CN1287138A - Surface treatment for nanometer-level titania - Google Patents
Surface treatment for nanometer-level titania Download PDFInfo
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- CN1287138A CN1287138A CN 99114418 CN99114418A CN1287138A CN 1287138 A CN1287138 A CN 1287138A CN 99114418 CN99114418 CN 99114418 CN 99114418 A CN99114418 A CN 99114418A CN 1287138 A CN1287138 A CN 1287138A
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- surface treatment
- titanium oxide
- nano titanium
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Abstract
Nanometer-level titania material is treated through the steps of grading, dispersing, drying, hydrophilic surface treatment, purifying, dispersing, drying, heat treatment, grading, dispersing, hydrophobic surface treatment, drying, and crushing. The first eight steps constitute the hydrophilic treatment and the whole 13 steps constitute the hydrophobic treatment. The process produces nanometer-level titania with superfine and homogeneous size, great specific surface area, high UV-shielding performance and excellent dispersity, and may be used widely in sun-screening whitening and moisture maintaining cosmetics.
Description
The present invention relates to a kind of surface treatment of nano titanium oxide.
In recent years, when the nano titanium oxide synthesis technique constantly makes further progress, the research of aftertreatment technology also has been subjected to attention.By coating certain compound, to improve the application performance of nano titanium oxide, as weathering resistance, photostabilization, dispersiveness, surfactivity etc. on the nano titanium oxide surface.To existing many relevant report and the application of nano titanium oxide surface modification, the following two kinds of approach of the many employings of various surface treatments: inorganic coating is finished with liquid-phase coprecipitation, and organic absorption is then finished when comminution by gas stream.The titanium dioxide powder that makes like this, grain diameter is difficult for Be Controlled, and the every controlled variable in the surface treatment process is not clear, causes top coat inhomogeneous, and it is not good particularly to be applied in the makeup dispersiveness, and a lot of indexs do not reach expected effect.
The object of the present invention is to provide the surface treatment method of good wetting ability of shielding ultraviolet rays performance and hydrophobic nano-titanium dioxide.
For achieving the above object, the surface treatment method of a kind of nano titanium oxide of the present invention, with the nano titanium oxide is raw material, and its key step is: (1) classification, (2) dispersion, (3) drying, (4) Hydrophilic Surface Treatment, (5) purifying, (6) dispersion, (7) drying, (8) thermal treatment, (9) classification, (10) disperse, (11) hydrophobic surface is handled, (12) are dry, pulverize (13).
Surface treatment has hydrophilic surface to handle and hydrophobic surface treatments, and it is (1)-(8) steps that hydrophilic surface is handled key step, and the hydrophobic surface treatments key step is (1)-(13) steps.
Surface treatment process all is to carry out in liquid phase, its surface treatment is compound surface and coats, with the de-salted water is dispersion medium, adopt wet method to coat treatment technology, use tensio-active agent in the wet processing process, its temperature is controlled between 60-150 ℃ in the wet method coating process, the consumption of tensio-active agent be controlled at nano titanium oxide heavy 5% in, need high-speed stirring in the preparation process.Heat-treatment temperature range is in 1000 ℃, and wherein drying process is a spraying drying, and drying temperature is below 150 ℃.In the hydrophilic nano titanium dioxide surface treating processes with Na
2SiO
3, Al
2(SO
4)
3Deng being coating, be coating with organic lipid such as stearic acid series product etc. in the hydrophobic nano-titanium dioxide surface treatment process.
It is raw material that the present invention adopts nano titanium oxide, coats through organic and inorganic surface respectively and forms wetting ability and hydrophobic nano-titanium dioxide, and its particle diameter is even, ultra-fine, specific surface area is big, and shielding ultraviolet rays is to the injury of human body effectively.
Embodiment one: a kind of surface treatment of hydrophilic nano titanium dioxide: the choosing of (1) main raw material, (2) dispersion, (3) classification, (4) Hydrophilic Surface Treatment, (5) purifying, (6) disperse, (7) are dry, (8) thermal treatment.
(1) choosing of main raw material: the present invention selects for use the rutile type nano titanic oxide of Chinese patent 96117100.6 manufacturings as main raw material.Main raw material oneself preparation has reduced the consumption of cost, the nano titanium oxide particle diameter homogenous superfine of this method preparation, and specific surface is big, and ultraviolet ray is had the excellent absorption performance, and nontoxic pollution-free, is easy to suitability for industrialized production.
The significant parameter of rutile type nano titanic oxide is:
Outward appearance: white powder
Surface properties: wetting ability
Particle diameter (nm):＜100
Specific surface area (m
2/ g):＞35
PH value: 6-8
Purity (%):＞98.5
(2) disperse: this process is to adopt in order to carry out the even firm of size classification and the processing of assurance inorganic surfaces, nano titanium oxide is mixed with the slurry that solid content is 5%-30%, add polymeric surface active agent, make dispersion agent as polyoxyethylene glycol, trolamine, polymerizable acrylic monomer thing etc., reduce the agglomerating force between the particle, reduce agglomeration, the consumption of tensio-active agent is generally determined according to solid content of slurry, be generally titanium dioxide heavy 5% in, emulsification 1-3 hour.
(3) classification: this process is according to Stoker Si Dinglv: same substance is in same medium, and under the same terms, its sedimentation speed varies in size with material grains and different, and big more its settling velocity of particle is fast more, and particle is more little, and its settling velocity is slow more.Remove the coarse particles that does not meet the particle diameter requirement.
(4) Hydrophilic Surface Treatment: utilize Na
2SiO
3And Al
2(SO
4)
3Nano titanium oxide is carried out compound surface handle Na
2SiO
3With contained SiO
2Meter, Al
2(SO
4)
3With contained Al
2O
3Meter, the consumption of treatment agent is with TiO
2Meter: SiO
2: 1-10%, Al
2O
3: 1%-5%, pH value is controlled at more than 6.In reaction times in this process, stirring velocity and temperature all must have strict control.
(5) purifying: for purity, whiteness and the dispersiveness that improves powder, must be through purifying repeatedly to remove SO
4 2-, Na
+Deng foreign ion.
(6) disperse: in order to obtain finely dispersed slurry, prevent from the drying and dehydrating process hard aggregation to take place, the present invention adopts polymeric surface active agent such as polyoxyethylene glycol, polymerizable acrylic monomer thing, trolamine etc. as dispersion agent, consumption be controlled at titanium dioxide heavy 5% in, emulsification times is 0.5-4 hour.
(7) drying: the present invention adopts spray-dired method, prevents that as far as possible particle from growing up, and removes mechanical water, the high quality powder.
(8) thermal treatment: the heat-treatment temperature range broad of this technology, generally between 400-800 ℃, determine heat treated actual temp according to actual needs.
The significant parameter of the hydrophilic titanium oxide that the present invention is prepared is:
Outward appearance: white powder
Surface property: wetting ability
Particle diameter (nm):＜100
Specific surface area (m
2/ g)＞10
PH value: 6-8
Drying loss (%):＜0.55
Burning decrement (%):＜0.3
SPF (sun protection factor) (spf value):＞20
Arsenic content (ppm):＜0.5
Lead content (ppm):＜1
Mercury content (ppm):＜0.01
Embodiment two: the surface treatment of hydrophobic nano-titanium dioxide, preparation hydrophilic nano titanium dioxide with embodiment one is raw material, the steps include: that (9) classification, (10) hydrophilic nano titanium dioxide disperse, (11) hydrophobic surface is handled, (12) are dry, pulverize (13).
(9) classification: utilize the horizontal spiral centrifugal classifier, remove undesirable macrobead.
(10) hydrophilic nano titanium dioxide disperses: in order to obtain finely dispersed slurry, prevent from the drying and dehydrating process hard aggregation to take place, this process adopts high molecular tensio-active agent, as polyoxyethylene glycol, tween series, trolamine or polymerizable acrylic monomer thing, consumption be controlled at titanium dioxide heavy 5% in, emulsification times is 0.5-4 hour.
(11) hydrophobic surface is handled: adopting stearic acid series is surperficial coating, de-salted water is as dispersion medium, and add potassium oleate, glyceryl monostearate, sodium laurate or Sodium dodecylbenzene sulfonate tensio-active agent, the consumption of tensio-active agent be controlled at titanium dioxide weight 5% in.In surface treatment process, temperature is controlled at 60 ℃-100 ℃, coating is the stearic acid series product, as stearic acid, calcium stearate, aluminum stearate etc., consumption is controlled at the 1%-10% of titanium dioxide weight, be dispersed in coating dissolving in the de-salted water after, more classified slurry is added wherein, emulsification 1-2 hour, TiO
2Concentration is controlled at 10%-30%.
(12) drying: adopt rotation rapid dryer or spray-drier.
(13) pulverize: adopt the Emery grains micronizer mill, powder particle is pulverized the particle that reverts to raw state.
The hydrophobic nano-titanium dioxide significant parameter of the present invention's preparation is:
Crystal formation: rutile-type
Outward appearance: white powder
Surface properties: hydrophobicity
Purity (%):＞98.5
Particle diameter (nm):＜100
Specific surface area (m
2/ g):＞10
SPF (sun protection factor) (spf value):＞20
Drying loss (%):＜3.3
Arsenic content (ppm):＜0.5
Lead content (ppm):＜1
Mercury content (ppm):＜0.01
Claims (11)
1, a kind of surface treatment method of nano titanium oxide, with the nano titanium oxide is raw material, its key step is: (1) classification, (2) dispersion, (3) drying, (4) Hydrophilic Surface Treatment, (5) purifying, (6) disperse, (7) are dry, (8) thermal treatment, and (9) classification, (1 0) disperse, (11) hydrophobic surface is handled, (12) are dry, pulverize (13).
2, the surface treatment of a kind of nano titanium oxide according to claim 1 is characterized in that being divided into hydrophilic surface and handles and hydrophobic surface treatments, and it is (1)-(8) steps that hydrophilic surface is handled key step; The hydrophobic surface treatments key step is (1)-(13).
3, the surface treatment of a kind of nano titanium oxide according to claim 1 is characterized in that surface treatment is to carry out in liquid phase.
4, the surface treatment of a kind of nano titanium oxide according to claim 1 is characterized in that its surface treatment is compound surface and coats, and is dispersion medium with the de-salted water, adopts wet method to coat treatment technology.
5, the surface treatment of a kind of nano titanium oxide according to claim 1 is characterized in that using tensio-active agent in the wet processing process.
6, the surface treatment of a kind of nano titanium oxide according to claim 1 is characterized in that its temperature is controlled between 60-150 ℃ in the wet method coating process.
7, the surface treatment of a kind of nano titanium oxide according to claim 5, it is characterized in that the surplus consumption of surfactivity be controlled at nano titanium oxide heavy 5% in.
8, the surface treatment of a kind of nanometer titanium dioxide iron according to claim 1 is characterized in that needing high-speed stirring in the preparation process, and needs suitably heating.
9, the surface treatment of a kind of nano titanium oxide according to claim 1 is characterized in that its thermal treatment temp is controlled at below 800 ℃.
10, the surface treatment of a kind of nano titanium oxide according to claim 1 is characterized in that its drying process is a spraying drying, and drying temperature is below 150 ℃.
11, the surface treatment of a kind of nano titanium oxide according to claim 1 is characterized in that it is to be coating with organic lipid etc. that its hydrophobic surface is handled.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99114418 CN1287138A (en) | 1999-09-03 | 1999-09-03 | Surface treatment for nanometer-level titania |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99114418 CN1287138A (en) | 1999-09-03 | 1999-09-03 | Surface treatment for nanometer-level titania |
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| Publication Number | Publication Date |
|---|---|
| CN1287138A true CN1287138A (en) | 2001-03-14 |
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ID=5277505
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|---|---|---|---|
| CN 99114418 Pending CN1287138A (en) | 1999-09-03 | 1999-09-03 | Surface treatment for nanometer-level titania |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102009037A (en) * | 2010-10-25 | 2011-04-13 | 江苏考普乐新材料股份有限公司 | Method for protecting metal by photoelectrochemistry |
| CN103613955A (en) * | 2013-11-29 | 2014-03-05 | 芮城新泰纳米材料有限公司 | Method for preparing special nano calcium carbonate (nano-CaCO3) for vehicle adhesive |
| CN111484755A (en) * | 2020-04-09 | 2020-08-04 | 行謇人工智能科技(上海)有限责任公司 | Lauric acid modified nano titanium dioxide and preparation method and application thereof |
| CN113184902A (en) * | 2021-05-20 | 2021-07-30 | 黑龙江省公路建设中心 | Method for hydrophobic modification of nano titanium dioxide |
-
1999
- 1999-09-03 CN CN 99114418 patent/CN1287138A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102009037A (en) * | 2010-10-25 | 2011-04-13 | 江苏考普乐新材料股份有限公司 | Method for protecting metal by photoelectrochemistry |
| CN102009037B (en) * | 2010-10-25 | 2013-06-19 | 江苏考普乐新材料股份有限公司 | Method for protecting metal by photoelectrochemistry |
| CN103613955A (en) * | 2013-11-29 | 2014-03-05 | 芮城新泰纳米材料有限公司 | Method for preparing special nano calcium carbonate (nano-CaCO3) for vehicle adhesive |
| CN103613955B (en) * | 2013-11-29 | 2015-05-13 | 芮城新泰纳米材料有限公司 | Method for preparing special nano calcium carbonate (nano-CaCO3) for vehicle adhesive |
| CN111484755A (en) * | 2020-04-09 | 2020-08-04 | 行謇人工智能科技(上海)有限责任公司 | Lauric acid modified nano titanium dioxide and preparation method and application thereof |
| CN113184902A (en) * | 2021-05-20 | 2021-07-30 | 黑龙江省公路建设中心 | Method for hydrophobic modification of nano titanium dioxide |
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