CN106799258B - A kind of method that chemical modification method prepares nanoscale Asia titanium oxide composite photo-catalyst - Google Patents
A kind of method that chemical modification method prepares nanoscale Asia titanium oxide composite photo-catalyst Download PDFInfo
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- CN106799258B CN106799258B CN201710029490.1A CN201710029490A CN106799258B CN 106799258 B CN106799258 B CN 106799258B CN 201710029490 A CN201710029490 A CN 201710029490A CN 106799258 B CN106799258 B CN 106799258B
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- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 238000000034 method Methods 0.000 title claims abstract description 59
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 239000002131 composite material Substances 0.000 title claims abstract description 29
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 26
- 238000007385 chemical modification Methods 0.000 title claims abstract description 25
- 239000000843 powder Substances 0.000 claims abstract description 36
- 238000000889 atomisation Methods 0.000 claims abstract description 23
- 239000003795 chemical substances by application Substances 0.000 claims description 28
- 239000007789 gas Substances 0.000 claims description 23
- 230000004048 modification Effects 0.000 claims description 11
- 238000012986 modification Methods 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 11
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 4
- 150000001413 amino acids Chemical class 0.000 claims description 4
- 229910052698 phosphorus Inorganic materials 0.000 claims description 4
- 239000011574 phosphorus Substances 0.000 claims description 4
- 238000002604 ultrasonography Methods 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 3
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 239000007822 coupling agent Substances 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 10
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000000053 physical method Methods 0.000 abstract description 4
- 239000011347 resin Substances 0.000 abstract description 4
- 229920005989 resin Polymers 0.000 abstract description 4
- 229920001002 functional polymer Polymers 0.000 abstract description 3
- 239000011858 nanopowder Substances 0.000 description 21
- 239000000243 solution Substances 0.000 description 14
- 239000000463 material Substances 0.000 description 9
- 230000000694 effects Effects 0.000 description 7
- 238000005303 weighing Methods 0.000 description 7
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 6
- 239000003607 modifier Substances 0.000 description 6
- 239000007921 spray Substances 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 239000002096 quantum dot Substances 0.000 description 5
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 4
- 230000004913 activation Effects 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 235000011187 glycerol Nutrition 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 2
- CWERGRDVMFNCDR-UHFFFAOYSA-N thioglycolic acid Chemical compound OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 238000005267 amalgamation Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000002500 effect on skin Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 238000013386 optimize process Methods 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000004054 semiconductor nanocrystal Substances 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/04—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing carboxylic acids or their salts
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/0201—Oxygen-containing compounds
- B01J31/0202—Alcohols or phenols
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Catalysts (AREA)
Abstract
The present invention provides a kind of methods that chemical modification method prepares nanoscale Asia titanium oxide composite photo-catalyst, including, mechanical smashing, and ultrasonic high speed atomisation are carried out to sub- titanium oxide and/or miscellaneous element doping Asia titanium oxide；Air-flow smashing is carried out, Asia nano titanium oxide powder is made；It is surface modified.The method that chemical modification method provided by the present invention prepares nanoscale Asia titanium oxide composite photo-catalyst, simple, the large scale preparation nano-quantum point by physical method, and it is surface modified to increase its stability and resin system compatibility, inhibit it in the reunion behavior of the systems such as resin, high production efficiency, can large-scale application in industrialized production, lay a good foundation for the preparation of functional polymer and composite material.
Description
Technical field
The invention belongs to the preparation technical fields of function nano particle, and in particular to a kind of chemical modification method prepares nanoscale
The method of sub- titanium oxide composite photo-catalyst.
Background technique
Scale involved in this technology belongs to quantum point range, and quantum dot is also known as semiconductor nanocrystals, three of them dimension
Size all at 200 nanometers hereinafter, appearance is just like a very small pointing object, movement of the internal electron in all directions all by
To limitation.The special construction of quantum dot causes it to meet effect and macroscopic quantum with skin effect, quantum size effect, dielectric resistance
Tunnel-effect etc. has biggish application to show the physicochemical properties different from macroscopic material in terms of functional material
Potentiality.
By years of researches, establish the preparation method of a variety of quantum dots so far, and chemically based on, comprising:
It is synthesized in organic system using the method for colloid chemistry；It directly synthesizes in aqueous solution.But prepared by such method
Quantum dot yield is small, and kind is restricted, and quantum dot then rare report is prepared by physical method.In addition, both at home and abroad
For nano-function powder prepare, mostly use chemical technology, have the shortcomings that it is at high cost, complicated for operation, be unfavorable for industrialize answer
With.
Summary of the invention
The purpose of this section is to summarize some aspects of the embodiment of the present invention and briefly introduce some preferable implementations
Example.It may do a little simplified or be omitted to avoid our department is made in this section and the description of the application and the title of the invention
Point, the purpose of abstract of description and denomination of invention it is fuzzy, and this simplification or omit and cannot be used for limiting the scope of the invention.
In view of the technological gap of above-mentioned sub- titanium oxide composite photo-catalyst preparation, the present invention is proposed.
Therefore, the one of purpose of the present invention is to solve deficiency in the prior art, provides a kind of chemical modification legal system
The method of standby nanoscale Asia titanium oxide composite photo-catalyst.
In order to solve the above technical problems, the present invention provides the following technical scheme that a kind of chemical modification method prepares nanoscale
The method of sub- titanium oxide composite photo-catalyst, including, mechanical powder is carried out to sub- titanium oxide and/or miscellaneous element doping Asia titanium oxide
Essence, and ultrasonic high speed atomisation；Air-flow smashing is carried out, Asia nano titanium oxide powder is made；It is surface modified.
The one kind for preparing the method for nanoscale Asia titanium oxide composite photo-catalyst as chemical modification method of the present invention is excellent
Select scheme, in which: the Asia titanium oxide and/or miscellaneous element doping Asia titanium oxide, particle size range are 500~20000nm.
The one kind for preparing the method for nanoscale Asia titanium oxide composite photo-catalyst as chemical modification method of the present invention is excellent
Select scheme, in which: the miscellaneous element is one or more of nitrogen, phosphorus or sulphur.
The one kind for preparing the method for nanoscale Asia titanium oxide composite photo-catalyst as chemical modification method of the present invention is excellent
Select scheme, in which: the partial size of the Asia nano titanium oxide powder is 10~200nm.
The one kind for preparing the method for nanoscale Asia titanium oxide composite photo-catalyst as chemical modification method of the present invention is excellent
Select scheme, in which: it is described ultrasound high speed atomisation, wherein ultrasonic power be 200~250W, high speed atomisation revolving speed be 20000~
24000rpm。
The one kind for preparing the method for nanoscale Asia titanium oxide composite photo-catalyst as chemical modification method of the present invention is excellent
Select scheme, in which: the air-flow crushing, gas flow are 2~4m3/ min, gas pressure are 0.5~0.7MPa, gas temperature
Degree is 90~120 DEG C.
The one kind for preparing the method for nanoscale Asia titanium oxide composite photo-catalyst as chemical modification method of the present invention is excellent
Select scheme, in which: the mechanical smashing, smashing time are 0.5~1h, and revolving speed is 250~350rpm.
The one kind for preparing the method for nanoscale Asia titanium oxide composite photo-catalyst as chemical modification method of the present invention is excellent
Select scheme, in which: the surface modification, the dosage of dressing agent are the 1~10% of powder quality, mass concentration is 4~
6wt.%.
The one kind for preparing the method for nanoscale Asia titanium oxide composite photo-catalyst as chemical modification method of the present invention is excellent
Select scheme, in which: the dressing agent, atomization droplets diameter are 1~20 μm.
The one kind for preparing the method for nanoscale Asia titanium oxide composite photo-catalyst as chemical modification method of the present invention is excellent
Select scheme, in which: the dressing agent includes one of silane coupling agent, titanate coupling agent or amino acids dressing agent or several
Kind.
Possessed by of the invention the utility model has the advantages that
(1) method that chemical modification method provided by the present invention prepares nanoscale Asia titanium oxide composite photo-catalyst, passes through
Physical method is simple, large scale preparation nano-quantum point, and is surface modified to it to increase its stability and resin system
Compatibility, high production efficiency, can large-scale application in industrialized production, established for the preparation of functional polymer and composite material
Basis.
(2) method that chemical modification method provided by the present invention prepares nanoscale Asia titanium oxide composite photo-catalyst uses
A small amount of coating material can be prepared by the superior nano-powder of performance.
(3) chemical modification method provided by the present invention is prepared prepared by the method for nanoscale Asia titanium oxide composite photo-catalyst
Obtained nano-powder, partial size is small and has excellent surface active index and dispersibility in the base.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, required use in being described below to embodiment
Attached drawing be briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for this
For the those of ordinary skill of field, without any creative labor, it can also be obtained according to these attached drawings other
Attached drawing.Wherein:
Fig. 1 is the sub- titanium oxide powder that 1 gained diameter of embodiment is 100 rans；
Fig. 2 is the sub- titanium oxide powder that 3 gained diameter of embodiment is 50 rans.
Specific embodiment
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, right combined with specific embodiments below
A specific embodiment of the invention is described in detail.
In the following description, numerous specific details are set forth in order to facilitate a full understanding of the present invention, but the present invention can be with
Implemented using other than the one described here other way, those skilled in the art can be without prejudice to intension of the present invention
In the case of do similar popularization, therefore the present invention is not limited by the specific embodiments disclosed below.
Secondly, " one embodiment " or " embodiment " referred to herein, which refers to, may be included at least one realization side of the invention
A particular feature, structure, or characteristic in formula." in one embodiment " that different places occur in the present specification not refers both to
The same embodiment, nor the individual or selective embodiment mutually exclusive with other embodiments.
Embodiment 1
The Asia 3t titanium oxide (partial size is 10000~20000nm) is weighed, is added in the mechanical crusher of 350rpm revolving speed,
It crushes 45 minutes, and uses ultrasonic high speed atomisation assisted comminution, ultrasonic power 250W simultaneously, high speed atomisation revolving speed is
24000rpm, powder gathers weighing after smashing；Coating material Thioglycolic acid 0.15t is weighed in 5wt.% ratio, adjusts gas
Flow disintegrating machine, gas flow 3m3/ min, gas pressure 0.6MPa, air themperature are 100 DEG C, and dressing agent solution concentration is
5wt.%, the flow for modifying agent solution is 1ml/min, and being atomized is 1~20 μm, starts to spray into dressing agent after crushing, crushes and complete
After to obtain average diameter be 100 nanometers, surface modification, finely dispersed Asia nano titanium oxide powder.
This is sample 1.
Embodiment 2
The Asia 3t titanium oxide (partial size is 5000~10000nm) is weighed, is added in the mechanical crusher of 300rpm revolving speed, powder
Broken 60 minutes, and ultrasonic high speed atomisation assisted comminution, ultrasonic power 200W are used simultaneously, high speed atomisation revolving speed is
22000rpm, powder gathers weighing after smashing；Amino acids coating material 0.24t is weighed in 8wt.% ratio, adjusts gas
Flow disintegrating machine, gas flow 3m3/ min, gas pressure 0.6MPa, air themperature are 110 DEG C, and dressing agent solution concentration is
6wt.%, the flow for modifying agent solution is 1ml/min, and being atomized is 1~20 μm, starts to spray into dressing agent after crushing, crushes and complete
After to obtain average diameter be 100 nanometers, surface modification, finely dispersed Asia titanium oxide powder.
This is sample 2.
Embodiment 3
The Asia 3t titanium oxide (partial size is 500~5000nm) is weighed, is added in the mechanical crusher of 250rpm revolving speed, crushes
45 minutes, and simultaneously using ultrasonic high speed atomisation assisted comminution, ultrasonic power 250W, high speed atomisation revolving speed is 20000rpm,
Powder gathers weighing after smashing；Glycerine 0.18t is weighed in 6wt.% ratio, adjusts air-flow disintegrating machine, gas flow is
3m3/ min, gas pressure 0.6MPa, air themperature are 100 DEG C, and dressing agent solution concentration is 4wt.%, modifies agent solution
Flow is 1ml/min, and being atomized is 1~20 μm, starts to spray into dressing agent after crushing, and average diameter is obtained after the completion of crushing and is received for 50
Rice, surface modification, finely dispersed Asia titanium oxide powder.
This is sample 3.
Embodiment 4
The Asia 3t titanium oxide (partial size is 500~5000nm) is weighed, is added in the mechanical crusher of 300rpm revolving speed, crushes
30 minutes, and simultaneously using ultrasonic high speed atomisation assisted comminution, ultrasonic power 200W, high speed atomisation revolving speed is 24000rpm,
Powder gathers weighing after smashing；Glycerine 0.33t is weighed in 10wt.% ratio, adjusts air-flow disintegrating machine, gas flow is
2m3/ min, gas pressure 0.7MPa, air themperature are 120 DEG C, and dressing agent solution concentration is 5wt.%, modifies agent solution
Flow is 1.2ml/min, and being atomized is 1~20 μm, starts to spray into dressing agent after crushing, and it is 80 that average diameter is obtained after the completion of crushing
Nanometer, surface modification, finely dispersed Asia titanium oxide powder.
This is sample 4.
Embodiment 5
3t N doping Asia titanium oxide (partial size is 500~5000nm) is weighed, the mechanical crusher of 300rpm revolving speed is added to
In, it crushes 30 minutes, and use ultrasonic high speed atomisation assisted comminution, ultrasonic power 200W simultaneously, high speed atomisation revolving speed is
24000rpm, powder gathers weighing after smashing；Glycerine 0.33t is weighed in 10wt.% ratio, adjusts air-flow disintegrating machine, gas
Body flow is 2m3/ min, gas pressure 0.7MPa, air themperature are 120 DEG C, and dressing agent solution concentration is 5wt.%, modification
The flow of agent solution is 1.2ml/min, and being atomized is 1~20 μm, starts to spray into dressing agent after crushing, is averaged after the completion of crushing
Diameter is 80 nanometers, surface modification, finely dispersed N doping Asia titanium oxide powder.
Embodiment 6
3t phosphorus doping Asia titanium oxide (partial size is 5000~10000nm) is weighed, the mechanical crushing of 300rpm revolving speed is added to
It in machine, crushes 60 minutes, and uses ultrasonic high speed atomisation assisted comminution, ultrasonic power 200W simultaneously, high speed atomisation revolving speed is
22000rpm, powder gathers weighing after smashing；Amino acids coating material 0.24t is weighed in 8wt.% ratio, adjusts gas
Flow disintegrating machine, gas flow 3m3/ min, gas pressure 0.6MPa, air themperature are 110 DEG C, and dressing agent solution concentration is
6wt.%, the flow for modifying agent solution is 1ml/min, and being atomized is 1~20 μm, starts to spray into dressing agent after crushing, crushes and complete
After to obtain average diameter be 100 nanometers, surface modification, finely dispersed phosphorus doping Asia titanium oxide.
Embodiment 7:
Take commercially available nano level modified sub- titanium oxide powder, amount of modifier 15wt%, as sample 5.
200ml deionized water is added in each 5.0g of separately sampled product 1,2,3,4,5, and magnetic agitation 5min is stood, and removes drift
The powder bubbled through the water column, by the sample filtering to sink under water, drying, weighing, quality is denoted as M, calculates and activates according to following formula
Index:
Concrete outcome such as following table
As result as it can be seen that modified powder prepared by the present invention has excellent effect in terms of activation index.Inventor
It has been investigated that the activation index of modified powder can be remarkably reinforced, and stablize when control amount of modifier is in 1~10wt%
90% or more.Although in commercially available modified powder, amount of modifier serious offense 10wt%, since it is in modifying process, out
It is soft-agglomerated between existing original nano-powder and modified nano powder, so that forming " aggregate particle size ", it can not effectively optimize activation and refer to
Number.The present invention destroys the reunion between nano-powder in mechanical smash, while with ultrasound or high speed atomisation, avoids and directly adds
The soft-agglomerated phenomenon for entering modifying agent and generating, and carry out modifying simultaneously that when being mechanically pulverized, machine can be corroded, lead to mechanical disorder.
Embodiment 8:
Take commercially available nano level modified titanium dioxide powder, amount of modifier 15wt%, as sample 5.
Separately sampled product 1,2,3,4,5 are added carbon tetrachloride, are made into the dispersion liquid of 0.1wt%, ultrasonic disperse 10min is set
It in the graduated test tube with grinding port plug of 10ml, stands at room temperature, records the solvent of supernatant liquor, the body with organic phase
Product (10ml) ratio indicates the sedimentation rate of nano-powder to evaluate its dispersibility.
Timing 180 minutes, every 30 minutes record sedimentation rate data, the following chart of arrangement:
As result as it can be seen that modified powder prepared by the present invention has excellent effect in terms of dispersibility.Nano-powder
Same basis material whether can be embodied and stablize uniformly dispersed in amalgamation and basis material, key is to control nano powder
Body uniform particle sizes and nano-powder are sufficiently modified.Inventor passes through mechanical crushing, unification the study found that by nano-powder particle
Control in 200nm hereinafter, and this during using ultrasound, high speed atomisation rather than add modifier modification, it is more enough to avoid modifying process
Middle modified Nano particle is soft-agglomerated with former nanoparticle, so that particle diameter distribution is relatively narrow, it is not in that " aggregate particle size " is existing
As；It is further smashed using air-flow, and does surface modification with modifying agent simultaneously, then in the uniform situation of particle diameter distribution, into
Step refining partial size, and simultaneously, it is modified compared to mechanical smashing method, sufficiently nanoparticle is changed near " one-to-one "
Property.To sum up, method provided by the present invention, can control particle diameter of nanometer powder uniformly and nano-powder is sufficiently modified, embody
Excellent dispersibility in the base.
Embodiment 9:
Sample 1,2,3,4 is mixed with corresponding matrix, is made finished product 1~4, carry out electric conductivity, ultraviolet radiation absorption,
The aptitude tests of this four aspect of photothermal conversion, light degradation formaldehyde.As a result such as following table.
As result as it can be seen that modified powder prepared by the present invention, drops in ultraviolet radiation absorption, conductive capability, photothermal conversion, light
In terms of solving formaldehyde function, there is excellent effect.Function nano powder, if excellent functional effect can be embodied, key is
1. whether nano-powder particle itself is sufficiently modified；2. nano-powder whether in the base stable fusion；3. whether nano-powder
It is uniformly dispersed in the base.This three, complements each other.Inventor by first wheel to nano-powder the study found that crushed and same
Shi Chaosheng or high velocity fog processing, can prevent the soft-agglomerated phenomenon of nano-powder, so that it will not be because of " secondary grain
Diameter " and occur that particle diameter distribution is wide, modified insufficient situation occurs.In this way, in the partial size of effectively control nano-powder
In the case where distribution and modified abundant degree, the preparation-obtained nano-powder of the present invention is allowed for, it being capable of work with higher
Change index and dispersibility excellent in the base.In turn, even if compared with the higher common commercially available function powder of modifier content,
Fabric prepared by powder produced by the present invention can embody more excellent functional effect.
It is noted that being in the prior art that nanoscale Asia titanium oxide powder is made in chemical method, the present invention uses object
The powder of better effect has been made in reason method.It has abandoned in traditional preparation process, the method for now modifying post-processing, using ultrasonic mist
Change aid in treatment, and preferably optimize process conditions, promotes sub- titania surface atom and stretch to " dangling bonds " in space to sky
The absorption of gas, with the progress of crushing and the facilitation of ultrasonic atomizatio, the three-dimensional periodic potential field inside sub- titanium oxide is continuous
On surface by very fast interruption, electronic state and the mutually dramatic variation of body, lead to its in addition to adsorption site is stablized in bridging oxygen vacancy etc.
A degree of dissociation occurs for the gas that he adsorbs, affect in sub- titanium oxide system there is hybrid ionic and covalent bond make
With the lower order of magnitude can be crushed to so that sub- titanium oxide stability dies down.
In conclusion chemical modification method provided by the present invention prepares the side of nanoscale Asia titanium oxide composite photo-catalyst
Method, simple, the large scale preparation nano-quantum point by physical method, and it is surface modified to increase its stability and tree
Resin system compatibility, high production efficiency, can large-scale application in industrialized production, be the preparation of functional polymer and composite material
It lays a good foundation；The method that chemical modification method provided by the present invention prepares nanoscale Asia titanium oxide composite photo-catalyst uses
A small amount of coating material can be prepared by the superior nano-powder of performance；Chemical modification method provided by the present invention prepares nanoscale
The preparation-obtained nano-powder of method of sub- titanium oxide composite photo-catalyst, partial size is small and has excellent surface in the base
Activation index and dispersibility.
It should be noted that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting, although referring to preferable
Embodiment describes the invention in detail, those skilled in the art should understand that, it can be to technology of the invention
Scheme is modified or replaced equivalently, and without departing from the spirit and scope of the technical solution of the present invention, should all be covered in this hair
In bright scope of the claims.
Claims (3)
1. a kind of method that chemical modification method prepares nanoscale Asia titanium oxide composite photo-catalyst, it is characterised in that: including,
Mechanical smashing, and ultrasonic high speed atomisation are carried out to sub- titanium oxide or miscellaneous element doping Asia titanium oxide:
Air-flow smashing is carried out, Asia titanium oxide or miscellaneous element doping Asia nano titanium oxide powder is made:
It is surface modified；Wherein,
The miscellaneous element is nitrogen or phosphorus；
The ultrasound high speed atomisation, wherein ultrasonic power is 200~250W, and high speed atomisation revolving speed is 20000~24000rpm；
The air-flow crushing, gas flow are 2~4m3/ min, gas pressure be 0.5~0.7MPa, gas temperature be 90~
120℃；
The mechanical smashing, smashing time are 0.5~lh, and revolving speed is 250~350rpm；
The surface modification, the dosage of dressing agent are the 1~10% of powder quality, and mass concentration is 4~6wt.%；
The dressing agent, atomization droplets diameter are 1~20 μm；
The dressing agent includes one or more of silane coupling agent, titanate coupling agent or amino acids dressing agent.
2. the method that chemical modification method prepares nanoscale Asia titanium oxide composite photo-catalyst according to claim 1, feature
Be: the Asia titanium oxide or miscellaneous element doping Asia titanium oxide, particle size range are 500~20000nm.
3. the method that chemical modification method prepares nanoscale Asia titanium oxide composite photo-catalyst according to claim 1, feature
Be: the partial size of the Asia nano titanium oxide powder is 10~200nm.
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| CN102496704A (en) * | 2011-12-08 | 2012-06-13 | 中信国安盟固利电源技术有限公司 | Lithium titanate/titanium black anode material and preparation method thereof |
| CN103991904A (en) * | 2014-06-10 | 2014-08-20 | 中山大学 | Magneli phase titanium oxide nanowire array and preparation method thereof |
| CN106242585A (en) * | 2016-09-29 | 2016-12-21 | 四川大学 | A kind of sub-titanium oxide spherical powder and preparation method thereof |
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| CN102496704A (en) * | 2011-12-08 | 2012-06-13 | 中信国安盟固利电源技术有限公司 | Lithium titanate/titanium black anode material and preparation method thereof |
| CN103991904A (en) * | 2014-06-10 | 2014-08-20 | 中山大学 | Magneli phase titanium oxide nanowire array and preparation method thereof |
| CN106242585A (en) * | 2016-09-29 | 2016-12-21 | 四川大学 | A kind of sub-titanium oxide spherical powder and preparation method thereof |
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