CN106634154A - Stabilization method of diatomite/nanometer TiO2 photocatalytic paint additive - Google Patents
Stabilization method of diatomite/nanometer TiO2 photocatalytic paint additive Download PDFInfo
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- CN106634154A CN106634154A CN201611178899.1A CN201611178899A CN106634154A CN 106634154 A CN106634154 A CN 106634154A CN 201611178899 A CN201611178899 A CN 201611178899A CN 106634154 A CN106634154 A CN 106634154A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a stabilization method of a diatomite/nanometer TiO2 photocatalytic paint additive. A diatomite/nanometer TiO2 composite material is synthesized by using diatomite and tetrabutyl titanate as raw materials by an in-situ polymerization method. The method comprises the following steps that A, the diatomite, the tetrabutyl titanate and ethyl alcohol are mixed; stirring is performed for dissolution to obtain a mixed solution; B, the temperature is gradually raised, so that the ethyl alcohol is completely volatilized; water is added; then, heating is continuously preformed, so that moisture is volatilized to obtain dry solids; C, the dry solids are washed for many times; heating and drying are performed to obtain dry ingredients; the dry ingredients are calcined to obtain powder, i.e., the diatomite/nanometer TiO2 composite material; D, the diatomite/nanometer TiO2 composite material is infiltrated in a polystyrene solution; filtering and drying are performed, so that a polystyrene protection layer is formed on the surface of the composite materia, and the product of the diatomite/nanometer TiO2 photocatalytic coating additive is obtained. The composite material with a good formaldehyde removal function can be prepared by the method provided by the invention.
Description
Technical field
Present invention relates particularly to a kind of diatomite/nano-TiO2The stabilization method of light catalyzed coating additive.
Background technology
At present, simply composite made an addition in coating, it is easy to cause the inactivation of catalysis material, and may shadow
Ring the stability of coating.
The content of the invention
It is an object of the invention to provide diatomite/nano-TiO2The stabilization method of light catalyzed coating additive, solves
The low problem of existing catalysis material photocatalysis efficiency.
The present invention is achieved through the following technical solutions：
Diatomite/nano-TiO2The stabilization method of light catalyzed coating additive, with diatomite, butyl titanate as original
Material, using situ aggregation method diatomite/nano-TiO is synthesized2Composite, comprises the following steps：
A, by diatomite, butyl titanate, ethanol mixing, stirring and dissolving obtains mixed liquor；
B, it is gradually heating to make ethanol volatilize completely, adds water, then proceeding to heating makes moisture evaporation, obtains being dried solid
Body；
C, drying solid is washed for several times, heating, drying obtains dry ingredient, the calcining of this dry ingredient is obtained into powder, as
Diatomite/nano-TiO2Composite；
D, by diatomite/nano-TiO2Composite is infiltrated in polystyrene solution, after filtering drying so as to surface shape
Into polystyrene protective layer, product is obtained final product；Wherein, the particle diameter of products obtained therefrom is 50～100nm.
Above-mentioned synthetic method specifically includes following steps：
(1) diatomite is added in there-necked flask, it is slowly added to ethanol, butyl titanate in water bath with thermostatic control with 300～
The speed of 600r/min stirs 5～60min, obtains uniform mixed solution；
(2) being warming up to 50～90 DEG C of speed stirring mixed solutions with 300～600r/min makes ethanol volatilize, and adds
Water, is then heated to moisture evaporation, obtains drying solid；
(3) drying solid is washed for several times, is vacuum dried 6～16 hours at a temperature of 35～65 DEG C, finally 300～
Calcine 3～8 hours at a temperature of 600 DEG C, that is, obtain diatomite/nano-TiO2Composite；
(4) using styrene as monomer, n-BuLi is initiator, and triethoxysilane is that activity ends agent is obtained polyphenyl
Ethene, adds tetraethyl orthosilicate that the diatomite/nano-TiO of polystyrene protection is obtained by situ aggregation method2Composite.
Further, diatomaceous addition is 1～10g in step (1), and the addition of butyl titanate is 1～30ml,
The addition of ethanol is 50～150ml.
Yet further, the addition of water is 80～205ml in step (2), and after ethanol volatilizees completely, is added
Water.
Further, styrene addition is 1～8g in step (4), and styrene addition is less than diatomaceous
Addition.
In addition, the capacity of there-necked flask is 250ml in step (1), diatomite addition is 8g, and the addition of ethanol is
120ml, butyl titanate addition is 15ml.
Additionally, the addition of water is 150ml in step (2).
Further, styrene addition is 6g in step (4).
Yet further, when step (4) adds tetraethyl orthosilicate, in-situ polymerization is carried out as catalyst using ammoniacal liquor or hydrochloric acid
Method.
Further, the addition of catalyst is 2～5ml.
What deserves to be explained is, the present invention carries out the protection of polystyrene to composite, makes the nano-TiO of load2Obtain
Certain protection, it is to avoid with the various compound directly contacts in coating, and do not destroy diatomaceous microcellular structure as far as possible, in order to avoid
Affect the adsorption effect of its PARA FORMALDEHYDE PRILLS(91,95).
In order to preferably realize the present invention, specific parameter is as follows in building-up process：
Mixing speed is 500r/min in step (1), and mixing time is 40min；Vacuum drying temperature is 50 in step (3)
DEG C, vacuum drying time is 8h, and calcining heat is 450 DEG C, and calcination time is 5h.
Its principle：It is the compound of in-situ synthesis and sol-gel synthesis method to prepare polystyrene protection composite
Technique, can make the nano titanium oxide that reaction is generated in diatomite surface uniform load and protect nano-TiO2Spherical junctions
Structure, can be greatly improved nano-TiO2Photocatalysis efficiency.
The present invention has advantages below and beneficial effect：
The present invention carries out certain pretreatment to composite, makes the nano-TiO of load2Obtain certain protection, it is to avoid
With the various compound directly contacts in coating, and as far as possible diatomaceous microcellular structure is not destroyed, in order to avoid affect its PARA FORMALDEHYDE PRILLS(91,95)
Adsorption effect.For this purpose, composite is infiltrated in certain density polystyrene solution, after filtering drying so as to surface shape
Into the suitable polystyrene protective layer of thickness.Due to nano-TiO2Diatomaceous surface is carried on (including the table of its inner void
Face), nano level polystyrene protective layer had both protected catalysis material, and did not destroy the microcellular structure of composite, so as to
Reach the unification of function and performance.The method of this original creation solves how composite is protected with coating compounding from bottom-layer design
The problem of its performance is held, the key issue that formaldehyde absorbing is applied to coating products in decomposition multifunctional paint additive is solved,
Jing tests achieve good effect.
Specific embodiment
With reference to embodiment, the present invention is further illustrated, but embodiments of the present invention are not limited to this.
Embodiment 1
Diatomite/nano-TiO2The stabilization method of light catalyzed coating additive, with diatomite, butyl titanate and benzene second
Alkene is raw material, and using situ aggregation method synthetic polystyrene diatomite/nano-TiO is protected2Composite, comprises the following steps：
(1) 10g diatomite is added in 250ml there-necked flasks, 100ml ethanol, 10ml butyl titanates is slowly added to 25
30min is stirred with the speed of 450r/min under DEG C water bath with thermostatic control, diatomite and solution of tetrabutyl titanate is well mixed；
(2) 55 DEG C of speed stirring mixed solutions with 500r/min are warming up to volatilize completely to ethanol, water is added, are heated
Volatilize completely to moisture, obtain drying solid；
(3) it is drying solid washing is multiple, after being vacuum dried 12h at a temperature of 50 DEG C, it is put at a temperature of 450 DEG C and forges
5h is burnt, that is, obtains diatomite/nano-TiO2Composite；
(4) using 8g styrene as monomer, n-BuLi is initiator, and triethoxysilane is that activity ends agent is prepared poly-
Styrene, adds tetraethyl orthosilicate that the diatomite/nano-TiO of polystyrene protection is obtained by situ aggregation method2Composite, Jing
Overscanning electron-microscope scanning particle diameter is about 50～100nm.
Above-mentioned diatomite/nano-TiO2Composite, using UV-Vis DRS the optical property of catalyst is detected,
It can be found that diatomite/nano-TiO2Light absorbs of the composite wavelength less than 500nm, and diatomite/nano-TiO2Composite
For the light absorbs of 500nm-800nm, the utilization rate of natural light is substantially increased, such that it is able to improve the photocatalysis of composite
Efficiency.
Embodiment 2
Diatomite/nano-TiO2The stabilization method of light catalyzed coating additive, with diatomite, butyl titanate and benzene second
Alkene is raw material, and using situ aggregation method synthetic polystyrene diatomite/nano-TiO is protected2Composite, comprises the following steps：
(1) 6g diatomite is added in 250ml there-necked flasks, 80ml ethanol, 15ml butyl titanates is slowly added at 35 DEG C
35min is stirred with the speed of 550r/min under water bath with thermostatic control, diatomite and solution of tetrabutyl titanate is well mixed；
(2) 60 DEG C of speed stirring mixed solutions with 600r/min are warming up to volatilize completely to ethanol, water is added, are heated
Volatilize completely to moisture, obtain drying solid；
(3) it is drying solid washing is multiple, after being vacuum dried 8h at a temperature of 60 DEG C, it is put at a temperature of 500 DEG C and forges
4h is burnt, that is, obtains diatomite/nano-TiO2Composite；
(4) using 5g styrene as monomer, n-BuLi is initiator, and triethoxysilane is that activity ends agent is prepared poly-
Styrene, adds tetraethyl orthosilicate, with ammoniacal liquor as catalyst, by situ aggregation method the diatomite/receive of polystyrene protection is obtained
Rice TiO2Composite, it is about 50～100nm to be scanned through electron-microscope scanning particle diameter.
Embodiment 3
Diatomite/nano-TiO2The stabilization method of light catalyzed coating additive, with diatomite, butyl titanate and benzene second
Alkene is raw material, and using situ aggregation method synthetic polystyrene diatomite/nano-TiO is protected2Composite, comprises the following steps：
(1) 12g diatomite is added in 250ml there-necked flasks, 120ml ethanol, 25ml butyl titanates is slowly added to 40
36min is stirred with the speed of 500r/min under DEG C water bath with thermostatic control, diatomite and solution of tetrabutyl titanate is well mixed；
(2) 65 DEG C of speed stirring mixed solutions with 500r/min are warming up to volatilize completely to ethanol, water is added, are heated
Volatilize completely to moisture, obtain drying solid；
(3) it is drying solid washing is multiple, after being vacuum dried 9h at a temperature of 65 DEG C, it is put at a temperature of 550 DEG C and forges
3.8h is burnt, that is, obtains diatomite/nano-TiO2Composite；
(4) using 6g styrene as monomer, n-BuLi is initiator, and triethoxysilane is that activity ends agent is prepared poly-
Styrene, adds tetraethyl orthosilicate, with ammoniacal liquor as catalyst, by situ aggregation method the diatomite/receive of polystyrene protection is obtained
Rice TiO2Composite, it is about 50～100nm to be scanned through electron-microscope scanning particle diameter.
Above-mentioned diatomite/nano-TiO2Composite, using UV-Vis DRS the optical property of catalyst is detected,
It can be found that diatomite/nano-TiO2Light absorbs of the composite wavelength less than 500nm, and diatomite/nano-TiO2Composite
For the light absorbs of 500nm-800nm, the utilization rate of natural light is substantially increased, such that it is able to improve the photocatalysis of composite
Efficiency.
Embodiment 4
Diatomite/nano-TiO2The stabilization method of light catalyzed coating additive, with diatomite, butyl titanate and benzene second
Alkene is raw material, and using situ aggregation method synthetic polystyrene diatomite/nano-TiO is protected2Composite, comprises the following steps：
(1) 15g diatomite is added in 250ml there-necked flasks, 130ml ethanol, 25ml butyl titanates is slowly added to 30
40min is stirred with the speed of 450r/min under DEG C water bath with thermostatic control, diatomite and solution of tetrabutyl titanate is well mixed；
(2) 70 DEG C of speed stirring mixed solutions with 600r/min are warming up to volatilize completely to ethanol, water is added, are heated
Volatilize completely to moisture, obtain drying solid；
(3) it is drying solid washing is multiple, after being vacuum dried 8h at a temperature of 70 DEG C, it is put at a temperature of 600 DEG C and forges
4h is burnt, that is, obtains diatomite/nano-TiO2Composite；
(4) using 8g styrene as monomer, n-BuLi is initiator, and triethoxysilane is that activity ends agent is prepared poly-
Styrene, adds tetraethyl orthosilicate, with hydrochloric acid as catalyst, by situ aggregation method the diatomite/receive of polystyrene protection is obtained
Rice TiO2Composite, it is about 50～100nm to be scanned through electron-microscope scanning particle diameter.
Embodiment 5
Diatomite/nano-TiO2The stabilization method of light catalyzed coating additive, with diatomite, butyl titanate and benzene second
Alkene is raw material, and using situ aggregation method synthetic polystyrene diatomite/nano-TiO is protected2Composite, comprises the following steps：
(1) 15g diatomite is added in 250ml there-necked flasks, 130ml ethanol, 22ml butyl titanates is slowly added to 38
45min is stirred with the speed of 480r/min under DEG C water bath with thermostatic control, diatomite and solution of tetrabutyl titanate is well mixed；
(2) 80 DEG C of speed stirring mixed solutions with 600r/min are warming up to volatilize completely to ethanol, water is added, are heated
Volatilize completely to moisture, obtain drying solid；
(3) it is drying solid washing is multiple, after being vacuum dried 7h at a temperature of 75 DEG C, it is put at a temperature of 600 DEG C and forges
4.2h is burnt, that is, obtains diatomite/nano-TiO2Composite；
(4) using 10g styrene as monomer, n-BuLi is initiator, and triethoxysilane is obtained for activity ends agent
Polystyrene, add tetraethyl orthosilicate, with ammoniacal liquor as catalyst, by situ aggregation method obtain polystyrene protection diatomite/
Nano-TiO2Composite, it is about 50～100nm to be scanned through electron-microscope scanning particle diameter.
Above-mentioned diatomite/nano-TiO2Composite, using UV-Vis DRS the optical property of catalyst is detected,
It can be found that diatomite/nano-TiO2Light absorbs of the composite wavelength less than 500nm, and diatomite/nano-TiO2Composite
For the light absorbs of 500nm-800nm, the utilization rate of natural light is substantially increased, such that it is able to improve the photocatalysis of composite
Efficiency.
Embodiment 6
Diatomite/nano-TiO2The stabilization method of light catalyzed coating additive, with diatomite, butyl titanate and benzene second
Alkene is raw material, and using situ aggregation method synthetic polystyrene diatomite/nano-TiO is protected2Composite, comprises the following steps：
(1) 9g diatomite is added in 250ml there-necked flasks, 90ml ethanol, 20ml butyl titanates is slowly added at 38 DEG C
50min is stirred with the speed of 350r/min under water bath with thermostatic control, diatomite and solution of tetrabutyl titanate is well mixed；
(2) 90 DEG C of speed stirring mixed solutions with 600r/min are warming up to volatilize completely to ethanol, water is added, are heated
Volatilize completely to moisture, obtain drying solid；
(3) it is drying solid washing is multiple, after being vacuum dried 6h at a temperature of 80 DEG C, it is put at a temperature of 600 DEG C and forges
4h is burnt, that is, obtains diatomite/nano-TiO2Composite；
(4) using 6g styrene as monomer, n-BuLi is initiator, and triethoxysilane is that activity ends agent is prepared poly-
Styrene, adds tetraethyl orthosilicate, with hydrochloric acid as catalyst, by situ aggregation method the diatomite/receive of polystyrene protection is obtained
Rice TiO2Composite, it is about 50～100nm to be scanned through electron-microscope scanning particle diameter.
Test result：
20g composites obtained in embodiment 4 are weighed, in being scattered in 200ml water, is coated on 4 pieces of glass plates, adopted
With《JC/T1074-2008 function of purifying indoor air coating material purifying properties》On method to diatomite/nano-TiO2It is multiple
The performance of condensation material is measured.
Table 1
It can be seen from Table 1 that, diatomite/nano-TiO that the present invention is prepared2Composite has good except formaldehyde
Ability, is a kind of excellent coating additive.
It should be noted that above example is only to illustrative and not limiting technical scheme, although with reference to upper
State embodiment to be described in detail the present invention, it will be understood by those within the art that：Still can be to the present invention
Modify or equivalent, any modification or partial replacement without departing from the spirit and scope of the present invention, it all should contain
Cover in scope of the presently claimed invention.
Claims (10)
1. a kind of diatomite/nano-TiO2The stabilization method of light catalyzed coating additive, it is characterised in that with diatomite, metatitanic acid
Four butyl esters are raw material, and using situ aggregation method diatomite/nano-TiO is synthesized2Composite, comprises the following steps：
A, by diatomite, butyl titanate, ethanol mixing, stirring and dissolving obtains mixed liquor；
B, it is gradually heating to make ethanol volatilize completely, adds water, then proceeding to heating makes moisture evaporation, obtains drying solid；
C, drying solid is washed for several times, heating, drying obtains dry ingredient, and the calcining of this dry ingredient is obtained into powder, as diatom
Soil/nano-TiO2Composite；
D, by diatomite/nano-TiO2Composite is infiltrated in polystyrene solution, after filtering drying so as to which surface forms poly-
Styrene protective layer, obtains final product product；Wherein, the particle diameter of products obtained therefrom is 50～100nm.
2. diatomite/nano-TiO according to claim 12The stabilization method of light catalyzed coating additive, its feature exists
In specifically including following steps：
(1) diatomite is added in there-necked flask, is slowly added to ethanol, butyl titanate in water bath with thermostatic control with 300～600r/
The speed of min stirs 5～60min, obtains uniform mixed solution；
(2) being warming up to 50～90 DEG C of speed stirring mixed solutions with 300～600r/min makes ethanol volatilize, and adds water, so
After be heated to moisture evaporation, obtain drying solid；
(3) drying solid is washed for several times, is vacuum dried 6～16 hours at a temperature of 35～65 DEG C, finally 300～600
Calcine 3～8 hours at a temperature of DEG C, that is, obtain diatomite/nano-TiO2Composite；
(4) using styrene as monomer, n-BuLi is initiator, and triethoxysilane is that activity ends agent is obtained polyphenyl second
Alkene, adds tetraethyl orthosilicate that the diatomite/nano-TiO of polystyrene protection is obtained by situ aggregation method2Composite.
3. diatomite/nano-TiO according to claim 22The stabilization method of light catalyzed coating additive, its feature exists
In diatomaceous addition is 5～20g in step (1), and the addition of butyl titanate is 5～25ml, and the addition of ethanol is
50～150ml.
4. diatomite/nano-TiO according to claim 32The stabilization method of light catalyzed coating additive, its feature exists
In the addition of water is 80～205ml in step (2), and after ethanol volatilizees completely, adds water.
5. diatomite/nano-TiO according to claim 42The stabilization method of light catalyzed coating additive, its feature exists
In styrene addition is 1～8g in step (4), and styrene addition is less than diatomaceous addition.
6. diatomite/nano-TiO according to claim 32The stabilization method of light catalyzed coating additive, its feature exists
In the capacity of there-necked flask is 250ml in step (1), and diatomite addition is 8g, and the addition of ethanol is 120ml, the fourth of metatitanic acid four
Ester addition is 15ml.
7. diatomite/nano-TiO according to claim 42The stabilization method of light catalyzed coating additive, its feature exists
In the addition of water is 150ml in step (2).
8. diatomite/nano-TiO according to claim 62The stabilization method of light catalyzed coating additive, its feature exists
In styrene addition is 6g in step (4).
9. diatomite/nano-TiO according to claim 22The stabilization method of light catalyzed coating additive, its feature exists
When, step (4) adds tetraethyl orthosilicate, situ aggregation method is carried out as catalyst using ammoniacal liquor or hydrochloric acid.
10. diatomite/nano-TiO according to claim 92The stabilization method of light catalyzed coating additive, its feature exists
In the addition of catalyst is 2～5ml.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107433185A (en) * | 2017-09-05 | 2017-12-05 | 霍邱金木鱼农业科技有限公司 | A kind of material for air purification and preparation method thereof |
| CN107537451A (en) * | 2017-09-05 | 2018-01-05 | 霍邱金木鱼农业科技有限公司 | A kind of porous zeolite material for air purification and preparation method thereof |
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| CN107629501A (en) * | 2017-10-13 | 2018-01-26 | 陶红雨 | A kind of preparation method of environmental friendly indoor construction material |
| CN108424082A (en) * | 2018-04-19 | 2018-08-21 | 俞小峰 | A kind of preparation method of pleat-free cement-base waterproof coating |
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Application publication date: 20170510 |