CN1587059A - Process for preparing sunproof skin color zinc oxide nano powder - Google Patents
Process for preparing sunproof skin color zinc oxide nano powder Download PDFInfo
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- CN1587059A CN1587059A CN 200410051253 CN200410051253A CN1587059A CN 1587059 A CN1587059 A CN 1587059A CN 200410051253 CN200410051253 CN 200410051253 CN 200410051253 A CN200410051253 A CN 200410051253A CN 1587059 A CN1587059 A CN 1587059A
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- zinc oxide
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Abstract
The nano sunproof skin color zinc oxide powder is prepared with zinc nitrate hexahydrate in 4-6 molar portions and urea in 1 molar portion and through reaction at 100-120 deg.c for 3-7 hr, washing precipitate, filtering, ultrasonic treatment for 20-60 min, filtering, drying, grinding into powder, and heat treatment at 250-480 deg.c for 55-65 min. The preparation process is simple, low in cost, high in safety and easy in industrial application, and the product has high ultraviolet shielding performance.
Description
(1) technical field
The present invention relates to a kind of preparation method of Sun block complexional zinc oxide nano powder, belong to the preparation and the utilisation technology of nano material, can be applied to fields such as makeup and coating.
(2) technical background
As everyone knows, ZnO has good ultraviolet shielding function, nontoxic, safety of while, and raw material is inexpensive, is very ideal candidate material of sun-proof articles.But because the opalescence that the prepared pure ZnO powder of general technology has pale white is very unnatural as sun-proof articles.The non-ferrous metal element oxide that has many workers to try every possible means in ZnO to add other makes it painted, but these metallic elements itself are poisonous, harmful contaminate environment easily again, so do not advocate employing this method.Gu Da etc. according to the principle that forms colour of skin ZnO, are that raw material generates Zn (OH) with ZnSO4 and ammoniacal liquor in " the novel process research of ultra-fine colour of skin ZnO preparation " literary composition (" powder technology ", 1996 the 3rd phases)
2, add an amount of NH then therein
4HCO
3Generate zinc subcarbonate, carry out thermal decomposition process again and prepare colour of skin ZnO.Li Xiaoe etc. the new preparation process of the nanometer complexional zinc oxide " research " literary composition (" chemical engineering ", 2002 the 30th the 2nd phases of volume) with zinc salt (concentration is 0.1-0.5mol/L) solution under vigorous stirring with the (NH of 0.1-0.5mol/L
4)
2CO
3Reaction generates white precipitate---zinc subcarbonate, will precipitate after filtration, washing, ammonia scrubbing and organic solvent washing, oven dry again, obtains the nanometer complexional zinc oxide in 250-350 ℃ of following calcination.Also be to utilize the precipitator method, just raw materials cost has reduced, has simplified the operation technology also simply.More than these two kinds of methods all be to be divided into two steps, technology is still relatively long, raw material type is many, introduce impurity easily, thereby reduces performances such as ultraviolet shielded.
(3) Fa Ming content
The objective of the invention is to the problem that exists at prior art, a kind of preparation method of new Sun block complexional zinc oxide nano powder be provided, this method have that technology is simple, cost is low and safe, uv-shielding capacity good, be easy to characteristics such as industrialization.
The present invention is on the coprecipitation method basis, adds the method for sonic oscillation, with Zn (NO
3)
26H
2O, urea (CO (NH
2)
2) be raw material, mainly prepare fleshtone nano ZnO by control proportion of raw materials and treatment process, specifically comprise the steps:
(1) with the Zn (NO of 4-6 molar part
3)
26H
2The urea of O and 1 molar part is dissolved in the deionized water, control Zn
2+Concentration be 0.5-1.5mol/L, obtain A solution;
(2) A solution is placed under 100～120 ℃ of conditions reaction 3-7 hour, generate white precipitate B;
(3) with after the washing of B precipitate with deionized water, filtering, be reentered into 1.5-2 and doubly handled 20-60 minute to the deionized water for ultrasonic of solid precipitation volume;
(4) will pulverize after the sample filtering of gained in the step (3), the drying, and place 250 ℃～480 ℃ condition thermal treatments to obtain required Sun block complexional zinc oxide nano powder in 55-65 minute.
In aforesaid method, the concrete operations of step (2) are: A solution is contained in the glassware that lid arranged, then it is inserted reacting by heating in the process furnace of Controllable Temperature; In the step (3), sedimentary washing of B and filtration generally need repeat 5-7 time; In the step (4), the temperature of sample drying generally adopts 80-90 ℃, and thermal treatment is generally carried out in process furnace.
Zn (NO in the step (1)
3)
26H
2The mol ratio of O and urea preferably 4.5: 1, Zn
2+Concentration 1.2mol/L preferably; In the step (2), the optimum temps of reaction is 105 ℃, and optimum reacting time is 4.4 hours; In the step (3), the supersound process time is preferably 40 minutes; In the step (4), thermal treatment temp is preferably 400 ℃.
Compared with prior art, the present invention has following advantage or effect:
(1) sample of prepared in accordance with the method for the present invention is 48-55nm, and the wavelength below 370nm all has the specific absorption of 97.9-98.2%; In the visible region, has the colour of skin of nature; Color can reach existing level.Therefore, have sun-proof and the dual-purpose effect of foundation cream.
(2) in this preparation method, step of reaction does not adopt stirring method, but introduces common supersound process after reaction, preparation cycle and operation steps had both been shortened, also reduced the requirement of equipment, simultaneously owing to the kind that has reduced raw material, so the corresponding production cost that reduced.
(3) materials safety that adopts of present method is non-stimulated, does not have ammoniacal liquor in the raw material, and is harmless to operator, operation environment safety.
(4) concrete embodiment
Embodiment 1:
(1) with the Zn (NO of 4 molar part
3)
26H
2The urea of O and 1 molar part is dissolved in the deionized water, control Zn
2+Concentration be 1.5mol/L, obtain A solution;
(2) A solution is placed under 100 ℃ of conditions reaction 3 hours, generate white precipitate B;
(3) with after the washing of B precipitate with deionized water, filtering (repeating 5 times), being reentered into volume is 60 minutes (the getting final product under the room temperature) of deionized water for ultrasonic processing of 2 times of volumes of solid precipitation;
(4) with the sample filtering of gained in the step (3), pulverizing after the drying under 85 ℃ of conditions, and place 400 ℃ of condition thermal treatments 60 minutes, obtain required Sun block complexional zinc oxide nano powder.
Products obtained therefrom adopts the general ultraviolet visible spectrum method in this area to measure, and the ultraviolet region specific absorption that records this product reaches 97.93%; Detect by an unaided eye and be the shallow colour of skin.
Embodiment 2:
Other is with embodiment 1.In the step (1), Zn (NO
3)
26H
2The mol ratio of O and urea is 6: 1, Zn
2+Concentration be 0.5mol/L; In the step (2), temperature of reaction is 120 ℃, and the reaction times is 7 hours; The supersound process time is 20 minutes in the step (3); Thermal treatment temp is 250 ℃ in the step (4), and the time is 55 minutes.
Products obtained therefrom adopts the general ultraviolet-visible light spectral method in this area to measure, and the specific absorption that records the UV-light of this product reaches 98.02%; Detect by an unaided eye: color is the shallow colour of skin, and the color of the ZnO in the ratio 1 is dark slightly.
Embodiment 3:
Other is with embodiment 1.In the step (1), Zn (NO
3)
26H
2The mol ratio of O and urea is 5: 1, Zn
2+Concentration be 1.1mol/L; In the step (2), temperature of reaction is 105 ℃, and the reaction times is 5 hours; The supersound process time is 50 minutes in the step (3); Thermal treatment temp is 480 ℃ in the step (4), and the time is 65 minutes.
Products obtained therefrom adopts the general ultraviolet-visible light spectral method in this area to measure, and the specific absorption that records the UV-light of this product reaches 98.19%; Detect by an unaided eye, color is the shallow colour of skin, and the color of the ZnO in the ratio 2 is dark slightly.
Embodiment 4:
Other is with embodiment 1.In the step (1), Zn (NO
3)
26H
2The mol ratio of O and urea is 4.5: 1, Zn
2+Concentration be 1.2mol/L; In the step (2), temperature of reaction is 105 ℃, and the reaction times is 4.4 hours; The supersound process time is 40 minutes in the step (3).
Products obtained therefrom adopts the general ultraviolet-visible light spectral method in this area to measure, and the specific absorption that records the UV-light of this product reaches 98.12%; Detect by an unaided eye, color is the colour of skin, and the color of the ZnO in the ratio 3 is dark slightly.
Claims (7)
1, a kind of preparation method of Sun block complexional zinc oxide nano powder is characterized in that comprising the steps:
(1) with the Zn (NO of 4-6 molar part
3)
26H
2The urea of O and 1 molar part is dissolved in the deionized water, control Zn
2+Concentration be 0.5-1.5mol/L, obtain A solution;
(2) A solution is placed under 100～120 ℃ of conditions reaction 3-7 hour, generate white precipitate B;
(3) with after the washing of B precipitate with deionized water, filtering, be reentered into the deionized water for ultrasonic that doubles the solid precipitation volume and handled 20-60 minute;
(4) will pulverize after the sample filtering of gained in the step (3), the drying, and place 250 ℃～480 ℃ condition thermal treatments to obtain required Sun block complexional zinc oxide nano powder in 55-65 minute.
2, the method for claim 1 is characterized in that: the concrete operations of step (2) are: A solution is contained in the glassware that lid arranged, then it is inserted reacting by heating in the process furnace of Controllable Temperature; In the step (3), sedimentary washing of B and filtration need repeat 5-7 time; In the step (4), the temperature of sample drying is 80-90 ℃, and thermal treatment is carried out in process furnace.
3, method as claimed in claim 1 or 2 is characterized in that: Zn (NO in the step (1)
3)
26H
2The mol ratio of O and urea is 4.5: 1, Zn
2+Concentration be 1.2mol/L.
4, method as claimed in claim 1 or 2 is characterized in that: in the step (2), the temperature of reaction is 105 ℃, and the reaction times is 4.4 hours.
5, method as claimed in claim 1 or 2 is characterized in that: in the step (3), the supersound process time is 40 minutes.
6, method as claimed in claim 1 or 2 is characterized in that: in the step (4), thermal treatment temp is 400 ℃.
7, method as claimed in claim 1 or 2 is characterized in that: Zn (NO in the step (1)
3)
26H
2The mol ratio of O and urea is 4.5: 1, Zn
2+Concentration be 1.2mol/L; In the step (2), the temperature of reaction is 105 ℃, and the reaction times is 4.4 hours; In the step (3), the supersound process time is 40 minutes; In the step (4), thermal treatment temp is 400 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410051253 CN1261357C (en) | 2004-08-30 | 2004-08-30 | Process for preparing sunproof skin color zinc oxide nano powder |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410051253 CN1261357C (en) | 2004-08-30 | 2004-08-30 | Process for preparing sunproof skin color zinc oxide nano powder |
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| Publication Number | Publication Date |
|---|---|
| CN1587059A true CN1587059A (en) | 2005-03-02 |
| CN1261357C CN1261357C (en) | 2006-06-28 |
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ID=34602417
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200410051253 Expired - Fee Related CN1261357C (en) | 2004-08-30 | 2004-08-30 | Process for preparing sunproof skin color zinc oxide nano powder |
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|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891239B (en) * | 2009-05-18 | 2012-04-25 | 合肥学院 | Method for preparing red zinc oxide nano powder |
| CN108056926A (en) * | 2018-01-29 | 2018-05-22 | 华南师范大学 | The preparation method and applications of long wave blackspot effect UV blocker |
-
2004
- 2004-08-30 CN CN 200410051253 patent/CN1261357C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891239B (en) * | 2009-05-18 | 2012-04-25 | 合肥学院 | Method for preparing red zinc oxide nano powder |
| CN108056926A (en) * | 2018-01-29 | 2018-05-22 | 华南师范大学 | The preparation method and applications of long wave blackspot effect UV blocker |
| CN108056926B (en) * | 2018-01-29 | 2022-04-05 | 华南师范大学 | Preparation method and application of long-wave black spot effect ultraviolet separant |
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| Publication number | Publication date |
|---|---|
| CN1261357C (en) | 2006-06-28 |
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