic membrane according to claim 1, it is characterized in that described nascent state film spinning solution makes the nascent state hollow fiber ceramic membrane through the inversion of phases technique of overdrying spray-wet spinning, the outer gel media distance of spinneret distance is 0～20cm; Outer gel media is running water, and temperature range is 20～50 ℃; The inner gel medium is deionized water, and temperature range is 20～50 ℃; The nascent state hollow-fibre membrane soaked in the running water of 20～50 ℃ 10～24 hours.
9. a kind of method of utilizing tantalum niobium CHARACTERISTICS OF TAILINGS SAND to prepare hollow fiber ceramic membrane according to claim 1, it is characterized in that described nascent state hollow fiber ceramic membrane obtains nascent state hollow fiber ceramic membrane idiosome after super-dry, adopt following sintering process in Muffle furnace: first rise to 200 ℃ with 2～5 ℃/min programming rate, and be incubated 0.5～1 hour under 200 ℃; Be increased to 500 ℃ with 1～3 ℃/min programming rate again, and be incubated 1～2 hour; Be increased to 900 ℃ with 1～2 ℃/min programming rate again, be incubated 4～6 hours under 900 ℃; Be increased to 1400 ℃ with 2～5 ℃/min again, be incubated 2～4 hours; Be reduced to 10～35 ℃ with 1～5 ℃/min rate of temperature fall at last, obtain hollow fiber ceramic membrane.
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| CN108977927A (en) * | 2018-05-30 | 2018-12-11 | 南昌航空大学 | A kind of nano-tailings sand hollow fiber damping material and preparation method thereof |
| CN110526683A (en) * | 2019-08-28 | 2019-12-03 | 洛阳北玻硅巢技术有限公司 | A method of the composite foamed ceramic thermal insulation plate of crystallite is prepared using Ta Nb tailings |
| CN112960858A (en) * | 2021-02-18 | 2021-06-15 | 杭州楠大环保科技有限公司 | Sewage treatment process based on hollow fiber membrane |
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| CN112960858A (en) * | 2021-02-18 | 2021-06-15 | 杭州楠大环保科技有限公司 | Sewage treatment process based on hollow fiber membrane |
| CN112960858B (en) * | 2021-02-18 | 2022-05-24 | 杭州楠大环保科技有限公司 | Sewage treatment process based on hollow fiber membrane |
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