CN109351205A - A kind of silicon-oxygen-carbon ceramic hollow-fibre membrane and preparation method thereof - Google Patents
A kind of silicon-oxygen-carbon ceramic hollow-fibre membrane and preparation method thereof Download PDFInfo
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- CN109351205A CN109351205A CN201811095139.3A CN201811095139A CN109351205A CN 109351205 A CN109351205 A CN 109351205A CN 201811095139 A CN201811095139 A CN 201811095139A CN 109351205 A CN109351205 A CN 109351205A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/024—Oxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0039—Inorganic membrane manufacture
- B01D67/0044—Inorganic membrane manufacture by chemical reaction
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/08—Hollow fibre membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
- B01D69/125—In situ manufacturing by polymerisation, polycondensation, cross-linking or chemical reaction
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
Abstract
The invention belongs to separate technical field of membrane, and in particular to a kind of silicon-oxygen-carbon ceramic hollow-fibre membrane and preparation method thereof.Silicon-oxygen-carbon ceramic hollow fiber composite membrane of the invention, including silicon-oxygen-carbon ceramic separating layer and macropore ceramic supporting body, preparation method include: that (1) prepares ceramic powder-polymer solution；(2) casting solution made from step (1) prepares supporter；(3) polysiloxanes colloidal sol is prepared；(4) supporter made from step (2) is immersed in polysiloxane solution made from step (3) and silicon-oxygen-carbon ceramic hollow fiber composite membrane is made.The silicon-oxygen-carbon ceramic hollow fiber composite membrane of unsymmetric structure of the invention realizes the accuracy controlling to aperture structure, reduces ceramic membrane preparation cost, improve the acid-proof alkaline of ceramic die by applying silicon-oxygen-carbon ceramic breakcoating in macropore ceramic supporting body.
Description
Technical field
The invention belongs to separate technical field of membrane, and in particular to a kind of silicon-oxygen-carbon ceramic hollow-fibre membrane and its preparation side
Method.
Background technique
In recent years, as social economy continues to develop, industrial wastewater is increasingly severe to the destruction of water body environment, is increasingly becoming
One global problem urgently to be resolved.Membrane separation technique is a kind of novel environmental improvement means, utilizes the energy of film two sides
The selective penetrated property of difference or film itself realizes separation to mixture, and extracts, purifies to product, being concentrated, being classified or rich
Collection has many advantages, such as that system is simple and convenient to operate, separative efficiency is high, energy conservation and environmental protection.
Ceramic hollow fibrous membrane has excellent high-temperature stability, chemical stability, mechanical stability, big specific surface
Product, high separative efficiency, water process, gas separation, liquid separation, membrane reactor, in terms of have important answer
With.Traditional hollow fiber ceramic membrane preparation process need to be applied repeatedly with high temperature sintering so that graded pore structure is made to improve
Separating effect.This process significantly improves complex process degree and preparation cost, is unfavorable for realizing and commercially produces and apply.Pass through
Phase inversion can simplify preparation process, and ceramic hollow fibrous membrane is made in a step, low in cost.Patent CN200710113478.5 is public
The preparation method for having opened a kind of composite structural ceramic hollow fiber membrane is made pottery by adding ceramic seperated be made in a polymer solution
Porcelain-polymer paste, then above-mentioned slurry is spun into solidification in solidification liquid by spinning head and obtains the primary film of doughnut, most pass through afterwards
Specific program is sintered to obtain the ceramic hollow fibrous membrane of composite construction.Though above-mentioned technique can simplify part preparation process, but still have
There are follow-up sintering temperature height, the deficiencies such as ceramic membrane aperture is big, and filtering accuracy is low.Patent CN100460358C discloses a kind of utilization
Porous oxidation template is purchased the preparation method of high-specific surface area siloxicon ceramic nano-tube.But this method need to be removed with pickling and be aoxidized
Aluminum alloy pattern plate, time and effort consuming.
Though existing dry-wet spinning technique simplifies ceramic membrane preparation engineering, high temperature sintering is still needed to assign ceramic membrane foot
Enough mechanical strengths, the process significantly improve preparation cost, and ceramic membrane aperture structure easy to damage, aperture are made to be difficult to accurately control
System reduces separating effect.
Summary of the invention
In consideration of it, multiple it is necessary to provide a kind of silicon-oxygen-carbon ceramic doughnut with unsymmetric structure regarding to the issue above
Close the preparation method of film.Obtain that there is fine pore structure by applying silicon-oxygen-carbon ceramic breakcoating in macropore ceramic supporting body
Silicon-oxygen-carbon ceramic composite membrane realizes being precisely controlled for pore structure while reducing ceramic membrane preparation cost.
The present invention is achieved by the following technical solutions:
A kind of silicon-oxygen-carbon ceramic hollow fiber composite membrane, including silicon-oxygen-carbon ceramic separating layer and macropore ceramic supporting body.
A kind of preparation method of silicon-oxygen-carbon ceramic hollow fiber composite membrane, comprising the following steps:
(1) ceramic powder-polymer solution is prepared；
(2) casting solution made from step (1) prepares supporter；
(3) polysiloxane solution is prepared；
(4) supporter made from step (2) is immersed in polysiloxane solution made from step (3) and silicon oxygen carbon pottery is made
Porcelain hollow fiber composite membrane.
Further, the step (1) prepares ceramic powder-polymer solution, and concrete operations include: by polyether sulfone and to gather
Vinylpyrrolidone, which is dissolved in N-Methyl pyrrolidone solvent, forms polymer solution, and ceramic powder and sintering aid is then added
And be sufficiently stirred 10~50 hours, so that ceramic powder and sintering aid are dispersed in polymer solution and form casting solution；
By casting solution vacuum defoamation 0~2 hour, place spare.
Further, the step (1) prepares ceramic powder-polymer solution, the mass percent of each component are as follows: polyethers
10~30wt% of sulfone, 0.1~2wt% of polyvinylpyrrolidone, 20~40wt% of N-Methyl pyrrolidone, ceramic powder 30~
50wt%, 0~1.5wt% of sintering aid；The sum of weight percent of each component is 100%.
It further, is Zirconium powder as the ceramic powder of ceramic aggregate, diameter of particle selects two kinds of sizes of size,
Little particle diameter of particle range is 10-50nm, and bulky grain powder particle size range is 100-750nm；Sintering aid is Fe2O3。
Further, step (2) supporter preparation, concrete operations include: by casting solution made from step (1) and interior
(in interfacial contact liquid-liquid exchange occurs for solidification liquid.So that casting solution occurs split-phase and forms pore structure) it is squeezed out through spinneret, pass through
The air gap enters in outer solidification liquid (effect is with interior solidification liquid), and ceramic supporting body green body is made in standing and drying；By base obtained
Ceramic supporting body is made through being sintered in body.
Further, the interior solidification liquid is deionized water or alcohols；The outer solidification liquid is deionized water or alcohols.
Further, the speed that the casting solution and interior solidification liquid are squeezed out through spinneret is 3cm/s.
Further, the length of the casting solution and interior solidification liquid after spinneret squeezes out by the air gap is 15cm.
Further, the sintering process are as follows: first rise to 300 DEG C from room temperature with 1-5 DEG C/min, then with 1-5 DEG C/min after
It is continuous to be warming up to 400-600 DEG C, then be warming up to 900-1300 DEG C with 1-5 DEG C/min and keep the temperature 4 hours, finally cool down.
Preferably, the sintering process are as follows: first rise to 300 DEG C from room temperature with 5 DEG C/min, then continue to heat up with 5 DEG C/min
To 600 DEG C, then with DEG C/min be warming up to 1150 DEG C and keep the temperature 4 hours, finally cool down.
Further, the step (3) prepares polysiloxanes colloidal sol, and concrete operations include: by polysiloxanes and pore creating material
It is mixed and stirred for 0~2 hour, stand for standby use.Wherein, the polysiloxanes is MK resin, polymethyl hydrogen siloxane or tetramethyl
One or more of tetravinyl cyclotetrasiloxane；The pore creating material is dimethicone, ethenyl blocking poly dimethyl silicon
One or more of oxygen alkane or 201 methyl-silicone oils；The sum of weight percent of the polysiloxanes and pore creating material is 100%.
Further, in the polysiloxanes colloidal sol each component content range are as follows: 0~70wt% of MK resin；Poly- methyl
30~80wt% of hydrogen siloxane；30~80wt% of t etram-ethyltetravinylcyclotetrasiloxane；0~50wt% of dimethicone；Second
Alkenyl blocks 0~50wt% of dimethyl silicone polymer；201 0~50wt% of methyl-silicone oil.
Further, step (4) concrete operations include: that supporter made from step (2) is immersed in step (3) system
0~30s in the polysiloxane solution obtained reacts 10~120min in 60~70 DEG C of baking oven, then lazy at 700~1000 DEG C
Property atmosphere in be heat-treated 1~4h, repeating above-mentioned " dipping-baking oven reaction-heat treatment " process 1-5 time is to obtain in silicon-oxygen-carbon ceramic
Hollow fiber composite membrane.
The invention has the advantages that:
The present invention provides the preparation methods of silicon-oxygen-carbon ceramic hollow fiber composite membrane, are pore-creating using flexible methyl-silicone oil
Agent, on hollow ceramic supporter coating have can control accurate nano grade pore gauge structure silicon oxygen carbon separating layer.The invention
Ceramic membrane sintering temperature can be significantly reduced to reduce film preparation cost, while improving the control to membrane aperture, improve separation essence
Degree.
The silicon-oxygen-carbon ceramic hollow fiber composite membrane of unsymmetric structure of the invention, by being applied in macropore ceramic supporting body
Silicon-oxygen-carbon ceramic breakcoating realizes the accuracy controlling to aperture structure, reduces ceramic membrane preparation cost, improves the resistance to of ceramic die
Soda acid performance.
Detailed description of the invention
Fig. 1 is the cross-sectional scans electron microscope of ceramic supporting body of the present invention.
Fig. 2 is the scanning electron microscope (SEM) photograph of silicon oxygen carbon coating of the present invention.
Specific embodiment
Technical solution problem to be solved, the technical solution of use and reach beneficial in order to better illustrate the present invention
Effect is further described now in conjunction with specific embodiment.It is worth noting that technical solution of the present invention is including but not limited to following
Embodiment.
Particular technique or condition are not specified in the embodiment of the present invention, according to the literature in the art described technology or
Condition is carried out according to product description.Reagents or instruments used without specified manufacturer, being can be by commercially available etc.
The conventional products that approach obtains.
Embodiment 1 prepares silicon-oxygen-carbon ceramic hollow fiber composite membrane of the invention
Including following operating procedure:
(1) prepare ceramic powder-polymer solution: by polyether sulfone (10wt%), polyvinylpyrrolidone (0.5wt%) is molten
Polymer solution is formed in N-Methyl pyrrolidone solvent (39.5wt%), the yttrium oxide for being slowly added to average grain diameter 50nm is steady
Determine zirconium oxide (YSZ, 49.8wt%) and iron oxide sintering aid (0.2wt%), after being sufficiently stirred 10~50 hours, is transferred to material
In flow container, vacuum defoamation 0~2 hour, stand for standby use；
(2) prepared by supporter: casting solution and interior solidification liquid (water) being squeezed out with the speed of 3cm/s, between the air through 15cm
Gap enters the outer coagulating bath of tap water, air drying after standing 24 hours.Green body after drying presses following works in Muffle furnace
Skill sintering: 300 DEG C first are risen to from room temperature with 5 DEG C/min, then is continuously heating to 600 DEG C with 2 DEG C/min, then with 5 DEG C/min heating
To 1150 DEG C and 4 hours are kept the temperature, last furnace cooling.
(3) polysiloxanes colloidal sol is prepared: by polymethyl hydrogen siloxane (35wt%), t etram-ethyltetravinylcyclotetrasiloxane
It is small that (35wt%), dimethicone (15wt%) and ethenyl blocking dimethyl silicone polymer (15wt%) are stirred at room temperature 2
When, stand for standby use.
(4) it takes out after ceramic supporting body made from step (2) being impregnated in above-mentioned polysiloxane solution 5s, is reacted at 80 DEG C
1 hour, then under nitrogen protection 800 DEG C obtain silicon-oxygen-carbon ceramic hollow-fibre membrane within pyrolysis 1 hour.It ties in the aperture of test film
Structure and acid resistance.The result shows that the porosity 41% of silicon-oxygen-carbon ceramic hollow-fibre membrane, pore size 50-200nm,
20wt%H2SO4Boil and impregnate 8 hours only weightlessness 0.09wt% in solution.
Comparative example 1:
(1) prepare ceramic powder-polymer solution: by polyether sulfone (15wt%), polyvinylpyrrolidone (0.5wt%) is molten
Polymer solution is formed in N-Methyl pyrrolidone solvent (34.5wt%), the yttrium oxide for being slowly added to average grain diameter 50nm is steady
Determine zirconium oxide (YSZ, 49.8wt%) and iron oxide sintering aid (0.2wt%) is transferred to material liquid tank after being sufficiently stirred 24 hours
In, vacuum defoamation 2 hours, stand for standby use；
(2) prepared by supporter: casting solution and interior solidification liquid (water) being squeezed out with the speed of 3cm/s, between the air through 15cm
Gap enters the outer coagulating bath of tap water, air drying after standing 24 hours.Green body after drying presses following works in Muffle furnace
Skill sintering: 300 DEG C first are risen to from room temperature with 5 DEG C/min, then is continuously heating to 600 DEG C with 5 DEG C/min, then with 5 DEG C/min heating
To 1150 DEG C and 4 hours are kept the temperature, last furnace cooling.
(3) polysiloxanes colloidal sol is prepared: by polymethyl hydrogen siloxane (45wt%), t etram-ethyltetravinylcyclotetrasiloxane
(45wt%), dimethicone (10wt%) stir 2 hours at room temperature, stand for standby use.
(4) it takes out after ceramic supporting body made from step (2) being impregnated in above-mentioned polysiloxane solution 5s, is reacted at 80 DEG C
1 hour, then under nitrogen protection 800 DEG C obtain silicon-oxygen-carbon ceramic hollow-fibre membrane within pyrolysis 1 hour.It ties in the aperture of test film
Structure and acid resistance.The result shows that the porosity 35.5% of silicon-oxygen-carbon ceramic hollow-fibre membrane, pore size is 100nm-1 μm,
In 20wt%H2SO4Boil and impregnate 8 hours weightlessness 0.5wt% in solution.
The pore creating material of embodiment 1 is using dimethicone and ethenyl blocking dimethyl silicone polymer by 1:1 ratio connection
With comparative example 1 only used a kind of pore creating material of dimethicone；Comparative example 1 is compared to embodiment 1: porosity reduction, whole hole
Diameter has increase tendency, water retention property decline.
Comparative example 2:
(1) prepare ceramic powder-polymer solution: by polyether sulfone (10wt%), polyvinylpyrrolidone (0.5wt%) is molten
Polymer solution is formed in N-Methyl pyrrolidone solvent (39.5wt%), the yttrium oxide for being slowly added to average grain diameter 50nm is steady
Determine zirconium oxide (YSZ, 48.5wt%) and iron oxide sintering aid (1.8wt%), after being sufficiently stirred 10~50 hours, is transferred to material
In flow container, vacuum defoamation 0~2 hour, stand for standby use；
(2) prepared by supporter: casting solution and interior solidification liquid (water) being squeezed out with the speed of 3cm/s, between the air through 15cm
Gap enters the outer coagulating bath of tap water, air drying after standing 24 hours.Green body after drying presses following works in Muffle furnace
Skill sintering: 300 DEG C first are risen to from room temperature with 5 DEG C/min, then is continuously heating to 600 DEG C with 2 DEG C/min, then with 5 DEG C/min heating
To 1150 DEG C and 4 hours are kept the temperature, last furnace cooling.
Hollow ceramic made from comparative example 2 is compared with example 1, and mechanical strength is increased to 265MPa by 142MPa, but hole is tied
Structure is almost closed, and pure water flux drops to 46Lm by 1542-2h-1It is not suitable for the supporter of filter membrane.
Comparative example 3:
(1) prepare ceramic powder-polymer solution: by polyether sulfone (10wt%), polyvinylpyrrolidone (0.5wt%) is molten
Polymer solution is formed in N-Methyl pyrrolidone solvent (39.5wt%), the yttrium oxide for being slowly added to average grain diameter 50nm is steady
Determine zirconium oxide (YSZ, 49.8wt%) and iron oxide sintering aid (0.2wt%), after being sufficiently stirred 10~50 hours, is transferred to material
In flow container, vacuum defoamation 0~2 hour, stand for standby use；
(2) prepared by supporter: casting solution and interior solidification liquid (water) being squeezed out with the speed of 3cm/s, between the air through 15cm
Gap enters the outer coagulating bath of tap water, air drying after standing 24 hours.Green body after drying presses following works in Muffle furnace
Skill sintering: 300 DEG C first are risen to from room temperature with 5 DEG C/min, then is continuously heating to 600 DEG C with 2 DEG C/min, then with 5 DEG C/min heating
To 1150 DEG C and 4 hours are kept the temperature, last furnace cooling.
(3) polysiloxanes colloidal sol is prepared: by polymethyl hydrogen siloxane (35wt%), t etram-ethyltetravinylcyclotetrasiloxane
(35wt%), dimethicone (20wt%) and ethenyl blocking dimethyl silicone polymer (10wt%) stir 2 hours at room temperature,
Stand for standby use.
(4) it takes out after ceramic supporting body made from step (2) being impregnated in above-mentioned polysiloxane solution 5s, is reacted at 80 DEG C
1 hour, then under nitrogen protection 800 DEG C obtain silicon-oxygen-carbon ceramic hollow-fibre membrane within pyrolysis 1 hour.It ties in the aperture of test film
Structure and acid resistance.The result shows that the porosity 42.5% of silicon-oxygen-carbon ceramic hollow-fibre membrane, pore size is 100nm-1 μm,
In 20wt%H2SO4Boil and impregnate 8 hours only weightlessness 0.15wt% in solution.
The pore creating material of embodiment 1 uses the ratio in 1:1 of dimethicone and ethenyl blocking dimethyl silicone polymer
Combination, and comparative example 3 is combined using 2:1, comparative example 3 and is compared to embodiment 1: porosity increases, whole aperture has
Increase tendency.
1500 DEG C or more of high temperature compared to the prior art, the method for the present invention only need 700~1000 DEG C of sintering temperature
The asymmetric silicon oxygen carbon hollow-fibre membrane that it is 10nm-1 μm with pore size that degree, which can be made, the reduction of temperature are greatly saved
Energy consumption significantly reduces ceramic membrane and is sintered cost.Ceramic hollow fibrous membrane porosity produced by the present invention is 30%-42%, pure water
Flux is 1000-1549L m-2h-1, acid and alkali-resistance characteristic is good.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
Limitations on the scope of the patent of the present invention therefore cannot be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to guarantor of the invention
Protect range.Therefore, protection scope of the present invention should be determined by the appended claims.
Claims (10)
1. a kind of silicon-oxygen-carbon ceramic hollow fiber composite membrane, which is characterized in that including silicon-oxygen-carbon ceramic separating layer and ceramic support
Body；The composite membrane pore size is 10nm-1 μm.
2. a kind of preparation method of silicon-oxygen-carbon ceramic hollow fiber composite membrane, which comprises the following steps:
(1) ceramic powder-polymer solution, i.e. casting solution are prepared；
(2) casting solution made from step (1) prepares supporter；
(3) polysiloxane solution is prepared；
(4) supporter made from step (2) is immersed in polysiloxane solution made from step (3) and is made in silicon-oxygen-carbon ceramic
Hollow fiber composite membrane.
3. the preparation method of silicon-oxygen-carbon ceramic hollow fiber composite membrane according to claim 2, which is characterized in that the step
Suddenly ceramic powder-polymer solution each component mass percent in (1) are as follows: 10~30wt% of polyether sulfone, polyvinylpyrrolidine
0.1~2wt% of ketone, 20~40wt% of N-Methyl pyrrolidone, 30~50wt% of ceramic powder, 0~1.5wt% of sintering aid；
The sum of weight percent of each component is 100%.
4. the preparation method of silicon-oxygen-carbon ceramic hollow fiber composite membrane according to claim 3, which is characterized in that ceramic powder
Body is Zirconium powder, and diameter of particle selects two kinds of sizes of size, and little particle diameter of particle range is 10-50nm, bulky grain powder
Body particle size range is 100-750nm.
5. the preparation method of silicon-oxygen-carbon ceramic hollow fiber composite membrane according to claim 3, which is characterized in that the step
Suddenly (1) prepares ceramic powder-polymer solution, and concrete operations include: that polyether sulfone and polyvinylpyrrolidone are dissolved in N- methyl
Polymer solution is formed in pyrrolidinone solvent, and ceramic powder and sintering aid is then added and is sufficiently stirred 10~50 hours,
So that ceramic powder and sintering aid are dispersed in polymer solution and form casting solution；Casting solution vacuum defoamation 0~2 is small
When, it places spare.
6. the preparation method of silicon-oxygen-carbon ceramic hollow fiber composite membrane according to claim 2, which is characterized in that the step
Suddenly prepared by (2) supporter, and concrete operations include: to squeeze out casting solution made from step (1) and interior solidification liquid through spinneret, passes through
The air gap enters in outer solidification liquid, standing and drying, and ceramic supporting body green body is made；Ceramics are made through being sintered in green body obtained
Supporter.
7. the preparation method of silicon-oxygen-carbon ceramic hollow fiber composite membrane according to claim 6, which is characterized in that the casting
The speed that film liquid and interior solidification liquid are squeezed out through spinneret is 3cm/s；The casting solution and interior solidification liquid pass through after spinneret squeezes out
The length for crossing the air gap is 15cm.
8. the preparation method of silicon-oxygen-carbon ceramic hollow fiber composite membrane according to claim 2, which is characterized in that the step
Suddenly (3) prepare polysiloxanes colloidal sol, and concrete operations include: to be mixed and stirred for polysiloxanes and pore creating material 0~2 hour, stand
It is spare；Wherein, the polysiloxanes is one in MK resin, polymethyl hydrogen siloxane or t etram-ethyltetravinylcyclotetrasiloxane
Kind is several；The pore creating material is one of dimethicone, ethenyl blocking dimethyl silicone polymer or 201 methyl-silicone oils
Or it is several；The sum of weight percent of the polysiloxanes and pore creating material is 100%.
9. the preparation method of silicon-oxygen-carbon ceramic hollow fiber composite membrane according to claim 8, which is characterized in that described to make
Hole agent is dimethicone and ethenyl blocking dimethyl silicone polymer；Dimethicone and ethenyl blocking polydimethylsiloxanes
Alkane ratio is 1:1.
10. the preparation method of silicon-oxygen-carbon ceramic hollow fiber composite membrane according to claim 2, which is characterized in that described
Step (4) concrete operations include: supporter made from step (2) is immersed in 0 in polysiloxane solution made from step (3)~
30s reacts 10~120min in 60~70 DEG C of baking oven；Then 1~4h is heat-treated in 700~1200 DEG C of inert atmospheres,
Repetition above-mentioned " dipping-baking oven reaction-heat treatment " process 1-5 times is to obtain silicon-oxygen-carbon ceramic hollow fiber composite membrane.
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| CN112830787A (en) * | 2021-01-15 | 2021-05-25 | 天津大学 | Preparation method of amorphous silicon-oxygen-carbon composite ceramic thermal barrier coating |
| CN113019134A (en) * | 2021-02-27 | 2021-06-25 | 北京工业大学 | Method for improving hydrophobic stability of porous ceramic membrane for desalination |
| CN115364677A (en) * | 2021-05-21 | 2022-11-22 | 三达膜科技（厦门）有限公司 | Preparation method of thermal stability modified spherical alumina ceramic microfiltration membrane |
| CN115364677B (en) * | 2021-05-21 | 2024-03-19 | 三达膜科技（厦门）有限公司 | Preparation method of thermal stability modified spherical alumina ceramic microfiltration membrane |
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