CN109776083A - A kind of multi-stage porous ceramic material and preparation method thereof with complex function - Google Patents
A kind of multi-stage porous ceramic material and preparation method thereof with complex function Download PDFInfo
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Abstract
The invention discloses a kind of multi-stage porous ceramic material and preparation method thereof with complex function, multi-stage porous ceramic material are formed by inorganic multi-stage porous matrix and by the complex function thin film that complex function colloidal sol is sprayed on inorganic multi-stage porous matrix surface；Complex function thin film is prepared by titanium dioxide, functional additive, acidic aqueous solution；The compound of two or more different function of the functional additive in Zinc oxide nanoparticle/cluster, copper oxide nanometer particle/cluster, halogenation silver nano-grain/cluster, pucherite nano particle/cluster, graphite phase carbon nitride nano particle/cluster, silver/copper nanocrystallite, gallic acid, polyvinyl alcohol, polyvinyl phenol.Multi-stage porous ceramic material provided by the invention with complex function belongs to solid phase supported catalyst, overcomes the recycling of subparticle catalyst difficulty, reuses the problems such as trouble absorption and decomposition, it can be achieved that the organic pollutants such as dyestuff, formaldehyde.
Description
Technical field
The present invention relates to a kind of functional nano-composites processing technology more particularly to a kind of multistages with complex function
Hole ceramic material and preparation method thereof.
Background technique
With the progress of social technology and the raising of manufacture level, more and more New Building Materials are applied, and are taking
While obtaining convenient, cheap and comfortable living environment, air in buildings quality, environmental quality are worse and worse.Such as exist following
Defect: (1) composite recycled material, paint, coating application so that indoor formaldehyde severely exceed, can not dissipate, seriously endanger people
Body health；(2) it significantling change such as the indoor humidity short time, indoor humidity is excessively high to lead to the easy mass propagation such as mould, acarid, or
Person's indoor humidity is too low, and to cause throat, nose that will be easy dry and astringent, has dry skin itch, influenza is easily sent out；(3) in addition, large area
High-compactness wall, easily causes sound wave to reflect, and causes indoor hearsay condition very poor, mood is caused to be had the fidgets；(4) current city
Various interior functional decorations can alleviate environmental problem to a certain extent on face, but due to having a single function, use synthesis
Effect is relatively low.
People make great efforts to develop novel and multifunctional ceramic decoration material always as a result, it is desirable to new decorative material for building itself
Pernicious gas is not generated, the ornament materials such as coating, wallpaper can be replaced to play decoration function.But currently, there is absorption point simultaneously
Solve pernicious gas, moisture absorption damping, antibacterial and mouldproof, anti-algae anti-condensation, sound absorption drop dry, antiallergy, antiviral, Far-infrared Heating physical therapy
Etc. multiple functions, can meet a material be mostly used demand functional decoration material be also not seen reported.
Summary of the invention
For overcome the deficiencies in the prior art, one of the objects of the present invention is to provide a kind of multistages with complex function
Hole ceramic material.Multi-stage porous ceramic material provided by the invention with complex function belongs to solid phase supported catalyst, overcomes
The problems such as trouble, is reused in the recycling of subparticle catalyst difficulty, and it is more preferable, it can be achieved that dyestuff, first to be equipped with illumination apparatus effect
The absorption of the organic pollutants such as aldehyde is with decomposition, it can be achieved that effect that a material is mostly used, is provided simultaneously with adsorption-decomposition function pernicious gas, moisture absorption
The effects of damping, antibacterial and mouldproof, anti-algae anti-condensation, the dry, antiallergy of sound absorption drop, antiviral, Far-infrared Heating physical therapy.
The second object of the present invention is to provide a kind of preparation method of multi-stage porous ceramic material with complex function.It should
The preparation method of material is simple and easy to control, and material quantity is rich inexpensive, in the various interiors for meeting healthy household, low-carbon green life requires
It has broad application prospects in wall decoration material.
An object of the present invention adopts the following technical scheme that realization: a kind of multi-stage porous ceramics material with complex function
Material, the complex function thin film group of inorganic multi-stage porous matrix surface is sprayed on by inorganic multi-stage porous matrix and by complex function colloidal sol
At；The complex function colloidal sol containing titanium salt, acidic aqueous solution, functional additive by being prepared；The functional additive is selected from
Zinc oxide nanoparticle/cluster, copper oxide nanometer particle/cluster, halogenation silver nano-grain/cluster, pucherite nano particle/
Cluster, graphite phase carbon nitride nano particle/cluster, silver/copper nanocrystallite, gallic acid, polyvinyl alcohol, two kinds in polyvinyl phenol
Or the compound of two or more different function.
Further, the inorganic multi-stage porous matrix is using a variety of inoganic solids powder as raw material, through granulation, molding, 600-
900 DEG C are made；The inoganic solids powder be selected from diatomite, allophane, montmorillonite, Emathlite, bentonite, zeolite,
One of attapulgite, sepiolite, flyash, waste gypsum, waste incineration ash content, float stone, medical stone, tourmaline, rutile
Or two or more composition.
Further, the aperture of the inorganic multi-stage porous matrix is distributed in nanometer scale to submillimeter magnitude.
Further, the complex function colloidal sol preparation method the following steps are included:
The step of preparing acidic aqueous solution: acid is added in aqueous solution, obtains acidic aqueous solution；
The step of preparing titanium solution: it disperses titaniferous salt in dehydrated alcohol, obtains titanium solution；
The step of mixing: under stirring, 5-40 DEG C of cryogenic conditions, resulting titanium solution is slowly added into acid water-soluble
In liquid, titaniferous aqueous solution is obtained；
The step of functional additive is added: function is added into resulting titaniferous aqueous solution under stirring, ultrasound condition and adds
Add agent；Under stirring condition, 5-40 DEG C ripening 1-5 days, obtain complex function colloidal sol；
The step of cryo-conservation: it will be saved under 5-40 DEG C of low temperature after the encapsulation of complex function colloidal sol, be stand-by.
Further, in the step of preparing acidic aqueous solution, acid one kind or two in acetic acid, hydrochloric acid, sulfuric acid
Kind or more mixed acid, the pH value of the acidic aqueous solution is 1-5.
Further, described to be selected from butyl titanate, titanium tetrachloride, four isopropyls containing titanium salt in the step of preparing titanium solution
One or more of alcohol titanium, isopropyl titanate, the dosage containing titanium salt are 0.5-50g/L.
Further, in the step of mixing, the speed of the stirring is 500-1000rpm, and the cryogenic conditions are 5-
40℃。
Further, in the step of functional additive is added, the speed of the stirring is 500-1000rpm, described super
Sound condition is 20-40KHz；The dosage of the functional additive is 0.05-25g/L.
The second object of the present invention adopts the following technical scheme that realization: a kind of multi-stage porous ceramic material with complex function
Preparation method, include the following steps:
The step of preparing inorganic multi-stage porous matrix: the inorganic multi-stage porous matrix using a variety of inoganic solids powder as raw material,
It is made through granulation, molding, 600-900 DEG C；
The step of preparing complex function colloidal sol: secure ph is the aqueous solution of 1-5, obtains acidic aqueous solution；Titanium salt will be contained
It is scattered in dehydrated alcohol, obtains titanium solution；Under stirring, 5-40 DEG C of cryogenic conditions, resulting titanium solution is slowly added to
Into acidic aqueous solution, titaniferous aqueous solution is obtained；Function is added into resulting titaniferous aqueous solution under stirring, ultrasound condition to add
Add agent, ripening 1-5 days under stirring condition obtains complex function colloidal sol；
The step of spraying: complex function colloidal sol is sprayed on the inorganic multi-stage porous matrix surface that temperature is 100-250 DEG C, so
Afterwards 300-600 DEG C at a temperature of be heat-treated 10-120 minutes.
Further, the preparation method, in the step of spraying, the complex function colloidal sol is in inorganic multi-stage porous base
The mass content in body surface face is 0.1-50g/m2。
Compared with prior art, the beneficial effects of the present invention are:
(1) multi-stage porous ceramic material of the present invention is, as matrix, to exist through colloid spraying technology with porous inorganic material
Inorganic multi-stage porous matrix surface sprays one layer with titanium dioxide (TiO2) photocatalyst film as main component；Inorganic multi-stage porous
The adsorbable multiple pollutant including formaldehyde, foul smell of matrix, while being TiO2Equal nano-photocatalysts provide load physics
Space decomposes functional layer of the pollutant based on the photocatalysis, deodorization；According to Functional Design needs, photocatalysis film is applied
It may include the oxidate nanos cluster such as ZnO, CuO in layer, also may include the functional additives such as the metal nanometre clusters such as Ag, it can also be with
Comprising the antianaphylaxis functions additive such as gallic acid, polyvinyl alcohol, polyvinyl phenol, the multi-stage porous pottery with complex function is constructed
Ceramic material.Gained contains TiO2The multi-stage porous ceramic material of equal nano-photocatalysts is mixed in ultraviolet light, visible light or ultraviolet-visible
Under illumination condition, organic volatile substances such as the formaldehyde of absorption or dye molecule can be decomposed into other small molecules, had
The effect of the organic pollutants such as sterilization, anti-mildew, damping, formaldehyde degradation, indoors household, hospital, school, home for destitute, office
The occasions such as room are used as wall decoration material, can significantly improve comfort level, realize the healthy living of high quality.
(2) the multi-stage porous ceramic material provided by the invention with complex function belongs to solid phase supported catalyst, overcomes
The problems such as trouble, is reused in the recycling of subparticle catalyst difficulty, can be achieved at the same time adsorption-decomposition function pernicious gas, moisture absorption tune
Dry, antiallergy, antiviral, Far-infrared Heating physical therapy and other effects drop in wet, antibacterial and mouldproof, anti-algae anti-condensation, sound absorption.
(3) preparation method of the material is simple and easy to control, and material quantity is rich inexpensive, is meeting healthy household, low-carbon green life
It is required that various indoor wall decoration materials in have broad application prospects.
Detailed description of the invention
Fig. 1 is the finished figure for the multi-stage porous ceramic material that the embodiment of the present invention 2 has complex function；
Fig. 2 is that 2 multi-stage porous ceramic material of the embodiment of the present invention degrades rhodamine aqueous solution with ultraviolet-visible light spoke
Take time extended decoloration picture；
Fig. 3 is rhodamine aqueous solution of degrading under 1-4 of embodiment of the present invention multi-stage porous ceramic material ultraviolet-visible light
Decolourize curve；
Fig. 4 is nitrogen adsorption-desorption curve of 2 multi-stage porous ceramic material of the embodiment of the present invention；
Fig. 5 is the pore size distribution curve of 2 multi-stage porous ceramic material of the embodiment of the present invention；
Fig. 6 is the electron scanning micrograph of 2 multi-stage porous ceramic material of the embodiment of the present invention.
Specific embodiment
In the following, being described further in conjunction with attached drawing and specific embodiment to the present invention, it should be noted that not
Under the premise of conflicting, new implementation can be formed between various embodiments described below or between each technical characteristic in any combination
Example.
In the present invention, if not refering in particular to, all parts, percentage are unit of weight, used equipment and raw material etc.
It is commercially available or commonly used in the art.Method in following embodiments is unless otherwise instructed the normal of this field
Rule method.
A kind of multi-stage porous ceramic material with complex function, sprays by inorganic multi-stage porous matrix and by complex function colloidal sol
It is formed in the complex function thin film of inorganic multi-stage porous matrix surface；The complex function colloidal sol is by containing titanium salt, acidic aqueous solution, function
Energy additive is prepared；
The functional additive is selected from Zinc oxide nanoparticle/cluster, copper oxide nanometer particle/cluster, halogenation silver nanoparticle
Particle/cluster, pucherite nano particle/cluster, graphite phase carbon nitride nano particle/cluster, silver/copper nanocrystallite, gallic acid,
The compound of two or more different function in polyvinyl alcohol, polyvinyl phenol.The Zinc oxide nanoparticle/
Cluster, copper oxide nanometer particle/cluster, halogenation silver nano-grain/cluster, pucherite nano particle/cluster, graphite phase carbon nitride are received
Forbidden bandwidth is in 2.0-3.2eV in rice grain/cluster, silver/copper nanocrystallite functional additive, in ultraviolet light, visible light or purple
All there is photocatalysis performance under outside-visible light.Halogenation silver nano-grain particle/cluster is because of Ag+Presence have sterilization, sterilizing
Effect, be a kind of excellent nontoxic sterilization material.Also, a small amount of Ag metal simple-substance has surface plasma resonance effect,
Visible light can be absorbed, further increase catalytic degradation and bactericidal effect.Titanium dioxide and functional additive are applied in combination can
To improve photocatalysis performance, photo-catalysis capability is weak under visible light for single titanium dioxide, can improve dioxy after being applied in combination
Change titanium photocatalysis performance under visible light.And can have stronger bactericidal effect, greatly improve titanium dioxide uses model
It encloses.In addition, gallic acid, tannic acid, polyvinyl alcohol and polyvinyl phenol have antianaphylactic effect.
As further embodiment, the inorganic multi-stage porous matrix is using a variety of inoganic solids powder as raw material, through making
Grain, molding, 600-900 DEG C be made；The inoganic solids powder be selected from diatomite, allophane, montmorillonite, Emathlite,
Bentonite, zeolite, attapulgite, sepiolite, flyash, waste gypsum, waste incineration ash content, float stone, medical stone, tourmaline, gold
The composition of one or more of red stone.
As further embodiment, the aperture of the inorganic multi-stage porous matrix is in nanometer scale to submillimeter magnitude point
Cloth.
As further embodiment, the preparation method of the complex function colloidal sol the following steps are included:
The step of preparing acidic aqueous solution: acid is added in aqueous solution, obtains acidic aqueous solution；
The step of preparing titanium solution: it disperses titaniferous salt in dehydrated alcohol, obtains titanium solution；
The step of mixing: under stirring, 5-40 DEG C of cryogenic conditions, resulting titanium solution is slowly added into acid water-soluble
In liquid, titaniferous aqueous solution is obtained；
The step of functional additive is added: function is added into resulting titaniferous aqueous solution under stirring, ultrasound condition and adds
Add agent, under stirring condition, 5-40 DEG C ripening 1-5 days, obtain complex function colloidal sol；Stirring can prevent molten in ageing process
Glue is layered and influences uniformity.
The step of cryo-conservation: it will be saved under 5-40 DEG C of low temperature after the encapsulation of complex function colloidal sol, be stand-by.
As further embodiment, in the step of preparing acidic aqueous solution, the acid is selected from acetic acid, hydrochloric acid, sulphur
One or more kinds of mixed acid in acid, the pH value of the acidic aqueous solution are 1-5.
It is described to be selected from butyl titanate, tetrachloro containing titanium salt in the step of preparing titanium solution as further embodiment
Change the one or more of titanium, titanium tetraisopropylate, isopropyl titanate, the dosage containing titanium salt is 0.5-50g/L.
As further embodiment, in the step of mixing, the speed of the stirring is 500-1000r/min, institute
Stating cryogenic conditions is 5-40 DEG C.
As further embodiment, in the step of functional additive is added, the speed of the stirring is 500-
1000r/min, the ultrasound condition are 20-40KHz；The dosage of the functional additive is 0.05-25g/L.
The second object of the present invention adopts the following technical scheme that realization: a kind of multi-stage porous ceramic material with complex function
Preparation method, include the following steps:
The step of preparing inorganic multi-stage porous matrix: the inorganic multi-stage porous matrix using a variety of inoganic solids powder as raw material,
It is made through granulation, molding, 600-900 DEG C；
The step of preparing complex function colloidal sol: secure ph is the aqueous solution of 1-5, obtains acidic aqueous solution；Titanium salt will be contained
It is scattered in dehydrated alcohol, obtains titanium solution；Under stirring, 5-40 DEG C of cryogenic conditions, resulting titanium solution is slowly added to
Into acidic aqueous solution, titaniferous aqueous solution is obtained；Function is added into resulting titaniferous aqueous solution under stirring, ultrasound condition to add
Add agent, ripening 1-5 days under stirring condition obtains complex function colloidal sol；
The step of spraying: complex function colloidal sol is sprayed on the inorganic multi-stage porous matrix surface that temperature is 100-250 DEG C, so
Afterwards 300-600 DEG C at a temperature of, be heat-treated 10-120 minutes.
As further embodiment, in the step of spraying, the complex function colloidal sol is in inorganic multi-stage porous matrix
The mass content on surface is 0.1-50g/m2。
It is specific embodiment of the present invention below, used raw material, equipment etc. remove special limit in the following embodiments
It can be obtained by buying pattern outside fixed.
Embodiment 1 is a kind of with adsorption-decomposition function pernicious gas+dehumidifying damping+deodorization complex function multi-stage porous ceramic material
The multi-stage porous ceramic material with complex function, is sprayed on by inorganic multi-stage porous matrix and by complex function colloidal sol
The complex function thin film of inorganic multi-stage porous matrix surface forms；The complex function thin film is by titanium dioxide, functional additive (oxygen
Change zinc nanoparticles/cluster), acidic aqueous solution is prepared；The functional additive is selected from Zinc oxide nanoparticle/cluster.
The preparation method of the multi-stage porous ceramic material, includes the following steps:
The step of preparing inorganic multi-stage porous matrix: inorganic multi-stage porous matrix is 1 He of inoganic solids powder of 3:1 with weight ratio
Inoganic solids powder 2 is raw material, is made through granulation, molding, 600-900 DEG C；Inoganic solids powder 1 is diatomite, inorganic
Solid powder 2 is bentonite.The aperture of the porous, inorganic matrix is 20nm-30nm.
The step of preparing complex function colloidal sol: secure ph is the aqueous solution of 1-3, obtains acidic aqueous solution；Titanium salt will be contained
It is scattered in dehydrated alcohol, obtains titanium solution；The titanium salt that contains is butyl titanate, and the dosage containing titanium salt is 0.5g/L.?
Under stirring, cryogenic conditions, the speed of the stirring is 800r/min, and the cryogenic conditions are 25 DEG C, and resulting titanium solution is delayed
Slowly it is added in acidic aqueous solution, obtains titaniferous aqueous solution；Under stirring, ultrasound condition, the speed of the stirring is 800r/
Min, the ultrasound condition are 35KHz；The Zinc oxide nanoparticle/cluster functional additive dosage is 0.05g/L, toward institute
Titaniferous aqueous solution in Zinc oxide nanoparticle/cluster functional additive is added, ripening 1-5 days under stirring condition, obtain
To complex function colloidal sol；
The step of spraying: complex function colloidal sol is sprayed on the inorganic multi-stage porous matrix surface that temperature is 100 DEG C, is then existed
At a temperature of 300 DEG C, it is heat-treated 10 minutes.The complex function colloidal sol is in the mass content of inorganic multi-stage porous matrix surface
0.1g/m2。
Embodiment 2 is a kind of with adsorption-decomposition function pernicious gas+dehumidifying damping+deodorization+antibacterial complex function multi-stage porous pottery
Ceramic material
The multi-stage porous ceramic material with complex function, as shown in Figure 1, by inorganic multi-stage porous matrix and by complex function
Colloidal sol is sprayed on the complex function thin film composition of inorganic multi-stage porous matrix surface；The complex function thin film is by titanium dioxide, function
Energy additive, acidic aqueous solution are prepared；The functional additive is selected from Zinc oxide nanoparticle/cluster, halogenation silver nanoparticle
Particle/cluster composition, Zinc oxide nanoparticle/cluster, halogenation silver nano-grain/cluster volume ratio are 4:1.
The preparation method of the multi-stage porous ceramic material, includes the following steps:
The step of preparing inorganic multi-stage porous matrix: inorganic multi-stage porous matrix is 1 He of inoganic solids powder of 1:1 with weight ratio
Inoganic solids powder 2 is raw material, is made through granulation, molding, 600-900 DEG C；Inoganic solids powder 1 is diatomite, inorganic
Solid powder 2 is zeolite.The aperture of the porous, inorganic matrix is 16nm-30nm.
The step of preparing complex function colloidal sol: secure ph is the aqueous solution of 1-3, obtains acidic aqueous solution；Titanium salt will be contained
It is scattered in anhydrous alcohol solution, obtains titanium solution；The titanium salt that contains is butyl titanate, and the dosage containing titanium salt is 4g/L.?
Under stirring, cryogenic conditions, the speed of the stirring is 800r/min, and the cryogenic conditions are 25 DEG C, and resulting titanium solution is delayed
Slowly it is added in acidic aqueous solution, obtains titaniferous aqueous solution；Under stirring, ultrasound condition, the speed of the stirring is 800r/
Min, the ultrasound condition are 35KHz；Zinc oxide nanoparticle/the cluster, halogenation silver nano-grain/cluster functional additive
Dosage be respectively 0.8g/L, 0.2g/L, functional additive is added into resulting titaniferous aqueous solution, under stirring condition at ageing
Reason 1-5 days, obtains complex function colloidal sol；
The step of spraying: complex function colloidal sol is sprayed on the inorganic multi-stage porous matrix surface that temperature is 150 DEG C, is then existed
At a temperature of 350 DEG C, it is heat-treated 20 minutes.The complex function colloidal sol is in the mass content of inorganic multi-stage porous matrix surface
1g/m2。
Embodiment 3 is a kind of with adsorption-decomposition function pernicious gas+dehumidifying damping+deodorization complex function multi-stage porous ceramic material
A kind of multi-stage porous ceramic material with complex function, sprays by inorganic multi-stage porous matrix and by complex function colloidal sol
It is formed in the complex function thin film of inorganic multi-stage porous matrix surface；The complex function thin film by titanium dioxide, functional additive,
Acidic aqueous solution is prepared；The functional additive be selected from copper oxide nanometer particle/cluster, halogenation silver nano-grain/cluster,
Pucherite nano particle/cluster composition.Copper oxide nanometer particle/cluster, halogenation silver nano-grain/cluster, pucherite nanometer
Particle/cluster is 1:1:1 with volume ratio.
The preparation method of the multi-stage porous ceramic material, includes the following steps:
The step of preparing inorganic multi-stage porous matrix: inorganic multi-stage porous matrix is 1 He of inoganic solids powder of 2:1 with weight ratio
Inoganic solids powder 2 is raw material, is made through granulation, molding, 600-900 DEG C；Inoganic solids powder 1 is sepiolite, inorganic
Solid powder 2 is montmorillonite.The aperture of the porous, inorganic matrix is 22nm-32nm.
The step of preparing complex function colloidal sol: secure ph is the aqueous solution of 1-3, obtains acidic aqueous solution；Titanium salt will be contained
It is scattered in anhydrous alcohol solution, obtains titanium solution；The titanium salt that contains is butyl titanate, and the dosage containing titanium salt is 50g/L.?
Under stirring, cryogenic conditions, the speed of the stirring is 800r/min, and the cryogenic conditions are 25 DEG C, and resulting titanium solution is delayed
Slowly it is added in acidic aqueous solution, obtains titaniferous aqueous solution；Under stirring, ultrasound condition, the speed of the stirring is 800r/
Min, the ultrasound condition are 35KHz；The dosage of complex function additive is 8g/L, is added into resulting titaniferous aqueous solution
Functional additive obtains complex function colloidal sol ripening 1-5 days under stirring condition；
The step of spraying: complex function colloidal sol is sprayed on the inorganic multi-stage porous matrix surface that temperature is 200 DEG C, is then existed
At a temperature of 500 DEG C, it is heat-treated 60 minutes.The complex function colloidal sol is in the mass content of inorganic multi-stage porous matrix surface
25g/m2。
Embodiment 4: one kind having adsorption-decomposition function pernicious gas+dehumidifying damping+ deodorizationThe multi-stage porous of+antiallergy complex function
Ceramic material
A kind of multi-stage porous ceramic material with complex function, sprays by inorganic multi-stage porous matrix and by complex function colloidal sol
It is formed in the complex function thin film of inorganic multi-stage porous matrix surface；The complex function thin film is by titanium dioxide, photo-catalysis function
Additive, acidic aqueous solution and gallic acid with anti-allergic effects, tannic acid, polyvinyl alcohol and polyvinyl phenol it is anti-
Allergy functional additive is prepared；The photo-catalysis function additive is copper oxide nanometer particle/cluster, cupric oxide nano
Grain/cluster is 1:1 with volume ratio.The volume ratio of gallic acid, polyvinyl alcohol and polyvinyl phenol in antianaphylaxis function additive
For 2:2:1.
The preparation method of the multi-stage porous ceramic material, includes the following steps:
The step of preparing inorganic multi-stage porous matrix: inorganic multi-stage porous matrix is 1 He of inoganic solids powder of 5:1 with weight ratio
Inoganic solids powder 2 is raw material, is made through granulation, molding, 600-900 DEG C；Inoganic solids powder 1 is allophane, nothing
Machine solid powder 2 is bentonite.The aperture of the porous, inorganic matrix is 16nm-32nm.
The step of preparing complex function colloidal sol: secure ph is the aqueous solution of 1-3, obtains acidic aqueous solution；Titanium salt will be contained
It is scattered in anhydrous alcohol solution, obtains titanium solution；The titanium salt that contains is butyl titanate, and the dosage containing titanium salt is 50g/L.?
Under stirring, cryogenic conditions, the speed of the stirring is 800r/min, and the cryogenic conditions are 25 DEG C, and resulting titanium solution is delayed
Slowly it is added in acidic aqueous solution, obtains titaniferous aqueous solution；Continue the function that addition has anti-allergic effects in above-mentioned phthalein solution
It can additive.Under stirring, ultrasound condition, the speed of the stirring is 800r/min, and the ultrasound condition is 35KHz；It is described
The dosage of functional additive is 25g/L, the addition photo-catalysis function additive into resulting titaniferous aqueous solution, old under stirring condition
Change processing 1-5 days, obtains complex function colloidal sol；
The step of spraying: complex function colloidal sol is sprayed on the inorganic multi-stage porous matrix surface that temperature is 250 DEG C, is then existed
At a temperature of 600 DEG C, it is heat-treated 120 minutes.The complex function colloidal sol is in the mass content of inorganic multi-stage porous matrix surface
50g/m2。
Effect assessment and performance detection
1. being verifying example, the ability of observation multi-stage porous ceramic material degradation rhodamine with embodiment 1-4.
Detection method is as follows: take four groups of test tubes, every group of test tube contains 7 test tubes, be separately added into the rhodamine of equivalent with
The water of equivalent is dissolved, then the complex function colloidal sol in the corresponding embodiment 1-4 that equivalent is added, in ultraviolet-visible light spoke
After 0min, 5min, 10min, 20min, 30min, 45min, 60min, observation complex function colloidal sol degrades to rhodamine
Decolorizing effect afterwards, and describe decoloration curve, the abscissa for the curve that decolourizes is light application time, and ordinate is that rhodamine is dense
Degree, as a result referring to fig. 2-6.
Fig. 2 is that 2 multi-stage porous ceramic material of the embodiment of the present invention degrades rhodamine aqueous solution with ultraviolet-visible light spoke
Take time extended decoloration picture；As seen from Figure 2, with the extension of ultraviolet-visible light irradiation time, complex function colloidal sol
To rhodamine degradation after decolorizing effect be more obvious, illustrate complex function colloidal sol of the invention can degrade rhodamine dye
Material is applied on specific inorganic multi-stage porous matrix, the applicable scene of its product can be made to add extensively.
Fig. 3 is rhodamine aqueous solution of degrading under 1-4 of embodiment of the present invention multi-stage porous ceramic material ultraviolet-visible light
Decolourize curve.As seen from Figure 3, embodiment 1-4 multi-stage porous ceramic material can degrade Luo Dan in rhodamine aqueous solution
Bright dyestuff.
Fig. 4 is nitrogen adsorption-desorption curve of 2 multi-stage porous ceramic material of the embodiment of the present invention；Specific surface as seen from Figure 4
Product is probably in 82.1295m2/g,.Hysteresis loop, which is begun with, in relative pressure 0.5 illustrates that hole is bigger.What higher-pressure region adsorbance rose
Comparatively fast, illustrate that macropore is relatively more, belong to IV type adsorption isotherm, aperture size is larger and distribution is relatively wide.
Fig. 5 is the pore size distribution curve of 2 multi-stage porous ceramic material of the embodiment of the present invention；The aperture of material as seen from Figure 5
For size range in 16nm-32nm, the absorption property of material is stronger.At this point, the main pore structure of material is mesoporous, and Jie
Hole aperture is inhomogenous.
Fig. 6 is the electron scanning micrograph of 2 multi-stage porous ceramic material of the embodiment of the present invention.By clearly visible in Fig. 6
The hole for having many sizes inhomogenous to multi-stage porous ceramic material surfaces.
2. being verifying example with embodiment 1-4, the ability of multi-stage porous ceramic material degradation of formaldehyde is observed
Test method is as follows:
1. experimental condition: carrying out test purification product removal gas with two Laboratory Modules (A is blank cabin, and B is sample chamber)
The concentration of polluter.2. experimental condition carries out at normal temperatures and pressures.The preparation of pollution sources: with the medical degreasing of 17cm*40cm
Reagent bottle of 500ml is fixed with cotton thread and be uprightly placed on it to 5 layers of gauze volume on 2 diameter 5mm, the glass bar of long 30cm
In, it is packed into 200ml, the formaldehyde that concentration is 0.2%.And container is pasted A1、B1.3. experimental procedure: sample is put into sample chamber B,
By the container A of the pollutant source of release prepared1And B1It is respectively placed in blank assay cabin A and sampling test cabin B, closes cabin immediately
Door.The fan of Laboratory Module is opened, so that air in cabin is simultaneously closed off wind with after the pollutant mixing of source of release release after opening 1min
Fan, samples the air in blank cabin, and the concentration value for measuring pollutants in air in blank cabin is initial concentration, is denoted as
C0.The pollutant concentration in two cabins is sampled after 24H, analysis test, the concentration value in the cabin A, B as in certain time period,
It is denoted as CAWith CB.Scavenging material is to pollutants removal rate according to formula
In formula:
Y-removal rate, %；
CA- blank assay cabin pollutant concentration value, mg/m3；
CBPollutant concentration value, mg/m in-sample chamber3；
Test result and analysis:
Table 1 is the aptitude tests result of embodiment 1-4 multi-stage porous ceramic material degradation of formaldehyde
As shown in table 1, blank cabin concentration of formaldehyde value is 1.08mg/m after test result is for 24 hours3, sample chamber concentration of formaldehyde value
0.04~0.07mg/m3, formaldehyde removal rate is 93.5~96.3% for 24 hours.
3. being verifying example with embodiment 2, the ability of multi-stage porous ceramic material antibacterial is observed
Test method is as follows: 1. tests use plate culture, and culture on certain colony inoculation to measuring samples is acted on
Certain time observes its clump count (cfu), calculates antibacterial product to the antibiotic rate of bacterium.Staphylococcus aureus is prepared first
With the culture medium of Escherichia coli, 85% physiological saline and phosphate buffer are then configured.2. operating method: 2.1 breakdown standards
Strain inoculated 3-4 branch on nutrient agar slopes in test tube, being placed in 36 DEG C of ± 1 DEG C of insulating boxs and cultivating 18~20h is the first generation,
2~8 DEG C are placed on to save backup.It takes first generation strain to be directly inoculated with nutrient agar slopes, is cultivated in 36 DEG C of ± 1 DEG C of insulating boxs
18~20h continuously reaches the third generation as experiment strain.Strain is scraped off dilution as bacterium standard by 2.2 preparation bacterium solutions
Opacity tube concentration is identical, and as 5 × 108A bacterium/ml.Then 1.0 × 10 are diluted to8After a bacterium/ml, carries out 10 times and be serially diluted
10-1~10-6Various concentration bacterium solution.2.3 take 10-1Dilution bacterium solution 0.1ml is directly inoculated in nutrient agar plate, is done 3 and is put down
For 24 hours in 36 DEG C of ± 1 DEG C of cultures, clump count is 0h clump count to ware.Take above-mentioned 10-3Dilution bacterium solution 0.5ml is inoculated in 50mm respectively
The surface of test piece of × 50mm is simultaneously paved, and is covered surface of test piece with insurance plastic film, is kept 90% or more humidity, make surface of test piece
Bacterium solution is not done after for 24 hours.Set 36 DEG C of ± 1 DEG C of cultures for 24 hours.Test specimen after taking culture for 24 hours, respectively will examination with 9.5ml physiological saline
Bacterium solution on part is flushed in sterilizing plates, is diluted to 5000~10000 bacterium/ml after mixing.At 5000~10000
1~2 signal bacterial concentration is selected between bacterium/ml, and 0.1ml is respectively taken to make clump count (cfu) calculating.Each dilution is inoculated with nutrition fine jade
Rouge plate three, result is observed for 24 hours in 36 DEG C of ± 1 DEG C of cultures.
In formula: the clump count on test specimen that A-is cultivated for 24 hours；
Clump count on B-" 0 " time of contact test specimen.
Test result and analysis: after tested the result shows that: the antibiotic rate of Escherichia coli be 99.27%, Staphylococcus aureus
The antibiotic rate of bacterium is 99.25%.
4. being verifying example with embodiment 3, the ability of multi-stage porous ceramic material deodorization is observed
Test method is as follows: 1. experimental conditions: carrying out test purification with two Laboratory Modules (A is blank cabin, and B is sample chamber)
The concentration of product removal gas pollutant.2. experimental condition carries out at normal temperatures and pressures.The preparation of pollution sources: 17cm* is used
5 layers of the medical absorbent cotton/gauze volume of 40cm are fixed with cotton thread on 2 diameter 5mm, the glass bar of long 30cm and are uprightly placed on it
In the reagent bottle of 500ml, it is packed into 200ml, the ammonia that concentration is 1%.And container is pasted A1、B1.3. experimental procedure: sample is put into
In sample chamber B, by the container A of the pollutant source of release prepared1And B1It is respectively placed in blank assay cabin A and sampling test cabin B,
Hatch door is closed immediately.The fan of Laboratory Module is opened, is made in cabin after the pollutant mixing of air and source of release release after opening 1min,
Fan is simultaneously closed off, the air in blank cabin is sampled, the concentration value for measuring ammonia in air in blank cabin is initial concentration,
It is denoted as C0.The concentration of the ammonia in two cabins is sampled after 24H, analysis test, the concentration in the cabin A, B as in certain time period
Value, is denoted as CAWith CB.4. sampling step:
Scavenging material is to pollutants removal rate according to formula
In formula:
Y-removal rate, %；
CA- blank assay cabin pollutant concentration value, mg/m3；
CBPollutant concentration value, mg/m in-sample chamber3；
Test result and analysis: blank cabin ammonia density value is 2.01mg/m after for 24 hours3, sample chamber ammonia density value 0.2mg/m3,
Ammonia removal rate is 90.0% for 24 hours.
5. being verifying example with embodiment 4, the damping of multi-stage porous ceramic material and antianaphylactic ability are observed
Test method is as follows: the temperature in constant temperature humidity chamber is set as (23 ± 0.5) DEG C.Selection is in low humidity shape first
It is tested under state, maintenance humidity is set as 30%, and moisture absorption process humidity is 55%, and humidity is maintained at 30% during moisture releasing.Conserve 2h
Samples weighing (m afterwards0) and be put under 55% damp condition and keep for 24 hours.Weight (the m of sample after measurement for 24 hoursa).Then quickly
Humidity in case is adjusted to 30% from 55%, keeps for 24 hours, then measuring the weight (m of sample at this timed)。
Antianaphylactic test: it is adsorbed on the solid phase carriers such as polystyrene, is immunized with soluble antigen or antibody
The qualitative and quantitative approach of reaction.That is elisa enzyme-linked immunosorbent assay method.
Test result and analysis: 3h hygroscopic capacity is 46 × 10-3kg/m2, 6h hygroscopic capacity is 88 × 10-3kg/m2, 12h moisture absorption
Amount is 121 × 10-3kg/m2, hygroscopic capacity is 171 × 10 for 24 hours-3kg/m2.Comply with standard and remote overproof hygroscopic capacity >=25 3h ×
10-3kg/m2, hygroscopic capacity >=35 × 10 6h-3kg/m2, hygroscopic capacity >=55 × 10 12h-3kg/m2, hygroscopic capacity >=60 × 10 for 24 hours-3kg/
m2.Moisture releasing amount is 124 × 10 for 24 hours-3kg/m2
Test result shows that Elisa concentration is less than 1ng/ml after the test of elisa antiallergy, and galla turcica is used alone
The result of acid is greater than 5ng/ml.
The above embodiment is only the preferred embodiment of the present invention, and the scope of protection of the present invention is not limited thereto,
The variation and replacement for any unsubstantiality that those skilled in the art is done on the basis of the present invention belong to institute of the present invention
Claimed range.
Claims (10)
1. a kind of multi-stage porous ceramic material with complex function, which is characterized in that by inorganic multi-stage porous matrix and by compound function
Energy colloidal sol is sprayed on the complex function thin film composition of inorganic multi-stage porous matrix surface；The complex function colloidal sol is by containing titanium salt, acid
Property aqueous solution, functional additive are prepared；The functional additive is selected from Zinc oxide nanoparticle/cluster, cupric oxide nano
Particle/cluster, halogenation silver nano-grain/cluster, pucherite nano particle/cluster, graphite phase carbon nitride nano particle/cluster,
Silver/copper nanocrystallite, gallic acid, polyvinyl alcohol, two or more different function in polyvinyl phenol compound.
2. as described in claim 1 with the multi-stage porous ceramic material of complex function, which is characterized in that the inorganic multi-stage porous
Matrix is made using a variety of inoganic solids powder as raw material through granulation, molding, 600-900 DEG C；The inoganic solids powder is selected from
Diatomite, allophane, montmorillonite, Emathlite, bentonite, zeolite, attapulgite, sepiolite, flyash, waste gypsum, rubbish
Rubbish burns the composition of one or more of ash content, float stone, medical stone, tourmaline, rutile.
3. as described in claim 1 with the multi-stage porous ceramic material of complex function, which is characterized in that the inorganic multi-stage porous
The aperture of matrix is distributed in nanometer scale to submillimeter magnitude.
4. as described in claim 1 with the multi-stage porous ceramic material of complex function, which is characterized in that the complex function is molten
The preparation method of glue the following steps are included:
The step of preparing acidic aqueous solution: acid is added in aqueous solution, obtains acidic aqueous solution；
The step of preparing titanium solution: it disperses titaniferous salt in dehydrated alcohol, obtains titanium solution；
The step of mixing: under stirring, 5-40 DEG C of cryogenic conditions, resulting titanium solution is slowly added into acidic aqueous solution
In, obtain titaniferous aqueous solution；
The step of functional additive is added: functional additive is added into resulting titaniferous aqueous solution under stirring, ultrasound condition；
Under stirring condition, 5-40 DEG C ripening 1-5 days, obtain complex function colloidal sol；
The step of cryo-conservation: it will be saved under 5-40 DEG C of low temperature after the encapsulation of complex function colloidal sol, be stand-by.
5. as claimed in claim 4 with the multi-stage porous ceramic material of complex function, which is characterized in that acid water-soluble preparing
In the step of liquid, acid mixed acid one or more kinds of in acetic acid, hydrochloric acid, sulfuric acid, the acidic aqueous solution
PH value is 1-5.
6. as claimed in claim 4 with the multi-stage porous ceramic material of complex function, which is characterized in that preparing titanium solution
It is described to be selected from one or more of butyl titanate, titanium tetrachloride, titanium tetraisopropylate, isopropyl titanate containing titanium salt in step,
The dosage containing titanium salt is 0.5-50g/L.
7. as claimed in claim 4 with the multi-stage porous ceramic material of complex function, which is characterized in that in the step of mixing
In, the speed of the stirring is 500-1000rpm, and the cryogenic conditions are 5-40 DEG C.
8. as claimed in claim 4 with the multi-stage porous ceramic material of complex function, which is characterized in that function addition is being added
In the step of agent, the speed of the stirring is 500-1000rpm, and the ultrasound condition is 20-40KHz；The functional additive
Dosage be 0.05-25g/L.
9. a kind of preparation method of the multi-stage porous ceramic material with complex function, which comprises the steps of:
The step of preparing inorganic multi-stage porous matrix: the inorganic multi-stage porous matrix is using a variety of inoganic solids powder as raw material, through making
Grain, molding, 600-900 DEG C be made；
The step of preparing complex function colloidal sol: secure ph is the aqueous solution of 1-5, obtains acidic aqueous solution；Titaniferous salt is dispersed
In dehydrated alcohol, titanium solution is obtained；Under stirring, 5-40 DEG C of cryogenic conditions, resulting titanium solution is slowly added into acid
In property aqueous solution, titaniferous aqueous solution is obtained；Function addition is added into resulting titaniferous aqueous solution under stirring, ultrasound condition
Agent obtains complex function colloidal sol ripening 1-5 days under stirring condition；
The step of spraying: complex function colloidal sol is sprayed on the inorganic multi-stage porous matrix surface that temperature is 100-250 DEG C, is then existed
It is heat-treated 10-120 minutes at a temperature of 300-600 DEG C.
10. preparation method as claimed in claim 9, which is characterized in that in the step of spraying, the complex function colloidal sol exists
The mass content of inorganic multi-stage porous matrix surface is 0.1-50g/m2。
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