CN106672910B - A kind of strong function nano powder preparation method for absorbing ultraviolet light - Google Patents
A kind of strong function nano powder preparation method for absorbing ultraviolet light Download PDFInfo
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- CN106672910B CN106672910B CN201710009436.0A CN201710009436A CN106672910B CN 106672910 B CN106672910 B CN 106672910B CN 201710009436 A CN201710009436 A CN 201710009436A CN 106672910 B CN106672910 B CN 106672910B
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- 239000011858 nanopowder Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- 238000000889 atomisation Methods 0.000 claims abstract description 18
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 17
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 17
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 14
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 8
- CXKCTMHTOKXKQT-UHFFFAOYSA-N cadmium oxide Inorganic materials [Cd]=O CXKCTMHTOKXKQT-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000011787 zinc oxide Substances 0.000 claims abstract description 6
- CFEAAQFZALKQPA-UHFFFAOYSA-N cadmium(2+);oxygen(2-) Chemical compound [O-2].[Cd+2] CFEAAQFZALKQPA-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 claims description 46
- 239000003795 chemical substances by application Substances 0.000 claims description 24
- 230000004048 modification Effects 0.000 claims description 13
- 238000012986 modification Methods 0.000 claims description 13
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 8
- CWERGRDVMFNCDR-UHFFFAOYSA-N thioglycolic acid Chemical compound OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 claims description 6
- 238000002604 ultrasonography Methods 0.000 claims description 6
- 235000011187 glycerol Nutrition 0.000 claims description 4
- 150000001413 amino acids Chemical class 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 12
- 230000008901 benefit Effects 0.000 abstract description 5
- 239000002537 cosmetic Substances 0.000 abstract description 4
- 239000004033 plastic Substances 0.000 abstract description 3
- 229920003023 plastic Polymers 0.000 abstract description 3
- 238000009941 weaving Methods 0.000 abstract description 3
- 239000002245 particle Substances 0.000 description 13
- 239000007789 gas Substances 0.000 description 12
- 239000000463 material Substances 0.000 description 11
- 230000000694 effects Effects 0.000 description 10
- 238000010521 absorption reaction Methods 0.000 description 7
- 238000009826 distribution Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000003607 modifier Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 230000004913 activation Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000004594 Masterbatch (MB) Substances 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000004062 sedimentation Methods 0.000 description 3
- 238000009987 spinning Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 235000013339 cereals Nutrition 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical class [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- HGWOWDFNMKCVLG-UHFFFAOYSA-N [O--].[O--].[Ti+4].[Ti+4] Chemical compound [O--].[O--].[Ti+4].[Ti+4] HGWOWDFNMKCVLG-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 238000005267 amalgamation Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005285 chemical preparation method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007812 deficiency Effects 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
- 238000002474 experimental method Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002074 melt spinning Methods 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/14—Methods for preparing oxides or hydroxides in general
- C01B13/145—After-treatment of oxides or hydroxides, e.g. pulverising, drying, decreasing the acidity
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G11/00—Compounds of cadmium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
- C01G19/02—Oxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The present invention provides a kind of strong function nano powder preparing methods for absorbing ultraviolet light, including, mechanical smashing, and ultrasonic high speed atomisation are carried out to metal oxide；Air-flow smashing is carried out, is surface modified, finally obtains product.The strong function nano powder preparation method for absorbing ultraviolet light provided by the present invention, used zinc oxide, cadmium oxide, titanium dioxide, stannic oxide, all have the function of good shielding ultraviolet rays, also have simultaneously non-stimulated to skin, it does not decompose, it never degenerates, the good advantage of thermal stability can be widely applied to the industries such as cosmetics, plastics, weaving.
Description
Technical field
The invention belongs to function nano Preparation Technique of Powders fields, and in particular to a kind of strong function nano for absorbing ultraviolet light
Powder preparation method.
Background technique
Ultraviolet light according to wavelength can be divided into shortwave (UVC, 200-280nm), medium wave (UVB, 280-320nm), long wave (UVA,
320-400nm).Ultraviolet (UV) C is relatively unabsorbed by ozone, and harm of the ultraviolet light to the mankind is generally drawn by the comprehensive function of UVA and UVB
It rises.
Nanosize metal oxide powder less than 200nm, has the function of good shielding ultraviolet rays.The amount of nano-powder
Sub- dimensional effect makes it have with " blue-shifted phenomenon " and to the absorption of various wavelength that " widthization shows to the light absorption of certain wavelength
As ", thus the absorption of ultraviolet light is significantly increased.Therefore nano material is used as and absorbs ultraviolet light functional material, for changing in living
Cosmetic, daily necessities etc. have the huge market demand.
However, nano particle diameter is small, specific surface is big, easily reunites, surface polarity is big, with most of polymer compatibility
Difference is difficult to obtain evenly dispersed on nanoscale using general blending technology；Mixing changes existing interface
Property technology is difficult to completely eliminate the interfacial tension between filler and polymeric matrix, it is difficult to realize ideal interfacial bonding, be not achieved
The nano-filled purpose of particle.
In addition, both at home and abroad for metal oxide nano function powder prepare, mostly use chemical technology, have it is at high cost,
The disadvantages of complicated for operation, is unfavorable for industrial applications.
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 metal oxide nano function powder preparation, the present invention is proposed.
Therefore, the one of purpose of the present invention is to solve deficiency in the prior art, and it is small and can to provide a kind of partial size
The strong function nano powder preparation method for absorbing ultraviolet light.
In order to solve the above technical problems, the present invention provides the following technical scheme that a kind of strong function of absorbing ultraviolet light is received
Rice flour preparation, including, mechanical smashing, and ultrasonic high speed atomisation are carried out to metal oxide；Air-flow smashing is carried out, is carried out
Surface modification finally obtains product.
A kind of preferred embodiment as the strong function nano powder preparation method for absorbing ultraviolet light of the present invention, in which:
The ultrasound high speed atomisation, wherein ultrasonic power is 200~250W, and high speed atomisation revolving speed is 20000~24000rpm.
A kind of preferred embodiment as the strong function nano powder preparation method for absorbing ultraviolet light of the present invention, in which:
The air-flow crushing, gas flow are 2~4m3/ min, gas pressure are 0.5~0.7MPa, and gas temperature is 90~120
℃。
A kind of preferred embodiment as the strong function nano powder preparation method for absorbing ultraviolet light of the present invention, in which:
The mechanical smashing, smashing time are 0.5~1h, and revolving speed is 250~350rpm.
A kind of preferred embodiment as the strong function nano powder preparation method for absorbing ultraviolet light of the present invention, in which:
The metal oxide includes zinc oxide, cadmium oxide, titanium dioxide, one or more of in stannic oxide.
A kind of preferred embodiment as the strong function nano powder preparation method for absorbing ultraviolet light of the present invention, in which:
The surface modification, wherein the flow of dressing agent is 0.8~1.2ml/min.
A kind of preferred embodiment as the strong function nano powder preparation method for absorbing ultraviolet light of the present invention, in which:
The dressing agent is 1~20 μm of drop, and mass concentration is 4~6wt.%.
A kind of preferred embodiment as the strong function nano powder preparation method for absorbing ultraviolet light of the present invention, in which:
The dressing agent includes the table of silane coupling agent series, titanate esters series or the small molecular organic compounds with 2~3 functional groups
Face is grafted one or more of chemical reagent.
A kind of preferred embodiment as the strong function nano powder preparation method for absorbing ultraviolet light of the present invention, in which:
The dressing agent includes Thioglycolic acid, amino acids, one or more of in glycerine.
A kind of preferred embodiment as the strong function nano powder preparation method for absorbing ultraviolet light of the present invention, in which:
The dosage of the dressing agent is the 1~10% of powder quality.
Possessed by of the invention the utility model has the advantages that
(1) the strong function nano powder preparation method for absorbing ultraviolet light provided by the present invention, using a small amount of surface modification
Agent can be prepared by the superior nano-powder of performance.
(2) the strong preparation-obtained nano powder of function nano powder preparation method for absorbing ultraviolet light provided by the present invention
Body, partial size is small and has excellent surface active index and dispersibility in the base.
(3) the strong function nano powder preparation method for absorbing ultraviolet light provided by the present invention, used zinc oxide, oxygen
Cadmium, titanium dioxide, stannic oxide, all have the function of good shielding ultraviolet rays, at the same also have it is non-stimulated to skin, regardless of
Solution, never degenerates, the good advantage of thermal stability can be widely applied to the industries such as cosmetics, plastics, weaving.
(4) function nano powder prepared by the strong function nano powder preparation method for absorbing ultraviolet light provided by the present invention
Body, by after surface modification, may make powder evenly dispersed in matrix, so functional material is further prepared, energy
Enough give full play to the strong effect for absorbing ultraviolet light.
(5) the strong function nano powder preparation method for absorbing ultraviolet light provided by the present invention, with traditional chemical preparation
Method is compared, cost reduce, easy to operate, the granularity of nano-powder is controllable, high production efficiency, can large-scale application in industrialization
Production.
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 1 gained zinc oxide nano-powder of embodiment, as seen from the figure, the method oxidation obtained through the invention
Zinc nano-powder, average grain diameter 100nm；
Fig. 2 is 2 gained nano TiO 2 powder of embodiment, as seen from the figure, through the invention two made from the method
Nano titanium oxide powder, average grain diameter 100nm；
Fig. 3 is powder sedimentation rate test experiments result figure in embodiment 6.
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.
It is of the present invention have it is strong absorb ultraviolet light function nano powder preparation method, by being combined to smashing mode, powder
Pure time, corresponding revolving speed, the advantageous embodiment for smashing the factors such as air themperature, the dosage of coating material, determine final system
Preparation Method, wherein
1, smashing mode combines
In terms of cost of material, commercial metal oxide powder does not reach Nano grade usually, or has Nano grade raw material but valence
Lattice are expensive, therefore select common grade metal-oxide powder raw material more economical；From feeding granularity requirement, machinery is smashed to this simultaneously
Without strict demand, air-flow smashing then has strict demand to this, and feeding granularity crosses conference and air-flow is made to smash production capacity reduction, machine damage
Consumption is big, therefore mechanical smashing processing coarse raw materials preferably, air-flow smash fine material of the processing through mechanical smashing processing preferably；
From smash powder the distribution of powder degree, air-flow is smashed to be smashed compared to machinery, and the size distribution of output powder is narrower；It is comprehensive
Consider economy, machine consumption, production capacity and product standard requirement, the present invention is by carrying out common metal oxides powder material
Machinery smashes, then carries out air-flow smashing.
2, the mechanical smashing time smashed
Inventor was the study found that in the case where other conditions are constant, metal-oxide powder raw material was smashed in machinery
Cheng Zhong, if smashing overlong time, sample particle can reunite, while product cost can also correspondingly increase.
Embodiment 1
3t zinc oxide coarse powder is weighed, is added in the mechanical crusher of 350rpm revolving speed, is crushed 45 minutes, and use simultaneously
Ultrasonic high speed atomisation assisted comminution, ultrasonic power 250W, high speed atomisation revolving speed are 24000rpm, and powder gathers title after smashing
Weight；Coating material Thioglycolic acid 0.15t is weighed in 5wt.% ratio, adjusts air-flow disintegrating machine, gas flow 3m3/ min,
Gas pressure is 0.6MPa, and air themperature is 100 DEG C, and dressing agent solution concentration is 5wt.%, and the flow for modifying agent solution is
1ml/min, being atomized is 1~20 μm, starts to spray into dressing agent after crushing, and it is 100 nanometers, that average diameter is obtained after the completion of crushing
Surface modification, finely dispersed zinc oxide nano-powder.
This is sample 1.
Embodiment 2
3t titanium dioxide coarse powder is weighed, is added in the mechanical crusher of 300rpm revolving speed, is crushed 60 minutes, and adopt simultaneously
With ultrasonic high speed atomisation assisted comminution, ultrasonic power 200W, high speed atomisation revolving speed is 22000rpm, and powder gathers after smashing
Weighing；Amino acids coating material 0.24t is weighed in 8wt.% ratio, adjusts air-flow disintegrating machine, gas flow 3m3/
Min, gas pressure 0.6MPa, air themperature are 110 DEG C, and dressing agent solution concentration is 6wt.%, modifies the flow of agent solution
For 1ml/min, being atomized is 1~20 μm, starts to spray into dressing agent after crushing, obtained after the completion of crushing average diameter be 100 nanometers,
Surface modification, finely dispersed titanium dioxide powder.
This is sample 2.
Embodiment 3
3t cadmium oxide coarse powder is weighed, is added in the mechanical crusher of 250rpm revolving speed, is crushed 45 minutes, and use simultaneously
Ultrasonic high speed atomisation assisted comminution, ultrasonic power 250W, high speed atomisation revolving speed are 20000rpm, and powder gathers title after smashing
Weight；Glycerine 0.18t is weighed in 6wt.% ratio, adjusts air-flow disintegrating machine, gas flow 3m3/ min, gas pressure are
0.6MPa, air themperature are 100 DEG C, and dressing agent solution concentration is 4wt.%, and the flow for modifying agent solution is 1ml/min, atomization
Be 1~20 μm, start to spray into dressing agent after crushing, obtained after the completion of crushing average diameter be 120 nanometers, surface modification,
Finely dispersed titanium dioxide powder.
This is sample 3.
Embodiment 4
3t stannic oxide coarse powder is weighed, is added in the mechanical crusher of 300rpm revolving speed, is crushed 30 minutes, and adopt simultaneously
With ultrasonic high speed atomisation assisted comminution, ultrasonic power 200W, high speed atomisation revolving speed is 24000rpm, and powder gathers after smashing
Weighing；Glycerine 0.33t is weighed in 10wt.% ratio, adjusts air-flow disintegrating machine, gas flow 2m3/ min, gas pressure are
0.7MPa, air themperature are 120 DEG C, and dressing agent solution concentration is 5wt.%, and the flow for modifying agent solution is 1.2ml/min, mist
1~20 μm is turned to, starts to spray into dressing agent after crushing, obtains that average diameter is 120 nanometers, surface has been repaired after the completion of crushing
Decorations, finely dispersed titanium dioxide powder.
This is sample 4.
Embodiment 5:
Take commercially available nano level modified titanium dioxide 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 6:
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 7:
Sample 1,2,3,4,5 is uniformly mixed with the tree powder body PBT, wherein ultraviolet absorber is with the tree powder body mass ratio
1:9；It is blended to be granulated through twin-screw extrusion after mixing and squeeze out, extrusion temperature is 160 DEG C, and revolving speed 150rpm obtains UV absorption
Master batch；Master batch is set into oven drying, drying temperature is 130 DEG C, time 5h；It is sliced uniformly mixing with PET afterwards, wherein master batch matter
Measuring accounting is 3%, and feeding spinning machine carries out melt spinning, and spinning temperature is 270 DEG C, speed 600m/min, at the beginning of filament spinning component
Beginning pressure 8MPa, is made high antiultraviolet fiber；Using woven mode, antiultraviolet fiber is used in broadwise, quality accounting is
15%, obtain target fabric 1,2,3,4,5.
With Lambda35 type ultraviolet/visible light spectrometer test fabric antiultraviolet (wavelength be 200~400nm) performance,
Test result is shown in Table
As result as it can be seen that modified powder prepared by the present invention has excellent effect in terms of ultraviolet radiation absorption function.
Function nano powder, if excellent functional effect can be embodied, key is whether 1. nano-powder particles itself sufficiently change
Property；2. nano-powder whether in the base stable fusion；3. whether nano-powder is uniformly dispersed in the base.This three, it is mutually auxiliary
It coordinates.Inventor, can be to prevent the study found that crushed by first wheel to nano-powder and ultrasound or high velocity fog processing simultaneously
The only soft-agglomerated phenomenon of nano-powder, so that it will not occur because of " aggregate particle size ", particle diameter distribution is wide, and modification is not filled
The case where dividing.In this way, just make in the case where the effectively particle diameter distribution of control nano-powder and modified abundant degree
Preparation-obtained nano-powder of the invention is obtained, it being capable of activation index with higher and dispersibility excellent in the base.Into
And even if compared with the higher common commercially available function powder of modifier content, fabric prepared by powder produced by the present invention,
More excellent ultraviolet radiation absorption effect can be embodied.
It is noted that being in the prior art that nanosize metal oxide powder is made in chemical method, the present invention uses
The powder of better effect has been made in physical method.It has abandoned in traditional preparation process, the method for now modifying post-processing, using ultrasound
It is atomized aid in treatment, and preferably optimizes process conditions, is promoted " dangling bonds " that metal oxide surface atom stretches to space
Absorption to air, the three-dimensional periodic gesture with the progress of crushing and the facilitation of ultrasonic atomizatio, inside metal oxide
Constantly on surface by very fast interruption, electronic state and the mutually dramatic variation of body, cause except the stabilization adsorption site such as bridging oxygen vacancy with
A degree of dissociation occur for gases of other outer absorption, affect in metal oxide system there is hybrid ionic and
Covalent bond effect can be crushed to the lower order of magnitude so that metal oxide stability dies down.
In conclusion the strong function nano powder preparation method for absorbing ultraviolet light provided by the present invention, using a small amount of table
Face dressing agent can be prepared by the superior nano-powder of performance；The strong function nano powder for absorbing ultraviolet light provided by the present invention
The preparation-obtained nano-powder of preparation method, partial size is small and has excellent surface active index and dispersibility in the base；
The strong function nano powder preparation method for absorbing ultraviolet light provided by the present invention, used zinc oxide, cadmium oxide, titanium dioxide
Titanium, stannic oxide, all have the function of good shielding ultraviolet rays, while also having non-stimulated to skin, do not decompose, never degenerate,
The good advantage of thermal stability, can be widely applied to the industries such as cosmetics, plastics, weaving；It is provided by the present invention absorb by force it is ultraviolet
Function nano powder prepared by the function nano powder preparation method of line, by after surface modification, may make that powder can be
It is evenly dispersed in matrix, so further preparing functional material, the strong effect for absorbing ultraviolet light can be given full play to；The present invention
The provided strong function nano powder preparation method for absorbing ultraviolet light, compared with traditional chemical preparation process, cost is reduced,
Easy to operate, the granularity of nano-powder is controllable, high production efficiency, can large-scale application in industrialized production.
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 (2)
1. a kind of strong function nano powder preparation method for absorbing ultraviolet light, it is characterised in that: including being carried out to metal oxide
Machinery smashes, and simultaneously using ultrasonic high speed atomisation assisted comminution；The mechanical crushing, smashing time are 0.5~1h, revolving speed
For 250~350rpm；It is described ultrasound high speed atomisation, wherein ultrasonic power be 200~250W, high speed atomisation revolving speed be 20000~
24000rpm；
Air-flow smashing, the air-flow crushing are carried out, gas flow is 2~4m3/ min, gas pressure are 0.5~0.7MPa, gas
Temperature is 90~120 DEG C；
It is surface modified while air-flow crushing, finally obtains product；
Dressing agent used in surface modification includes Thioglycolic acid, amino acids, one or more of in glycerine；The dressing agent
Dosage is the 1~10% of powder quality；
The metal oxide includes zinc oxide, cadmium oxide, titanium dioxide, one or more of in stannic oxide.
2. absorbing the function nano powder preparation method of ultraviolet light by force according to claim 1, it is characterised in that: the modification
Agent is 1~20 μm of drop, and mass concentration is 4~6wt.%.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1260366A (en) * | 2000-01-28 | 2000-07-19 | 中国科学院广州化学研究所 | Modified nm zinc oxide UV ray shielding and absorbing material |
| CN1657415A (en) * | 2005-02-02 | 2005-08-24 | 苏州大学 | Preparation method of nanometer zinc oxide |
| CN101543466A (en) * | 2009-04-23 | 2009-09-30 | 河南大学 | Nano zinc oxide surface modifying method |
| CN103360854A (en) * | 2012-03-28 | 2013-10-23 | 厦门纳诺泰克科技有限公司 | High-transparency low-radiation energy-saving combined material for glass and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP4195254B2 (en) * | 2002-03-06 | 2008-12-10 | 石原産業株式会社 | Rutile type titanium dioxide fine particles and method for producing the same |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1260366A (en) * | 2000-01-28 | 2000-07-19 | 中国科学院广州化学研究所 | Modified nm zinc oxide UV ray shielding and absorbing material |
| CN1657415A (en) * | 2005-02-02 | 2005-08-24 | 苏州大学 | Preparation method of nanometer zinc oxide |
| CN101543466A (en) * | 2009-04-23 | 2009-09-30 | 河南大学 | Nano zinc oxide surface modifying method |
| CN103360854A (en) * | 2012-03-28 | 2013-10-23 | 厦门纳诺泰克科技有限公司 | High-transparency low-radiation energy-saving combined material for glass and preparation method thereof |
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