CN101172641B - Method of producing fleshtone nano-zinc oxide - Google Patents
Method of producing fleshtone nano-zinc oxide Download PDFInfo
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- CN101172641B CN101172641B CN2007101337313A CN200710133731A CN101172641B CN 101172641 B CN101172641 B CN 101172641B CN 2007101337313 A CN2007101337313 A CN 2007101337313A CN 200710133731 A CN200710133731 A CN 200710133731A CN 101172641 B CN101172641 B CN 101172641B
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Abstract
The invention discloses a rapid preparative method of skin-color nanometer zinc oxide, belonging to the field of preparing inorganic nanometer material. The invention has the technical proposal that soluble zinc salt is used as the main raw material, nitrogen-rich ammonium salt is used as the main fuel; the soluble zinc salt, the nitrogen-rich ammonium salt and few combustion improver are mixed in certain ratio to acquire paste material; the mixed paste material is put to a container which is preheated to 600 to 900 DEGC, the substance after combustion is collected and the powder of skin-color nanometer zinc oxide in flocculent form is obtained after completing the combustion process. The nanometer powder produced by the invention has the advantages of small granularity, even distribution, equal color, good dispersivity and strong screen property against ultraviolet. Because of rapid synthesizing speed, low cost, high yield, and good effect in preventing pollution, the process has great value in industrialized popularization.
Description
Technical field
The present invention relates to a kind of fast preparation method of fleshtone nano-zinc oxide, belong to field of inorganic nano-material preparation.
Background technology
Many characteristics such as that nano zine oxide (ZnO) has is nontoxic, non-migrating, specific surface area is big, magnetic is strong, absorption and scatters ultraviolet ability are strong can be widely used in packaging material for food, transmitter, effective catalyst, medical bactericide, makeup sun-screening agent, magneticsubstance etc.In recent years, because ozonosphere is constantly destroyed, the sickness rate of skin carcinoma increases, people recognize the injury of ultraviolet ray to human body more and more strongly, thereby promoted sun care preparations to develop rapidly, nano-ZnO is because have stronger ultraviolet shielded ability and performance such as excellent chemical stability, thermostability, nontoxicity and become ideal uvioresistant additive in the makeup.But simple nano-ZnO often presents white, be used for skin that makeup can make the people and seem pale and nature, the initial method that solves is to mix use with other pigment dyestuff or mineral dye, not only troublesome poeration, and pigment easily separates out, and influences its use properties.
In recent years, carried out R and D to ZnO is painted both at home and abroad, traditional method is to utilize the solid solution of element or compound to make ZnO painted, and for example the manganese oxide solid solution can make it be yellow in ZnO, and plumbous oxide then makes its show pink.But these heavy metals are harmful, especially are unwell to cosmetic industry.Researchist Li D, Saito N, Ohashi N, et al. (Synthesis of nanosized nitrogen containingMOX-ZnO (M=W, V, Fe) composite powders by spray pyrolysis and theirphotocatalysis in the gas phase acetaldehyde decomposition[A] .In:Li C.The3rd Asia Pacific Congress on Catalysis[C] .Dalian:Dalian Institute ofChemical Physics Press, 2003.589-590.) when investigating the adulterated ZnO photocatalyst of nitrogen, find, nitrogen mixes can cause the ZnO lattice imperfection, a spot of nitrogen doping can make ZnO take place visible light-responded and present the colour of skin, because this colour of skin is to be fused to ZnO crystal admittedly by nitrogen-atoms to make it painted, thereby harmless, this preparation for fleshtone nano ZnO provides new thinking.Japanese Patent (clear 55227857) discloses a kind of at NH
3Decompose the method that zinc oxalate prepares red zinc oxide in the atmosphere." preparation of colour of skin ultra-micro powder zinc oxide " ([J] coatings industry (1991), (4): 4～7) in the literary composition, disclose a kind of at NH
3And H
2The thermolysis zinc oxalate is prepared the method for colour of skin ultra-micro powder ZnO in the mixed atmosphere; " the novel process research of ultra-fine colour of skin ZnO preparation " ([J] powder technology, 1996,2 (3): 27～30) in the literary composition,, in the thermal decomposition process of zinc subcarbonate, add an amount of NH according to the principle that forms colour of skin ZnO
4HCO
3Preparation colour of skin ZnO; At " preparation and the sign of overweight force method nanometer complexional zinc oxide " ([J] Beijing University of Chemical Technology journal, 2004,31 (4): 28～31), proposed to be equipped with and added a small amount of coating materials in the process of nano zine oxide and carry out in-situ modification with the hypergravity legal system, the novel process of preparation colour of skin ZnO, and analyze to its finishing mechanism with to the ultraviolet-visible absorption mechanism; " the new preparation process research of nanometer complexional zinc oxide " ([J] chemical engineering, 2002,39 (2): 41～44) technical scheme in the literary composition is to generate zinc subcarbonate with zinc salt and volatile salt reaction, then after filtration, water washing, ammoniacal liquor wash, organic solvent is washed, and handles obtaining the nanometer complexional zinc oxide after the oven dry at a certain temperature; " the molten legal system of ammonia is equipped with the research of complexional zinc oxide " ([J] fine-chemical intermediate, 2004,, 34 (4): 60～62) in the literary composition, disclose and used the ammonia solvent zinc hydroxide, separated out secondary sedimentation by ammonia still process again, made the method for complexional zinc oxide at last; Chinese invention patent (CN1261357C) discloses a kind of preparation method of Sun block complexional zinc oxide nano powder, it adopts zinc nitrate and urea to react 3-7 hour down at 100-120 ℃, through precipitation, washing, filtration, ultrasonication, refilter, drying, handle at 250-480 ℃ then and obtained fleshtone nano-zinc oxide in about 1 hour.Above-mentioned several method substantially all is to adopt solution deposit, all need in the building-up process through precipitating, filter, wash, calcine these a series of processes, the operational path complexity, generated time is long, material composition is many, introduces impurity easily, and some technology also will be used a large amount of organic solvents, environment there is pollution, thereby has restricted its further application aborning.
Combustion synthesis method is owing to it has the efficiency height, is swift in response, is subjected to advantages such as the external environment factor affecting is little, repeatability is high, the synthetic product particle diameter is little, thereby cause that people greatly pay close attention to, being used for the synthesis of nano powder has many researchs report, as people such as Cheng-Shiung Lin with amino acid and zinc nitrate mix be pressed into bulk after, wrap up one deck detonator again at its skin, come initiation reaction by lighting detonator, generate the zinc oxide of different shape.People such as Zhao Yuna adopt combustion method to synthesize the zinc oxide of cage structure." self-propagating combustion ZnO powder preparing voltage dependent resistor " ([J] silicate journal, 2006,, 34 (9): 1055～1059) in the literary composition, disclosing with zinc nitrate, urea and other additive is raw material, by the disposable ZnO varistor dopen Nano powder that synthesized of self-propagating combustion.But up to the present, the content for preparing fleshtone nano-zinc oxide about combustion synthesis method is not appeared in the newspapers.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, provide a kind of reacting balance in order and the preparation method of the fleshtone nano-zinc oxide that smog is few, security is good, productive rate is high.
For reaching above purpose, technical scheme of the present invention is to adopt following procedure of processing to prepare fleshtone nano-zinc oxide:
(1) soluble zinc salt is made into the aqueous solution that concentration is 0.1～1.0mol/L;
(2) in above-mentioned zinc salt solution, be after 0.1～1.0: 1 the mixed with rich nitrogen ammonium salt fuel and zinc salt by mass ratio, the ignition dope that adds said mixture total amount 0.1～0.5% again, the mode by mechanical stirring or grinding is prepared into heavy-gravity paste liquid;
(3) described paste liquid is put into to be heated to temperature in advance be that 600 ℃～900 ℃ container burns, finished the back and collect products of combustion and obtain fleshtone nano-zinc oxide.
In the technique scheme, described zinc salt is water-soluble zinc salt, comprises zinc chloride, zinc sulfate, nitrate or zinc citrate.
Described rich nitrogen ammonium salt fuel comprises one or more the mixture in ammonium sulfate, volatile salt, bicarbonate of ammonia, ammoniumper chlorate, ammonium nitrate, urea or the amino acid.
Described ignition dope is polyoxyethylene glycol, citric acid, polyvinyl alcohol, trolamine or nonionogenic tenside.
Compared with prior art, outstanding advantage of the present invention is:
1, operational path is simple, the combustion processes quick and stable, and non smoke discharges in the reaction process, the productive rate height.
2, entire reaction finishes in the short period of time at the utmost point that (20～50s), that the product of preparation has is fluffy, color and luster is even, particle diameter is little, narrowly distributing, purity advantages of higher.
3, this technology does not need special production equipment, the efficiency height, and the product easily collecting, no waste water and gas discharging, save energy especially is fit to serialization production.
Description of drawings
Fig. 1 is the X diffractogram of the prepared fleshtone nano ZnO of one embodiment of the invention;
Fig. 2 is the sem photograph of the prepared fleshtone nano ZnO of one embodiment of the invention;
Fig. 3 is the x-ray photoelectron spectroscopy figure of the prepared fleshtone nano ZnO of one embodiment of the invention;
Fig. 4 is the ultraviolet permeability figure of fabric before and after the prepared fleshtone nano ZnO arrangement of one embodiment of the invention.
Embodiment
Below in conjunction with drawings and Examples the present invention is further described:
Embodiment 1:
The 4.15g zinc nitrate is dissolved in the 20ml deionized water, be made into settled solution, in zinc nitrate aqueous solution, add 0.35g urea, 0.1g ammoniumper chlorate, 0.01g citric acid and 0.02g polyoxyethylene glycol, high speed machine stirs the back and becomes heavy-gravity paste liquid, the porcelain dish that fills the paste mixing liquid is put into the retort furnace that is heated to 800 ℃ in advance, combustion processes (approximately about 25s) finishes the back and collects products of combustion, need not to grind and promptly get the cotton-shaped colour of skin ZnO powder of 1.02g (theoretical value is 1.13g), non smoke release in the combustion processes.
Referring to accompanying drawing 1, the colour of skin ZnO nano-powder X diffraction analysis result who makes by embodiment 1 described preparation method shows: [101], [002] and strong diffraction peaks such as [100] more sharp-pointed, [102], [110], [103] and weak diffraction peak such as [102] also all very obvious, (JCPDF 5-664) is in full accord with the zinc oxide normal data.
Referring to accompanying drawing 2, by the colour of skin ZnO nano-powder that embodiment 1 described preparation method makes, by scanning electron microscope image as can be known, particle diameter is 60nm, and particle distribution is even, good dispersity.
Referring to accompanying drawing 3, the colour of skin ZnO nano-powder that makes by embodiment 1 described preparation method, by xps energy spectrum as can be known, the main peak that is positioned at 399.64eV ascribes the N of Zn-N key constraint to, do not find peak from free state N or N2, illustrate that the N atom is that form with acceptor impurity is present in the lattice, its content is 1.02%
Referring to accompanying drawing 4, before and after the colour of skin ZnO nano-powder arrangement that makes by embodiment 1 described preparation method the ultraviolet permeability of fabric as can be known, the synthetic powder has shielding preferably to ultraviolet ray.
Embodiment 2:
The 4.15g zinc nitrate is dissolved in the 20ml deionized water, be made into settled solution, in zinc nitrate aqueous solution, add the propellant combination and the 0.02g nonionogenic tenside that contain 0.25g urea, 0.12g ammonium nitrate, 0.18g volatile salt, high speed machine stirs the back and becomes heavy-gravity paste liquid, the porcelain dish that fills the paste mixing liquid is put into the retort furnace that is heated to 850 ℃ in advance, combustion processes (approximately about 15s) finishes the back and collects products of combustion, need not to grind and promptly get the cotton-shaped colour of skin ZnO powder of 0.98g (theoretical value is 1.13g), non smoke release in the combustion processes.
Embodiment 3:
4.15g zinc sulfate is dissolved in the 15ml deionized water, be made into settled solution, in zinc sulfate solution, add and contain 0.30g urea, 0.15g Padil, 0.10g the propellant combination of ammonium nitrate and 0.01g polyethylene glycol type nonionogenic tenside, in mortar, grind to form heavy-gravity paste liquid, the porcelain dish that fills the paste mixing liquid is put into the retort furnace that is heated to 700 ℃ in advance, combustion processes (approximately about 30s) finishes the back and collects products of combustion, need not to grind and promptly get the cotton-shaped colour of skin ZnO powder of 1.01g (theoretical value is 1.23g), low smoke employing weak base absorption in the combustion processes.
Embodiment 4:
The 4.15g zinc citrate is dissolved in the 20ml deionized water, be made into settled solution, in the zinc citrate aqueous solution, add the propellant combination and the 0.01g trolamine that contain 0.25g urea, 0.15g citric acid, 0.15g ammonium nitrate, in mortar, grind to form heavy-gravity paste liquid, the porcelain dish that fills the paste mixing liquid is put into the retort furnace that is heated to 650 ℃ in advance, combustion processes (approximately 30s) finishes the back and collects products of combustion, need not to grind and promptly get the cotton-shaped colour of skin ZnO powder of 1.37g (theoretical value is 1.62g), non smoke release in the combustion processes.
Claims (4)
1. the preparation method of a fleshtone nano-zinc oxide is characterized in that preparation process is as follows:
(1) soluble zinc salt is made into the aqueous solution that concentration is 0.1～1.0mol/L;
(2) in above-mentioned zinc salt solution, be after 0.1～1.0: 1 the mixed with rich nitrogen ammonium salt fuel and zinc salt by mass ratio, the ignition dope that adds said mixture total amount 0.1～0.5% again, the mode by mechanical stirring or grinding is prepared into heavy-gravity paste liquid;
(3) described paste liquid is put into to be heated to temperature in advance be that 600 ℃～900 ℃ container burns, finished the back and collect products of combustion and obtain fleshtone nano-zinc oxide.
2. the preparation method of a kind of fleshtone nano-zinc oxide according to claim 1, it is characterized in that: described zinc salt is water-soluble zinc salt, comprises zinc chloride, zinc sulfate, zinc nitrate or zinc citrate.
3. the preparation method of a kind of fleshtone nano-zinc oxide according to claim 1 is characterized in that: described rich nitrogen ammonium salt fuel comprises one or more the mixture in ammonium sulfate, volatile salt, bicarbonate of ammonia, ammoniumper chlorate or the ammonium nitrate.
4. the preparation method of a kind of fleshtone nano-zinc oxide according to claim 1, it is characterized in that: described ignition dope is polyoxyethylene glycol, citric acid, polyvinyl alcohol or trolamine.
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| CN101891239B (en) * | 2009-05-18 | 2012-04-25 | 合肥学院 | Method for preparing red zinc oxide nano powder |
| CN102180513B (en) * | 2011-06-01 | 2013-03-06 | 舟山市质量技术监督检测院 | Method for preparing hexagonal pyramid-like zinc oxide by low temperature combustion synthesis method |
| CN102502779A (en) * | 2011-09-28 | 2012-06-20 | 苏州苏纳特科技有限公司 | Quick preparation method for silver-loaded zinc oxide nanometer composite powder |
| CN104017394B (en) * | 2013-12-24 | 2016-10-05 | 韦先飞 | The dry powder emulsion paint coating of efficient-decomposition formaldehyde |
| CN105708718A (en) * | 2016-04-13 | 2016-06-29 | 广州丹奇日用化工厂有限公司 | Acne-removal cosmetic composition containing nano-zinc |
| CN107385935A (en) * | 2017-06-28 | 2017-11-24 | 常州创索新材料科技有限公司 | A kind of preparation method of high-strength flooring laminate material |
| 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 |
| CN110591459A (en) * | 2019-10-08 | 2019-12-20 | 徐州鑫博金属制品有限公司 | Preparation method of aluminum alloy anticorrosive material |
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Address after: Suzhou City, Jiangsu Province, Suzhou Industrial Park 215123 Xinghu Street No. 328 international science and Technology Park B4-503 Patentee after: JIANGSU NADN TECHNOLOGY CO., LTD. Address before: Suzhou City, Jiangsu Province, Suzhou Industrial Park 215123 Xinghu Street No. 328 international science and Technology Park B4-503 Patentee before: Suzhou Supernano-textile Tech. Co., Ltd. |