CN1533985A - Preparation method of nano-grade zinc oxide powder - Google Patents
Preparation method of nano-grade zinc oxide powder Download PDFInfo
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- CN1533985A CN1533985A CNA031160794A CN03116079A CN1533985A CN 1533985 A CN1533985 A CN 1533985A CN A031160794 A CNA031160794 A CN A031160794A CN 03116079 A CN03116079 A CN 03116079A CN 1533985 A CN1533985 A CN 1533985A
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Abstract
A zinc oxide nanoparticles is prepared from zinc salt solution and carbonate solution through adding disperser to zinc salt solution, high-speed stirring while dropping carbonate solution for hydrothermal synthesis reaction to obtain suspension containing zinc carbonate, filtering, washing filtered cake, drying calcining and pulverizing. Its advantage is uniform and small granularity.
Description
Technical Field
The invention relates to a preparation method of a superfine inorganic material, in particular to a preparation method of nano-scale zinc oxide powder with an ultraviolet shielding function.
Background
The ultraviolet rays can be divided into three sections of UVC (200-280 nm), UVB (280-320 nm) and UVA (320-400 nm) according to the wavelength. Wherein, UVC segment is absorbed by ozone layer, which is not easy to hurt human body, but in recent years, the damage of ozone layer means that the content of UVC in sunlight is increased continuously, which endangers the dayThe benefit is obvious; the UVB segment and the UVA segment can cause skin erythema, inflammation, cancer, skin aging and connective tissue canceration, and seriously affect the health of people; in recent years, research and development of sunscreen agents such as nano ZnO and TiO has been actively conducted in countries such as America, Japan, Germany, Australia, and the like2And iron oxide red, are preferred because they are non-toxic, odorless, non-irritating to the skin, non-decomposing, non-deteriorating, and thermally stable. Among them, nano ZnO is widely used because it is white, can be simply colored, is cheap, has a strong ability to absorb ultraviolet rays, and has a shielding effect on UVA, UVB and UVC.
There are various methods available for preparing nano zinc oxide. Chinese patent CN1166454A discloses a method for preparing superfine zinc oxide by liquid phase nucleation growth step by step. Firstly, a precursor coated with zinc hydroxide colloidal particles is formed in a zinc salt solution, and nucleation and growth of zinc oxide are carried out step by utilizing different decomposition temperatures of zinc hydroxide and an outer coating substance, so as to prepare the nano zinc oxide with the particle size of 25-100 nm. The method has multiple steps and long time. JP02311314 discloses a method for preparing ultrafine zinc oxide. Introducing hydrogen sulfide into a solution of zinc and ammonia acetate, separating and dispersing the obtained precipitate into a non-aqueous solvent, degassing at 200-400 ℃, and then carrying out heat treatment at 500-800 ℃ to obtain zinc oxide powder. Japanese patent JP63288913 discloses a method for preparing ultrafine zinc oxide. The method comprises the steps of introducing carbon dioxide into zinc oxide slurry, reacting to obtain nano zinc oxide, and performing heat treatment at 250-1000 ℃ to prepare high-purity zinc oxide. Chinese patent (application No. 97108438.6) discloses a method for preparing nano zinc oxide by a uniform precipitation method. The method uses urea as a uniform precipitator, and hydrolyzes at 122-126 ℃ to prepare the nano zinc oxide. The hydrolysis temperature is high, the hydrolysis needs to be carried out in a high-pressure reaction kettle, the urea is easy to polymerize, the production control difficulty is high, the yield is low, and the powder is easy to agglomerate. The Chinese patent (application No. 00129459.8) proposes that zinc hydroxide precipitate is prepared, template agents such as polyethylene glycol are added, and nano zinc oxide powder is prepared through hydrothermal or solvent heat treatment, and the method has high cost. Japanese patent JP29339/99 proposes that metal zinc vapor is oxidized in an atmosphere containing oxygen and water vapor and inert gas is used as carrier and protective gas to prepare nano zinc oxide. U.S. Pat. No. 4, 09, 266202 proposes the preparation of nano zinc oxide by laser pyrolysis using zinc salt aerosol. These methods have high cost, difficult control of process production conditions, and difficult industrial production.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide the preparation method of the nano-grade zinc oxide powder, which has the advantages of simple process, low cost, convenient operation, uniform and controllable particle size and stable performance.
The purpose of the invention can be realized by the following technical scheme: a process for preparing nano-class zinc oxide powder includes such steps as adding disperser to zinc salt solution, high-speed stirring while dropping carbonate solution for hydrothermal synthesis reaction to obtain suspension containing zinc carbonate, filtering, washing filter cake, drying, calcining and pulverizing.
The concentration of the zinc salt solution is 1-2 mol/L, and the zinc salt of the zinc salt solution is selected from one or more of anhydrous zinc sulfate, zinc sulfate containing crystal water, zinc chloride, zinc nitrate and zinc acetate.
The concentration of the carbonate solution is 1-3 mol/L, and the carbonate of the carbonate solution is selected from one or more of sodium carbonate, sodium bicarbonate, ammonium carbonate, ammonium bicarbonate, potassium carbonate and potassium bicarbonate.
The dispersing agent is selected from one or more of sodium laurate, sodium stearate, sodium dodecyl sulfate, sodium hexametaphosphate, polyethylene glycol, tween, polyoxyethylene ether and triethanolamine.
The addition amount of the dispersing agent is 0.06-0.12% by mol of zinc oxide.
The molar ratio of the solute in the reaction of the zinc salt solution and the carbonate solution is 1-2: 1.
The rotating speed of the high-speed stirrer is 2000-5000 rpm when the zinc salt solution and the carbonate solution react.
The reaction temperature of the precursor hydro-thermal synthesis reaction is 20-100 ℃, and the reaction time is 0.5-3 hours.
The drying temperature of the zinc carbonate is 95-150 ℃, the calcining temperature is 250-500 ℃, and the calcining time is 0.5-3 hours.
The method of the invention has the main chemical reaction formula as follows:
the method has the advantages of simple process, low cost, convenient operation and uniform and controllable particle size, and the nano zinc oxide powder prepared by the method has the pH of 6.5-7.5, the zinc oxide content of more than 99 percent, the moisture content of less than 0.5 percent, the ignition loss of less than 1.0 percent, the screened substance of less than 0.01 percent and the specific surface area of 60-80 m2The particle size is 10-30 nm, and the powder performance is stable. The invention overcomes the defects of easy agglomeration, uneven particle size distribution, difficult control of particle size and the like of nano zinc oxide particles in the traditional method, and has strong ultraviolet shielding capability and visible light transmission capability.
Detailed Description
Example 1
0.06 percent of polyethylene glycol (calculated by the mole number of zinc oxide) is added into the zinc sulfate solution with the concentration of 1mol/L, and the mixture is uniformly dispersed. Heating to 60 deg.C, adding 1.5mol/L ammonium carbonate solution into zinc sulfate solution at constant speed of 12ml/min (molar ratio of ammonium carbonate to zinc sulfate is 1: 1.14) under high speed stirring at 5000rpm, reacting at constant temperature for 1.0 hr, filtering the obtained suspension,washing the filter cake until the filtrate is 0.1% BaCl2Solution testingNo white turbidity, i.e. no SO in the filtrate4 2-、NH4 +And (3) waiting for impurity ions, drying the filter cake at 105 ℃, calcining for 2.0 hours at 300 ℃, and crushing to prepare the nano zinc oxide powder without agglomeration and with uniform granularity. The obtained powder has the particle size of about 10-30 nm, the crystal form is a hexagonal crystal form, the pH value is 6.5-7.5, the zinc oxide is more than 99%, and the specific surface area is 70-90 m2(ii) in terms of/g. The nano zinc oxide has a strong shielding effect on ultraviolet rays with a wave band of 200-400 nm, the ultraviolet-resistant coverage frequency band is wide, the nano zinc oxide has almost no shielding capability on visible light, and the visible light wave with the wave band of 420-760 nm is basically and completely transmitted.
Example 2
0.06 percent of polyethylene glycol (calculated by the mole number of zinc oxide) is added into the zinc sulfate solution with the concentration of 2mol/L, and the mixture is uniformly dispersed. Heating to 60 ℃, stirring at high speed of 5000rpm and adding carbonic acid with the concentration of 3mol/LAdding the ammonium solution into the zinc sulfate solution at a constant speed of 12ml/min (the molar ratio of ammonium carbonate to zinc sulfate is 1: 1.14), and reacting for 2.0 hours at constant temperature; the resulting suspension was filtered and the filter cake was washed until the filtrate was washed with 0.1% BaCl2Checking the solution to have no white turbidity, drying the filter cake at 105 ℃, calcining at 300 ℃ for 2.0 hours, and crushing to obtain the nano zinc oxide powder. The obtained powder has the particle size of about 30-50 nm, a hexagonal crystal form, the pH value of 6.5-7.5, the zinc oxide content of more than 99 percent and the specific surface area of 50-70 m2/g。
Example 3
0.06 percent of polyethylene glycol (calculated by the mole number of zinc oxide) is added into the zinc sulfate solution with the concentration of 1mol/L, and the mixture is uniformly dispersed. Heating to 60 ℃, adding an ammonium carbonate solution with the concentration of 1.5mol/L into a zinc sulfate solution at a constant speed of 12ml/min under the high-speed stirring of 5000rpm (the molar ratio of the ammonium carbonate to the zinc sulfate is 1: 1.14), and reacting for 1.0 hour at constant temperature; the resulting suspension was filtered and the filter cake was washed until the filtrate was washed with 0.1% BaCl2Checking the solution to have no white turbidity, drying the filter cake at 105 ℃, calcining at 600 ℃ for 2.0 hours, and crushing to obtain the nano zinc oxide powder. The obtained powder has the particle size of 90-120 nm, a hexagonal crystal form, the pH value of 6.5-7.5, the zinc oxide content of more than 99 percent and the specific surface area of 30-50 m2(ii) in terms of/g. In this case, a sintering phenomenon occurs, and the zinc oxide particles rapidly increase in particle size and have a strong shielding effect against ultraviolet rays, but the visible light transmittance is significantly reduced.
Example 4
Heating the zinc sulfate solution with the concentration of 1mol/L to 60 ℃, adding the ammonium carbonate solution with the concentration of 1.5mol/L into the zinc sulfate solution at a constant speed of 24ml/min under the condition of high-speed stirring at 5000rpm (the molar ratio of the ammonium carbonate to the zinc sulfate is 1: 1.14), and reacting for 2.0 hours at constant temperature; the resulting suspension was filtered and the filter cake was washed until the filtrate was washed with 0.1% BaCl2Checking the solution to have no white turbidity, drying the filter cake at 105 ℃, calcining at 300 ℃ for 2.0 hours, and crushing to obtain the nano zinc oxide powder. The obtained powder has the particle size of about 50-70 nm, a hexagonal crystal form, the pH value of 6.5-7.5, the zinc oxide content of more than 99 percent and the specific surface area of 60-80 m2(ii) in terms of/g. No dispersant is added, the agglomeration phenomenon of zinc oxide particles is serious, and the particle size is increased.
Example 5
Adding 0.12% (based on the mol number of zinc oxide) of sodium laurate into the zinc chloride solution with the concentration of 2mol/L, and uniformly dispersing. Heating to 100 ℃, adding a sodium carbonate solution with the concentration of 1mol/L into a zinc chloride solution at a constant speed of 12ml/min under the high-speed stirring of 3500rpm (the molar ratio of sodium carbonate to zinc chloride is 1: 2), and reacting for 0.5 hour at constant temperature; the resulting suspension was filtered and the filter cake was washed until the filtrate was washed with 0.1% BaCl2Checking the solution to have no white turbidity, drying the filter cake at 150 deg.C, and calcining at 500 deg.C for 0.5 hrThen crushing to obtain the nano zinc oxide powder. The obtained powder has the particle size of about 20-40 nm, a hexagonal crystal form, the pH value of 6.5-7.5, the zinc oxide content of more than 99 percent and the specific surface area of 60-80 m2/g。
Example 6
0.12 percent (calculated by the mol number of zinc oxide) of sodium stearate or sodium dodecyl sulfate (or both) is added into a zinc nitrate solution with the concentration of 1mol/L, and the mixture is uniformly dispersed. Heating to 30 deg.C, adding 3mol/L sodium bicarbonate solution into zinc nitrate solution at constant speed of 12ml/min (molar ratio of sodium bicarbonate to zinc nitrate is 1: 1) under high speed stirring at 2000rpm, and reacting at constant temperatureThe reaction time is 2 hours; the resulting suspension was filtered and the filter cake was washed until the filtrate was washed with 0.1% BaCl2Checking the solution to have no white turbidity, drying the filter cake at 95 ℃, calcining at 250 ℃ for 3 hours, and crushing to obtain the nano zinc oxide powder. The obtained powder has the particle size of about 40-60 nm, a hexagonal crystal form, the pH value of 6.5-7.5, the zinc oxide content of more than 99 percent and the specific surface area of 30-50 m2/g。
Example 7
0.1 percent (calculated by the mol number of zinc oxide) of polyoxyethylene ether or triethanolammonium is added into a zinc acetate solution with the concentration of 2mol/L and is dispersed evenly. Heating to 50 ℃, adding a potassium carbonate solution with the concentration of 2mol/L into a zinc acetate solution at a constant speed of 12ml/min under the high-speed stirring of 2000rpm (the molar ratio of potassium carbonate to zinc acetate is 1: 1), and reacting for 2 hours at constant temperature; the resulting suspension was filtered and the filter cake was washed until the filtrate was washed with 0.1% BaCl2Checking the solution to have no white turbidity, drying the filter cake at 100 ℃, calcining at 400 ℃ for 1 hour, and crushing to obtain the nano zinc oxide powder. The obtained powder has the particle size of about 40-60 nm, a hexagonal crystal form, the pH value of 6.5-7.5, the zinc oxide content of more than 99 percent and the specific surface area of 30-50 m2/g。
Claims (9)
1. A process for preparing nano-class zinc oxide powder includes such steps as adding disperser to zinc salt solution, high-speed stirring while dropping carbonate solution for hydrothermal synthesis reaction to obtain suspension containing zinc carbonate, filtering, washing filter cake, drying, calcining and pulverizing.
2. The method for preparing nano-scale zinc oxide powder according to claim 1, wherein the concentration of the zinc salt solution is 1-2 mol/L, and the zinc salt of the zinc salt solution is one or more selected from anhydrous zinc sulfate, zinc sulfate containing crystal water, zinc chloride, zinc nitrate and zinc acetate.
3. The method for preparing nano-scale zinc oxide powder according to claim 1, wherein the concentration of the carbonate solution is 1-3 mol/L, and the carbonate of the carbonate solution is selected from one or more of sodium carbonate, sodium bicarbonate, ammonium carbonate, ammonium bicarbonate, potassium carbonate and potassium bicarbonate.
4. The method of claim 1, wherein the dispersing agent is one or more selected from the group consisting of sodium laurate, sodium stearate, sodium lauryl sulfate, sodium hexametaphosphate, polyethylene glycol, tween, polyoxyethylene ether, and triethanolammonium.
5. The method of claim 1, wherein the dispersant is added in an amount of 0.06-0.12 mol% based on the zinc oxide.
6. The method for preparing nano-scale zinc oxide powder according to claim 1, wherein the molar ratio of the solute in the reaction of the zinc salt solution and the carbonate solution is 1-2: 1.
7. The method for preparing nano-scale zinc oxide powder according to claim 1, wherein the rotation speed of the high-speed stirrer is 2000-5000 rpm when the zinc salt solution and the carbonate solution react.
8. The method for preparing nano-scale zinc oxide powder according to claim 1, wherein the reaction temperature of the precursor hydrothermal synthesis reaction is 20-100 ℃ and the reaction time is 0.5-3 hours.
9. The method of claim 1, wherein the drying temperature of zinc carbonate is 95-150 ℃, the calcining temperature is 250-500 ℃, and the calcining time is 0.5-3 hours.
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| CN1308244C (en) * | 2005-04-26 | 2007-04-04 | 华中师范大学 | Nano zine oxide with excitating light strength and frequency tuning fluorescent frequency and it preparation |
| CN100391848C (en) * | 2006-03-02 | 2008-06-04 | 浙江大学 | Process for preparing zinc oxide nano stick |
| CN102241413A (en) * | 2010-05-10 | 2011-11-16 | 东莞市同舟化工有限公司 | Method for preparing nano zinc oxide |
| CN104118898A (en) * | 2014-08-14 | 2014-10-29 | 安徽工业大学 | Preparation method of zinc carbonate nanoneedle |
| CN104326504A (en) * | 2014-10-13 | 2015-02-04 | 李大枝 | Preparation method for urchin-like nanometer zinc oxide |
| CN105236467A (en) * | 2014-08-01 | 2016-01-13 | 阜阳师范学院 | Mass preparation process of nano-grade zinc oxide, and application of nano-grade zinc oxide |
| CN105566681A (en) * | 2015-12-22 | 2016-05-11 | 成都新柯力化工科技有限公司 | Auxiliary capable of improving printing performance of composite ivory board and preparation method thereof |
| CN106006713A (en) * | 2016-07-07 | 2016-10-12 | 安徽省含山县锦华氧化锌厂 | Preparation process of active nano-zinc oxide |
| CN106115766A (en) * | 2014-11-25 | 2016-11-16 | 重庆文理学院 | A kind of preparation method of the nano material of efficient degradation dyestuff |
| CN107140678A (en) * | 2017-07-05 | 2017-09-08 | 四川康泰祥生物科技有限公司 | A kind of wet process technique of high-purity feed grade high-efficiency multiple zinc oxide |
| CN108440855A (en) * | 2018-03-29 | 2018-08-24 | 青岛元汇丰企业管理咨询服务有限公司 | A kind of UV resistance culture dish and preparation method thereof |
| CN110876689A (en) * | 2019-09-30 | 2020-03-13 | 成都理工大学 | Calcined kaolin loaded nano ZnO composite anti-ultraviolet agent and preparation technology thereof |
| CN111280369A (en) * | 2020-04-14 | 2020-06-16 | 上海邦成生物工程有限公司 | Plant extract-impregnated nano microporous zinc oxide solid and preparation method thereof |
| CN111747442A (en) * | 2020-08-05 | 2020-10-09 | 株洲安特新材料科技有限公司 | Method for producing active zinc oxide by wet process |
| CN112320836A (en) * | 2020-10-16 | 2021-02-05 | 杭州松鸿科技有限公司 | Zinc oxide production process |
| CN114524454A (en) * | 2022-03-30 | 2022-05-24 | 广州天赐高新材料股份有限公司 | Lipopeptide modified nano zinc oxide and synthesis method and application thereof |
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| CN117550645A (en) * | 2023-11-02 | 2024-02-13 | 南通三优佳磁业有限公司 | Preparation process and application of manganese zinc ferrite superfine powder |
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2003
- 2003-03-31 CN CNA031160794A patent/CN1533985A/en active Pending
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| CN1308244C (en) * | 2005-04-26 | 2007-04-04 | 华中师范大学 | Nano zine oxide with excitating light strength and frequency tuning fluorescent frequency and it preparation |
| CN100391848C (en) * | 2006-03-02 | 2008-06-04 | 浙江大学 | Process for preparing zinc oxide nano stick |
| CN102241413A (en) * | 2010-05-10 | 2011-11-16 | 东莞市同舟化工有限公司 | Method for preparing nano zinc oxide |
| CN102241413B (en) * | 2010-05-10 | 2013-07-17 | 东莞市同舟化工有限公司 | Method for preparing nano zinc oxide |
| CN105236467A (en) * | 2014-08-01 | 2016-01-13 | 阜阳师范学院 | Mass preparation process of nano-grade zinc oxide, and application of nano-grade zinc oxide |
| CN104118898A (en) * | 2014-08-14 | 2014-10-29 | 安徽工业大学 | Preparation method of zinc carbonate nanoneedle |
| CN104326504A (en) * | 2014-10-13 | 2015-02-04 | 李大枝 | Preparation method for urchin-like nanometer zinc oxide |
| CN106115766B (en) * | 2014-11-25 | 2017-08-29 | 重庆文理学院 | A kind of preparation method of the nano material of efficient degradation dyestuff |
| CN106115766A (en) * | 2014-11-25 | 2016-11-16 | 重庆文理学院 | A kind of preparation method of the nano material of efficient degradation dyestuff |
| CN105566681A (en) * | 2015-12-22 | 2016-05-11 | 成都新柯力化工科技有限公司 | Auxiliary capable of improving printing performance of composite ivory board and preparation method thereof |
| CN105566681B (en) * | 2015-12-22 | 2018-03-16 | 贵州金马包装材料有限公司 | A kind of auxiliary agent for lifting compound art post paperboard printing performance and preparation method thereof |
| CN106006713A (en) * | 2016-07-07 | 2016-10-12 | 安徽省含山县锦华氧化锌厂 | Preparation process of active nano-zinc oxide |
| CN107140678A (en) * | 2017-07-05 | 2017-09-08 | 四川康泰祥生物科技有限公司 | A kind of wet process technique of high-purity feed grade high-efficiency multiple zinc oxide |
| CN108440855A (en) * | 2018-03-29 | 2018-08-24 | 青岛元汇丰企业管理咨询服务有限公司 | A kind of UV resistance culture dish and preparation method thereof |
| CN110876689A (en) * | 2019-09-30 | 2020-03-13 | 成都理工大学 | Calcined kaolin loaded nano ZnO composite anti-ultraviolet agent and preparation technology thereof |
| CN111280369A (en) * | 2020-04-14 | 2020-06-16 | 上海邦成生物工程有限公司 | Plant extract-impregnated nano microporous zinc oxide solid and preparation method thereof |
| CN111280369B (en) * | 2020-04-14 | 2023-01-03 | 上海邦成生物工程有限公司 | Plant extract-impregnated nano microporous zinc oxide solid and preparation method thereof |
| CN111747442A (en) * | 2020-08-05 | 2020-10-09 | 株洲安特新材料科技有限公司 | Method for producing active zinc oxide by wet process |
| CN112320836A (en) * | 2020-10-16 | 2021-02-05 | 杭州松鸿科技有限公司 | Zinc oxide production process |
| CN114524454A (en) * | 2022-03-30 | 2022-05-24 | 广州天赐高新材料股份有限公司 | Lipopeptide modified nano zinc oxide and synthesis method and application thereof |
| CN114524454B (en) * | 2022-03-30 | 2023-11-28 | 广州天赐高新材料股份有限公司 | Lipopeptide modified nano zinc oxide and synthetic method and application thereof |
| CN115818708A (en) * | 2022-12-15 | 2023-03-21 | 常州纳欧新材料科技有限公司 | Preparation method of titanium-containing flaky zinc oxide composite physical sun-screening agent |
| CN117550645A (en) * | 2023-11-02 | 2024-02-13 | 南通三优佳磁业有限公司 | Preparation process and application of manganese zinc ferrite superfine powder |
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