CN108530039A - A kind of formula of ceramic membrane and preparation method thereof of load nano cupric oxide - Google Patents
A kind of formula of ceramic membrane and preparation method thereof of load nano cupric oxide Download PDFInfo
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- CN108530039A CN108530039A CN201810468564.6A CN201810468564A CN108530039A CN 108530039 A CN108530039 A CN 108530039A CN 201810468564 A CN201810468564 A CN 201810468564A CN 108530039 A CN108530039 A CN 108530039A
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Abstract
The invention discloses a kind of formulas of ceramic membrane and preparation method thereof of load nano cupric oxide, the ceramic membrane point includes supporter and separation membrane layer, the supporter includes major ingredient and auxiliary material, the major ingredient of the supporter is one or more of aluminium oxide, mullite, dolomite, bauxite, and the supporter auxiliary material is sintering aid, plasticizer, pore creating material and binder；The dispensing of the separation membrane layer is adhesive, nano cupric oxide particle, dispersant and plasticiser.The ceramic membrane of load nano cupric oxide prepared by the present invention, the material of supporter is simple and easy to get, and material has antibacterial, catalysis, the superperformances such as pore size is flexibly controllable, and the mechanical property of materials is excellent, coefficient of thermal expansion is low.
Description
Technical field
The present invention relates to inorganic ceramic membrane field, it is specifically a kind of load nano cupric oxide ceramic membrane formula and
Preparation method.
Background technology
Inorganic ceramic membrane is a kind of inorganic or high molecular material with special Selective Separation function, it can be fluid point
Two parts being not communicated with are divided into, one such or several substances is enable to penetrate, and other materials are separated.Due to nothing
Machine ceramic membrane has that high temperature resistant, acid and alkali-resistance, regenerability be good, technical advantage with long service life, has been widely used in doctor
The fields such as medicine, water process, chemical industry, electronics, food processing.
Generally use aluminium oxide, aluminium hydroxide, silica, silicon carbide, silicon nitride, which are used as, in the prior art prepares ceramic membrane
The material of main part of supporter.The mainstream that ceramic film support is existing ceramic membrane is prepared using aluminium oxide, aluminium hydroxide, silica
Technique, ceramic membrane uniform pore diameter, moderate cost made from such technique；Ceramic membrane tool is prepared using silicon carbide, silicon nitride simultaneously
There are the advantages such as high mechanical strength, thermal shock resistance be good.But due to using aluminium oxide, aluminium hydroxide, silica, silicon carbide, nitrogen
The ceramic membrane as the material of main part for preparing ceramic film support such as SiClx, preparation process is more stringent, due to needing in nitrogen
Supporter raw material are prepared under compression ring border, production technology cost is too big, and the cost of raw material silicon carbide is higher, in practical applications
Do not have the condition being widely popularized also.So support body material is simple and easy to get, simple production process, ceramic membrane effect is preferably produced
Product and technique, it is eager required for market.
Invention content
The purpose of the present invention is to provide a kind of support body material is simple and easy to get, simple production process, ceramic membrane effect compared with
The formula of ceramic membrane and preparation method thereof of good load nano cupric oxide, to solve the problems of the prior art.
To achieve the above object, the present invention provides the following technical solutions：A kind of ceramic membrane of load nano cupric oxide
Formula, the ceramic membrane point includes supporter and separation membrane layer, includes nano cupric oxide in the separation membrane layer dispensing
Particle.Nano cupric oxide particle has good antimicrobial acivity, and nano cupric oxide particle is added in separating layer, is had
Catalytic action, while there is fungistatic effect.
As an optimization, the major ingredient of the supporter is aluminium oxide, mullite, dolomite, one or more of bauxite,
The supporter auxiliary material is sintering aid, plasticizer, pore creating material and binder；The dispensing of the separation membrane layer is adhesive, receives
Rice copper oxide particle, dispersant and plasticiser.Aluminium oxide, mullite, dolomite, bauxite are simple and easy to get, and cost is relatively low.
As an optimization, sintering aid is kaolin in the supporter auxiliary material, plasticizer is basic magnesium carbonate, pore creating material is
Cornstarch, binder are PVA-1750 solution；Adhesive is hydroxyethyl cellulose in the separation membrane layer dispensing, dispersant is
Ammonium polymethacrylate, plasticiser are polyethylene glycol.Pass through sintering aid, plasticizer, pore creating material, binder and oxygen in supporter
Change these major ingredients such as aluminium, mullite, dolomite, bauxite to be coordinated, the ceramic membrane finally fired is made to be tied with good hole
Structure, uniform pore diameter is fine and close, and service life is very long, and material cost greatly reduces.And adhesive, dispersion in separation membrane layer
The combination of agent, plasticiser etc. and nano cupric oxide particle can be good at being combined with supporter, significantly improve the separation property of film
Energy.
As an optimization, the grain size of the supporter major ingredient is 0.1-500 μm, and the grain size of the sintering aid is 1-3 μm, institute
It is 1-80 μm to state pore creating material grain size, and the grain size of the nano cupric oxide particle is 10-1000nm.Select suitable dispensing and its
Thickness characteristics contribute to form high standard, the higher ceramic membrane of product quality, greatly improve product qualification rate.
As an optimization, the grain size of the supporter major ingredient is 0.1-100 μm, and the pore creating material grain size is 1-20 μm, described
The grain size of nano cupric oxide particle is 10-100nm.
As an optimization, the supporter major ingredient dosage is 70%-95% (wt), nano oxidized in the separation membrane layer dispensing
Copper particle mass concentration is 0.5-2%.
As an optimization, the supporter major ingredient dosage is 70%-95% (wt), and sintering aid and plasticizer share in auxiliary material
Amount is 1%-10% (wt), pore creating material dosage is 1%-20% (wt), consumption of binder is 1%-15% (wt)；The seperation film
Layer dispensing dosage be mass concentration be 40-60% adhesives, 0.5-2% nano cupric oxides particle, 40-60% dispersant and
The plasticiser of 1-4%.The dosage of supporter major ingredient will have a direct impact on the service life of ceramic membrane, and dosage leads to ceramics too much
Film is very crisp, and dosage is very little, and support effect will reduce, and the proportioning of suitable major ingredient and supplementary product consumption ensure that product mechanicalness
Can be excellent, triadic mean bending strength is up to 20MPa or more；And in separating layer dispensing dosage, affect separating layer and supporter
Laminating degree, while also to ensure the dosage of nano cupric oxide, to ensure catalysis, the fungistatic effect of product.
A kind of preparation method of the ceramic membrane of load nano cupric oxide, steps are as follows：
(1) preparation of supporter：It is ground after sintering aid, plasticizer are mixed with distilled water, then mixed with supporter major ingredient
Close uniform, material to be mixed is lightly ground after being completely dried, and pore creating material and binder is added in grinding while, eventually forms supporter
Dispensing；Then supporter dispensing is prepared into scale ceramic film support using extrusion moulding；Ceramic film support is dried
Afterwards, it is sintered in the electric furnace of temperature programmed control, then cooled to room temperature；
(2) preparation of plasma separation membrane：Nano cupric oxide particle is dispersed to ultrasonic method in dispersant, then with constant
Plasticiser is added in copper oxide suspension by medium speed, and bubble removing is removed after stirring a period of time；Then adhesive is added
Into water, at room temperature after low speed ramps up mixing to middling speed, slowly it is added in copper oxide suspension and mixes for use；
(3) coating of separation membrane layer：The ceramic film support that step (1) is obtained is with after hot water injection, in acetone phase
Ultrasound, drying；Then ceramic film support one side is sealed with paraffin, another side polishing cleaning；Then again using lifting dipping
Plasma separation membrane prepared by step (2) is polished coated in ceramic film support in the side of cleaning by method, after taking out drying, then
Secondary film and drying are carried out, then finished product.
As an optimization, the sintering temperature of ceramic film support is 1000-1500 DEG C in the step (1), is sintered to 1-3h.
Temperature and sintering time ensure that the mechanical performance and service life of supporter.
As an optimization, mixing time removes bubble removing after being 18-36h in the step (2), seperation film in the step (3)
Slurry is coated on ceramic film support and is dried again after 10-60s.
Compared with prior art, the beneficial effects of the invention are as follows：
1, the supporter major ingredient of ceramic membrane of the present invention is using aluminium oxide, mullite, dolomite, bauxite, these materials
Material is conveniently easy to get, and reduces the material cost of ceramic membrane；
2, the separating layer of ceramic membrane of the present invention adds nano cupric oxide particle, has catalytic action, while having antibacterial effect
Fruit；Nano cupric oxide particle is dispersed to ultrasonic method in dispersant simultaneously, then is added plasticiser with constant medium speed
Into copper oxide suspension, the uniformity of nano cupric oxide particle dispersion is ensure that, to improve the quality of ceramic membrane.
3, the ceramic membrane that the formula by the present invention and preparation method obtain, average pore size are 0.5-30 μm, porosity
30-60%, in the micron-scale between nanoscale, aperture can be flexibly controllable by technique for uniform pore diameter densification, pore size, production
Quality is effectively guaranteed；
4, preparation process of the invention has first carried out the sintering of supporter, has prepared, and is sintered in the electric furnace of common temperature control
, there is no strict requirements to sintering environment, instead of present sintering technology, that is, need to prepare supporter in a nitrogen environment
Technique, production technology substantially reduces, and operation is also very succinct；The preparation of plasma separation membrane ensure that the work(of separation membrane layer simultaneously
Under the premise of effect is not destroyed, every component has obtained good dispersion and integration, is finally separating the coating processes of film layer, will detach
Film slurry uniformly coated in the technology on supporter, being different from existing pressing seperation film, also ensures separation membrane layer in supporter
Upper good adhesive force, is not in demoulding, broken situation, increases the service life of ceramic membrane, while substantially reducing film
Energy consumption in preparation process；
5, ceramic membrane prepared by the present invention, mechanical performance is excellent, and triadic mean bending strength is also solved up to 20MPa or more
The low problem of coefficient of thermal expansion of having determined, service life greatly increase.
In conclusion the ceramic membrane of load nano cupric oxide prepared by the present invention, the material of supporter is simple and easy to get,
Material has antibacterial, catalysis, the superperformances such as pore size is flexibly controllable, and the mechanical property of materials is excellent, coefficient of thermal expansion is low.
Specific implementation mode
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.
Embodiment 1：
The preparation of the ceramic membrane of nano cupric oxide is loaded, steps are as follows：
(1) preparation of supporter：After 5% (wt), the kaolin that grain size is 2 μm, basic magnesium carbonate are mixed with distilled water
Grinding, then be uniformly mixed with the aluminium oxide of 85% (wt) and mullite material, material to be mixed is lightly ground after being completely dried, grinding
1000 mesh sieve is crossed afterwards, it is 2 μm of pore creating material cornstarch, 5% binder PVA-1750 solution simultaneously mixing that 5%, grain size, which is then added,
Eventually form supporter dispensing；Then supporter dispensing is prepared into scale ceramic film support using extrusion moulding；By ceramic membrane
After supporter is dry in 105 DEG C, it is sintered 2h in the electric furnace of 1400 DEG C of constant temperature, then cooled to room temperature；Wherein supporter
The mass ratio of major ingredient aluminium oxide and mullite is 1:2.
After testing, sintered ceramic film support average pore size is 15 μm, porosity 30-40%, be averaged three-point bending resistance
Intensity is 24MPa, better mechanical property, and coefficient of thermal expansion is relatively low.
(2) preparation of plasma separation membrane：By mass concentration be 1%, the nano cupric oxide particle of grain size 20nm is with ultrasonic method
Be dispersed to mass concentration be 45% ammonium polymethacrylate in, then with constant medium speed by mass concentration be 4% poly- second
Glycol is added in copper oxide suspension, and bubble removing is removed in stirring afterwards for 24 hours；Then the hydroxyethyl cellulose for being 50% by mass concentration
It is added in water, at room temperature after low speed ramps up mixing to middling speed, is slowly added in copper oxide suspension and mixes
For use；
(3) coating of separation membrane layer：The ceramic film support that step (1) is obtained is with after hot water injection, in acetone phase
Ultrasound, drying；Then ceramic film support one side is sealed with paraffin, another side polishing cleaning；Then again using lifting dipping
Plasma separation membrane prepared by step (2) is polished coated in ceramic film support in the side of cleaning by method, film time control
In 20s, the dry 12h at 40-60 DEG C is then taken out, then carry out secondary film and drying, operating condition and a coating process
It is identical, it is made after dry 5h at 105 DEG C.
Embodiment 2：
The preparation of the ceramic membrane of nano cupric oxide is loaded, steps are as follows：
(1) preparation of supporter：After 10% (wt), the kaolin that grain size is 1 μm, basic magnesium carbonate are mixed with distilled water
Grinding, then be uniformly mixed with aluminium oxide, the dolomite material of 75% (wt), material to be mixed is lightly ground after being completely dried, grinding
800 mesh sieve is crossed afterwards, and it is 11 μm of pore creating material cornstarch, 10% binder PVA-1750 solution simultaneously mixing that 5%, grain size, which is added, most
Supporter dispensing is formed afterwards；Then supporter dispensing is prepared into scale ceramic film support using extrusion moulding；By ceramic membrane branch
After support body is dry in 105 DEG C, it is sintered 3h in the electric furnace of 1100 DEG C of constant temperature, then cooled to room temperature；Wherein supporter master
Expect that the mass ratio of aluminium oxide and dolomite is 1:1.
After testing, sintered ceramic film support average pore size is 18 μm, porosity 35-47%, be averaged three-point bending resistance
Intensity is 26MPa, better mechanical property, and coefficient of thermal expansion is relatively low.
(2) preparation of plasma separation membrane：By mass concentration be 0.8%, the nano cupric oxide particle of grain size 500nm is with ultrasound side
Method is dispersed to mass concentration, then with constant medium speed by mass concentration be 3% it is poly-
Ethylene glycol is added in copper oxide suspension, and bubble removing is removed after stirring 20h；Then the ethoxy for being 46.2% by mass concentration
Cellulose is added in water, at room temperature after low speed ramps up mixing to middling speed, is slowly added to copper oxide suspension
Middle mixing is for use；
(3) coating of separation membrane layer：The ceramic film support that step (1) is obtained is with after hot water injection, in acetone phase
Ultrasound, drying；Then ceramic film support one side is sealed with paraffin, another side polishing cleaning；Then again using lifting dipping
Plasma separation membrane prepared by step (2) is polished coated in ceramic film support in the side of cleaning by method, film time control
In 40s, the dry 12h at 40-60 DEG C is then taken out, then carry out secondary film and drying, operating condition and a coating process
It is identical, it is made after dry 5h at 105 DEG C.
Embodiment 3：
The preparation of the ceramic membrane of nano cupric oxide is loaded, steps are as follows：
(1) preparation of supporter：After 20% (wt), the kaolin that grain size is 3 μm, basic magnesium carbonate are mixed with distilled water
Grinding, then be uniformly mixed with the aluminium oxide of 70% (wt), dolomite and bauxite material, material to be mixed is gently ground after being completely dried
Mill, crosses 150 mesh sieve after grinding, it is 80 μm of pore creating material cornstarch, 8% binder PVA-1750 solution that 2%, grain size, which is then added,
And mixing, eventually form supporter dispensing；Then supporter dispensing is prepared into scale ceramic film support using extrusion moulding；It will
After ceramic film support is dry in 105 DEG C, it is sintered 1.5h in the electric furnace of 1300 DEG C of constant temperature, then cooled to room temperature；Its
The mass ratio of middle supporter major ingredient dolomite and bauxite is 1:2.
After testing, sintered ceramic film support average pore size is 90 μm, porosity 40-54%, be averaged three-point bending resistance
Intensity is 27MPa, better mechanical property, and coefficient of thermal expansion is relatively low.
(2) preparation of plasma separation membrane：By mass concentration be 1.5%, the nano cupric oxide particle of grain size 800nm is with ultrasound side
Method is dispersed to mass concentration, then with constant medium speed by mass concentration for 1.8%
Polyethylene glycol is added in copper oxide suspension, and bubble removing is removed after stirring 31h；Then the hydroxyl second for being 41.7% by mass concentration
Base cellulose is added in water, at room temperature after low speed ramps up mixing to middling speed, is slowly added to copper oxide suspension
It is mixed in liquid for use；
(3) coating of separation membrane layer：The ceramic film support that step (1) is obtained is with after hot water injection, in acetone phase
Ultrasound, drying；Then ceramic film support one side is sealed with paraffin, another side polishing cleaning；Then again using lifting dipping
Plasma separation membrane prepared by step (2) is polished coated in ceramic film support in the side of cleaning by method, film time control
In 37s, the dry 12h at 40-60 DEG C is then taken out, then carry out secondary film and drying, operating condition and a coating process
It is identical, it is made after dry 5h at 105 DEG C.
The coefficient of thermal expansion (10 of ceramic membrane of the present invention-6/ K) it see the table below：
| Temperature (DEG C) | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| 400 | 4.919 | 5.012 | 4.978 |
| 500 | 6.848 | 6.911 | 6.899 |
| 600 | 7.365 | 7.428 | 7.412 |
| 700 | 8.097 | 8.101 | 8.091 |
| 800 | 8.834 | 8.922 | 8.866 |
As can be seen from the table, the coefficient of expansion of ceramic membrane at different temperatures is less than the coefficient of expansion of existing ceramic membrane,
For the present invention during detecting the coefficient of expansion, there is not deformation in itself structure, aperture is not also affected, and makes simultaneously
Powerful guarantee is obtained with the service life.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Profit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent requirements of the claims
Variation is included within the present invention.Any label in claim should not be considered as and be limited the claims involved.
Claims (10)
1. a kind of formula of the ceramic membrane of load nano cupric oxide, the ceramic membrane point includes supporter and seperation film
Layer, it is characterised in that：It include nano cupric oxide particle in the separation membrane layer dispensing.
2. a kind of formula of the ceramic membrane of load nano cupric oxide according to claim 1, it is characterised in that：It is described
The major ingredient of supporter is one or more of aluminium oxide, mullite, dolomite, bauxite, and the supporter auxiliary material is sintering
Auxiliary agent, plasticizer, pore creating material and binder；The dispensing of the separation membrane layer be adhesive, nano cupric oxide particle, dispersant and
Plasticiser.
3. a kind of formula of the ceramic membrane of load nano cupric oxide according to claim 2, it is characterised in that：It is described
Sintering aid is kaolin in supporter auxiliary material, plasticizer is basic magnesium carbonate, pore creating material is cornstarch, binder PVA-
1750 solution；Adhesive is hydroxyethyl cellulose in the separation membrane layer dispensing, dispersant is ammonium polymethacrylate, plasticiser
For polyethylene glycol.
4. a kind of formula of the ceramic membrane of load nano cupric oxide according to claim 3, it is characterised in that：It is described
The grain size of supporter major ingredient is 0.1-500 μm, and the grain size of the sintering aid is 1-3 μm, and the pore creating material grain size is 1-80 μm,
The grain size of the nano cupric oxide particle is 10-1000nm.
5. a kind of formula of the ceramic membrane of load nano cupric oxide according to claim 4, it is characterised in that：It is described
The grain size of supporter major ingredient is 0.1-100 μm, and the pore creating material grain size is 1-20 μm, and the grain size of the nano cupric oxide particle is
10-100nm。
6. a kind of formula of the ceramic membrane of load nano cupric oxide according to any one of claim 1 to 5, special
Sign is：The supporter major ingredient dosage is 70%-95% (wt), nano cupric oxide granular mass in the separation membrane layer dispensing
A concentration of 0.5-2%.
7. a kind of formula of the ceramic membrane of load nano cupric oxide according to claim 6, it is characterised in that：It is described
Supporter major ingredient dosage is 70%-95% (wt), and it is 1%-10% (wt), pore-creating that sintering aid and plasticizer, which share amount, in auxiliary material
Agent dosage is 1%-20% (wt), consumption of binder is 1%-15% (wt)；The dosage of the separation membrane layer dispensing is that quality is dense
Degree is 40-60% adhesives, 0.5-2% nano cupric oxides particle, the dispersant of 40-60% and the plasticiser of 1-4%.
8. a kind of preparation method of the ceramic membrane of load nano cupric oxide, which is characterized in that steps are as follows：
(1) preparation of supporter：It grinds after sintering aid, plasticizer are mixed with distilled water, then is mixed with supporter major ingredient
Even, material to be mixed is lightly ground after being completely dried, and pore creating material and binder are added while grinding, eventually forms supporter and matches
Material；Then supporter dispensing is prepared into scale ceramic film support using extrusion moulding；After ceramic film support is dried,
It is sintered in the electric furnace of temperature programmed control, then cooled to room temperature；
(2) preparation of plasma separation membrane：Nano cupric oxide particle is dispersed to ultrasonic method in dispersant, then with constant medium
Plasticiser is added in copper oxide suspension by speed, and bubble removing is removed after stirring a period of time；Then adhesive is added to water
In, at room temperature after low speed ramps up mixing to middling speed, slowly it is added in copper oxide suspension and mixes for use；
(3) coating of separation membrane layer：The ceramic film support that step (1) is obtained with after hot water injection, in acetone phase ultrasound,
It is dry；Then ceramic film support one side is sealed with paraffin, another side polishing cleaning；Then it will be walked using lifting infusion process again
Suddenly the plasma separation membrane that prepared by (2) is polished coated in ceramic film support in the side of cleaning, after taking out drying, then carries out two
Secondary film and drying, then finished product.
9. a kind of preparation method of the ceramic membrane of load nano cupric oxide according to claim 8, it is characterised in that：
The sintering temperature of ceramic film support is 1000-1500 DEG C in the step (1), is sintered to 1-3h.
10. a kind of preparation method of the ceramic membrane of load nano cupric oxide according to claim 8 or claim 9, feature
It is：Mixing time removes bubble removing after being 18-36h in the step (2), and plasma separation membrane is coated in ceramics in the step (3)
It is dried again after 10-60s on film support.
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Application publication date: 20180914 |