CN101175705A - Method for producing a wear-resistant reaction-bounded ceramic filtering membrane - Google Patents
Method for producing a wear-resistant reaction-bounded ceramic filtering membrane Download PDFInfo
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- CN101175705A CN101175705A CNA2006800165188A CN200680016518A CN101175705A CN 101175705 A CN101175705 A CN 101175705A CN A2006800165188 A CNA2006800165188 A CN A2006800165188A CN 200680016518 A CN200680016518 A CN 200680016518A CN 101175705 A CN101175705 A CN 101175705A
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Abstract
The invention relates to a method for producing a wear-resistant reaction-bounded ceramic filtering membrane, during which a porous metallic or non-metallic support for producing a green body is provided with a suspension. This suspension is obtained from a dispersant and from a dispersed phase, and this dispersed phase can be obtained from at least one ceramic raw material from the group of metal nitrides and, optionally, from at least one other ceramic raw material. The invention provides that the green body produced in this manner is fired at a temperature ranging from 700 DEG C to 1250 DEG C under atmospheric pressure in a oxidizing atmosphere in order to obtain a phase change of at least the ceramic raw material.
Description
Technical field
The present invention relates to the method described in the preamble as claimed in claim 1.
Background technology
The ceramic filtration membrane that is also referred to as membrane filter has various uses widely, for example in the purification of waste gas, in the purification for gas process or in foodstuffs industry, drink industry, pharmaceutical industry, chemical industry, semiconductor production, biotechnology field and in by the scavenging process in the fields such as the valuable material of waste recovery, have various uses widely.
Known in the prior art have a whole bag of tricks of making the coating be used for support, especially makes the whole bag of tricks of porousness filter membrane.Disclose the method that is used to make pottery sieve strainer among DE 43 28 295 A1, wherein metal or the nonmetal support to porous inorganic provides the suspension with at least a coating agent, and described coating agent comprises at least a ceramic raw material.In preceding method, can be used as the coating agent such as the ceramic raw materials such as oxide compound, carbide and nitride of Si, Al, Ti and Zr.Thus obtained material base is carried out high pressure-temperature to be handled to realize the phase transformation of described at least coating agent.Utilize previous currently known methods, can make sieve formula strainer or membrane filter with the aperture that can clearly define in advance, described aperture at macro-scope to nanometer range.Here, between mould material and supporting body material epitaxy can take place, the result forms stressless microtexture key, and this stressless microtexture key also can cause higher temperature resistance sex change except can producing higher thermostability.
Described hydrothermal method in DE 43 28 295 A1, it is that 10bar～200bar and temperature are to carry out high pressure-temperature in 200 ℃～700 ℃ the autoclave to handle that described hydrothermal method is included in pressure.Pressure in the autoclave is produced by water vapour.Film particles mutually combines by solution and recrystallization process under water vapour pressure just.Yet previous currently known methods needs very complicated processing, and only can carry out under expensive.
Summary of the invention
The purpose of this invention is to provide a kind of effective ways that are used to make the ceramic filtration membrane of attrition resistant reaction bonded (Reaktionsgebundene), this method can be carried out in simple and cost-effective mode, especially this method can obtain having void distribution that clearly define, uniform, and has fabulous fusible ceramic filtration membrane simultaneously between ceramic raw material and support.
For achieving the above object, provide in the method for the feature of the preamble with claim 1: material base under atmospheric pressure cures under 700 ℃～1250 ℃ temperature in oxidizing atmosphere, thereby realizes the phase transformation of described at least ceramic raw material.
By the invention enables such technology to become possibility, that is, use nitride can make the pottery of reaction bonded as reacted constituent, thus obtained filter membrane has lower processing complicacy and higher mechanical stability.Porcelain filter made according to the method for the present invention has high-caliber intensity, and has the size in the hole of macro-scope to the nanometer range that clearly defines in advance.But the filter membrane that adopts expensive hydrothermal method to obtain to have specific characteristic there is no need in prior art according to the present invention.Method of the present invention can guarantee that film particles is simultaneously in its each other coalescent and coalescent with supporting body material.This can obtain stressless microtexture key, produces high-caliber bonding strength and high-caliber filter membrane impedance thus.
Embodiment
As ceramic raw material, can use at least a from the nitride of metal titanium and/or zirconium from the group of metal nitride.Also can use aluminium nitride in principle.Can use the metal nitride of pure state metal types or the metal nitride of various metal mixtures.In addition, disperse phase can comprise from the pure metal group, especially at least a other ceramic raw materials of the group of titanium and/or zirconium and/or aluminium.Described other ceramic raw materials can be selected from metal oxide group, the especially oxide compound of titanium and/or zirconium and/or aluminium.When curing material base, under 700 ℃～1250 ℃ temperature, metal nitride and described other ceramic raw materials react, and generate metal oxide thus.Phase transformation can preferably be carried out under 800 ℃～1000 ℃ temperature, and this helps to make ceramic filtration membrane of the present invention to have good especially mechanical characteristics.
The nanometer powder that nitride also can be used as non-blast (nicht-explosive) obtains, and according to the present invention, this makes that to use granular size be 0.005 μ m becomes possibility as the disperse phase that is used to make ultra-filtration membrane to the metal nitride of＜0.1 μ m.Can certainly use the particle of granular size＞0.1 μ m to make millipore filtration in principle.Use the ultra-filtration membrane of method manufacturing of the present invention to have high-caliber mechanical surface wear resistance (abrasion resistance).Owing to have high strength and wear resistance, porcelain filter or ceramic membrane can use in the various application that those films that adopts prior art to obtain can wear and tear or damage.In addition, the less strainer of thin film layer thickness can be made, thereby transmembrane pressure can be when filter operation, reduced.Much less, bigger particulate also can be used for making filter membrane of the present invention, is 0.005 μ m～5 μ m thereby make the solid granular size that obtains in the disperse phase.
Disperse phase or solid phase should be preferably about 0.1 weight %～20 weight % with respect to the ratio of the quality of dispersion agent.This helps to make filter membrane of the present invention to have particularly preferred mechanical characteristics.Described dispersion agent can be water and/or at least a alcohol and/or at least a organogel formation agent.In addition, can according to circumstances select to use at least a organic dispersing agent.Organogel formation agent should be preferably about 0.1 weight %～5 weight % with respect to the ratio of the quality of described dispersion agent.Described dispersion agent should be preferably set to about 0.1 weight %～100 weight % with respect to the ratio of the quality of described disperse phase.Much less, aforementioned value only is a preferred value, and therefore greater or lesser in principle ratio also is possible.
Described suspension can be by flooding, spray, brush, suspend in midair or being applied on the described support by a pumping that is preferably the piped support.If suspension is applied on the support by dipping or pumping, then be preferably about 1 second～60 seconds the duration of contact of support and suspension.Like this, can guarantee that support fully is coated with, and guarantee that suspension can penetrate sufficiently in the supporting body material.
In a particularly preferred embodiment of the present invention, material base or unprocessed film before curing at normal atmosphere be about under 20 ℃～250 ℃ the temperature dry.This can make between ceramic particle and supporting body material Procuring takes place.
Be to make the multilayer filter membrane, can be repeatedly according to the present invention to support, preferred 2～5 times, use described suspension preferred especially 3 times.Equally preferably, material base carries out drying once more and/or cures after using suspension.Use, therefore process dry and that cure can take place 1～5 time, wherein stoving temperature preferably incrementally reduces each curing in the process in succession, thus the vesicular structure of the qualification that reduces in succession of the size of manufacturing hole after this manner.For example, the initial material base that forms can be at 1000 ℃～1250 ℃, are preferably under 1100 ℃ the starting temperature to cure.The material base of Xing Chenging cures under the size with the hole is defined as the outlet temperature of 0.005 μ m～5 μ m then at last, and the aperture of described filter membrane can be regulated by the target particles growth by the stoving temperature level.Using the method according to this invention, is that 0.005 μ m～5 μ m, bed thickness are the filter membrane of 1 μ m～10 μ m thereby can make the size with definite hole.Curing in the process of material base, the nitride/metal particle is oxide compound by phase transformation in its point of contact epitaxy, and growth is carried out to inside by particle surface.
Embodiment
The embodiment that describes below relates to the preferred implementation of the method according to this invention, but should be understood that the present invention suggested both be not limited to shown in the selection of each composition treatment condition shown in also being not limited to.
The TiN powder is mixed with about 1: 50 ratio with the water that comprises organic gel former.The suspension that obtains thus by the dipping or spray application on ceramic support to deposit unprocessed film.Subsequently, described unprocessed film cures in temperature is about 800 ℃～1250 ℃ stove, is the porousness TiO of about 0.05 μ m～1.8 μ m thereby obtain mean pore size
2Millipore filtration or ultra-filtration membrane.
The TiM powder forms agent with propyl alcohol and organogel to be mixed with about 1: 100 ratio.The suspension that obtains thus by the dipping or spray application on ceramic support to deposit unprocessed film.Subsequently, described unprocessed film is about 500 ℃～1000 ℃ in temperature, especially cure in＞700 ℃ to 1000 ℃ the stove in temperature, and be the porousness TiO of about 0.02 μ m～0.1 μ m thereby obtain mean pore size
2Ultra-filtration membrane.
In unique accompanying drawing, the aperture and the dependence of curing the temperature levels of process of the ceramic filtration membrane of using the method according to this invention acquisition described.The size or the aperture in hole can be regulated according to the temperature levels of the process of curing as can be known according to this accompanying drawing.When temperature T raise, aperture d pressed index law and increases.
In addition, should be noted that and developed the method relevant with the present invention, this method help to detect method of the present invention in making porcelain filter application or the application of suspension of the present invention.This detection method relevant with the present invention can more simple and easyly check whether used method manufacturing porcelain filter of the present invention or whether used suspension of the present invention quickly.
In a word, even should be noted in the discussion above that and not do specific emphasizing, the whole values shown in can being included in about the registration of the specified four corner of specification sheets of the present invention in the scope.
Claims (15)
1. method that is used to make the ceramic filtration membrane of attrition resistant reaction bonded, wherein provide suspension to be used to produce material base to porous metal or nonmetal support, wherein said suspension is obtained by dispersion agent and disperse phase, and described disperse phase wherein can be obtained by at least a ceramic raw material and available at least a other ceramic raw materials from the group of metal nitride, described method is characterised in that the material base that makes thus under atmospheric pressure cures under 700 ℃～1250 ℃ temperature in oxidizing atmosphere, thereby realize the phase transformation of described at least ceramic raw material.
2. the method described in claim 1 is characterized in that, at least a as a kind of ceramic raw material in the nitride of metal titanium and/or zirconium and/or aluminium.
3. the method described in claim 1 or 2, it is characterized in that, described other ceramic raw materials are selected from the group of metal, especially the metal group of titanium and/or zirconium and/or aluminium and/or be selected from group, the especially titanium of metal oxide and/or the group of the oxide compound of the metal of zirconium and/or aluminium.
4. the described method of one of claim as described above is characterized in that described phase transformation is carried out at 800 ℃～1000 ℃.
5. the described method of one of claim as described above is characterized in that, selecting granular size is a kind of ceramic raw material and/or the another kind of ceramic raw material of 0.005 μ m～5 μ m.
6. the described method of one of claim as described above is characterized in that described disperse phase is set at about 0.1 weight %～20 weight % with respect to the ratio of the quality of described dispersion agent.
7. the described method of one of claim as described above is characterized in that, water and/or at least a alcohol and/or at least a organogel form agent and available at least a organic dispersing agent as dispersion agent.
8. the described method of one of claim as described above is characterized in that, described organogel forms agent and is set at about 0.1 weight %～5 weight % with respect to the ratio of the quality of described dispersion agent.
9. the described method of one of claim as described above is characterized in that described dispersion agent is set at about 0.1 weight %～100 weight % with respect to the ratio of the quality of described disperse phase.
10. the described method of one of claim as described above is characterized in that, described suspension is by to flooding, spray, brush, jettisoning or being applied on the described support by a pumping that is preferably the tubulose support.
11. the described method of one of claim is characterized in that as described above, be set at about 1 second～60 seconds the duration of contact of described support and described suspension when dipping or pumping.
12. the described method of one of claim is characterized in that as described above, described material base preferably carries out drying under about 20 ℃～250 ℃ temperature and normal atmosphere before curing.
13. the described method of one of claim is characterized in that as described above, described suspension repeatedly is applied to described support, and wherein, preferably, described material base is dried after at every turn the using of described suspension and/or cures.
14. the described method of one of claim is characterized in that as described above, described stoving temperature cures in succession in the process and incrementally reduces at each, thus the filter membrane of the vesicular structure that the size of manufacturing hole reduces in succession.
15. the described method of one of claim as described above, it is characterized in that, the initial material base that forms preferably cures under 1100 ℃ starting temperature at 1000 ℃～1250 ℃, and the material base of Xing Chenging is defined as in the size with the hole curing under the outlet temperature of 0.005 μ m～5 μ m at last.
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE102005023053.9 | 2005-05-13 | ||
| DE102005023053 | 2005-05-13 | ||
| DE102005028452.3 | 2005-06-17 | ||
| DE102005031856.8 | 2005-07-06 |
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| Publication Number | Publication Date |
|---|---|
| CN101175705A true CN101175705A (en) | 2008-05-07 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2006800165188A Pending CN101175705A (en) | 2005-05-13 | 2006-05-13 | Method for producing a wear-resistant reaction-bounded ceramic filtering membrane |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110408922A (en) * | 2019-08-29 | 2019-11-05 | 西安石油大学 | A kind of preparation method of gradient composite porous membrane tube |
| CN110743388A (en) * | 2019-09-20 | 2020-02-04 | 三达膜科技（厦门）有限公司 | End-capping method for tubular ceramic membrane |
| CN112221251A (en) * | 2020-09-29 | 2021-01-15 | 潘锡丹 | Ceramic filter plate forming processing method |
-
2006
- 2006-05-13 CN CNA2006800165188A patent/CN101175705A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110408922A (en) * | 2019-08-29 | 2019-11-05 | 西安石油大学 | A kind of preparation method of gradient composite porous membrane tube |
| CN110743388A (en) * | 2019-09-20 | 2020-02-04 | 三达膜科技（厦门）有限公司 | End-capping method for tubular ceramic membrane |
| CN110743388B (en) * | 2019-09-20 | 2021-08-20 | 三达膜科技（厦门）有限公司 | End-capping method for tubular ceramic membrane |
| CN112221251A (en) * | 2020-09-29 | 2021-01-15 | 潘锡丹 | Ceramic filter plate forming processing method |
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