CN102531037A - Chemical preparation method of nanoscale zinc oxide powder - Google Patents
Chemical preparation method of nanoscale zinc oxide powder Download PDFInfo
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- CN102531037A CN102531037A CN2012100123996A CN201210012399A CN102531037A CN 102531037 A CN102531037 A CN 102531037A CN 2012100123996 A CN2012100123996 A CN 2012100123996A CN 201210012399 A CN201210012399 A CN 201210012399A CN 102531037 A CN102531037 A CN 102531037A
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Abstract
The invention discloses a chemical preparation method of nanoscale zinc oxide powder, and the method comprises the following steps of: (1) in a stirring container, adjusting the concentration of a zinc salt solution to be 0.5-2.0mol/L, heating to 20-80 DEG C, adding an alkali solution to cause the pH of the zinc salt solution to be 11-12, and reacting at the temperature of 20-80 DEG C for 1-2 hours, thus obtaining a zinc hydroxide precipitate and a zinc oxide precipitate; (2) filtering and separating to obtain a solid mixture of zinc hydroxide and zinc oxide, and washing the mixture of solid zinc hydroxide and zinc oxide until washing liquid contains no zinc salt anion; and (3) placing the mixture obtained by the step (2) into a flash dryer to be subjected to flashing and drying at the temperature of 150-250 DEG C, and smashing to obtain 96-99% nanoscale zinc oxide powder, wherein the grain diameter of the powder is 50-100nm, and the whiteness of the powder is higher than eighth level.
Description
Technical field
The present invention relates to a kind of preparation of nano-scale oxidized zinc powder, be specifically related to the chemical prepn process of nano-scale oxidized zinc powder.
Background technology
Nano-scale oxidized zinc powder is mainly used in fields such as rubber tyre, catalyzer, pottery, uvioresistant; Particularly be the important materials of making the high-speed abrasion-proof tire, and the sector market capacity is huge, has very much exploitation to be worth in the rubber tyre field.The method for preparing nanometer Zinc oxide powder is divided into dry method and wet method, and dry method mainly is to generate zinc fume through evaporation zinc ingot metal or zinc ore under certain condition, and aerating oxygen generates zinc oxide again, obtains finished product through capturing.Also have high temperature pyrolytic cracking (HTP), prepare zn cpds, the zn cpds decomposition is obtained zinc oxide nano-powder through solid phase or liquid-phase chemical reaction.Wet method is synthetic to be had multiplely, mainly is to utilize precipitation heat solution and hydrothermal synthesis method.The precipitation heat solution is in zinc solution, to add carbonate or urea etc. to be settled out zinc subcarbonate, and the decomposition of heating zinc subcarbonate obtains Zinc oxide powder or utilizes ammonia process production; Hydrothermal synthesis method is to be presoma with the zinc hydroxide, under certain pressure and temperature, obtains through the dehydration crystallization, needs HTHP to accomplish.Know that from above-mentioned all there are the relatively harsher situation of reaction conditions in dry method and wet method, energy consumption is high, is unfavorable for suitability for industrialized production.
Summary of the invention
The chemical prepn process that the purpose of this invention is to provide a kind of nano-scale oxidized zinc powder is to obtain to be easy to suitability for industrialized production, operational path cheaply.
The present invention realizes through following technical scheme:
A kind of chemical prepn process of nano-scale oxidized zinc powder comprises the following steps:
(1) in the container of stirring is arranged; Zinc solution concentration is adjusted into 0.5-2.0mol ∕ L, is heated to 20-80 ℃, it is 11-12 that the adding alkaline solution makes the PH of zinc solution; And after reacting 1-2 hour under the 20-80 ℃ of condition, obtain the deposition of zinc hydroxide and zinc oxide;
In reaction process, needing to keep PH is 11-12, as is lower than this value, then need add the alkali adjustment.
(2) filtering separation obtains solid hydrogen zinc oxide and zinc oxide mixture, and zinc hydroxide and zinc oxide mixture are washed, and in washings, does not contain till the zinc salt negatively charged ion; (said zinc salt negatively charged ion is sulfate ion, nitrate ion or green ion) is in the solid hydrogen zinc oxide and zinc oxide mixture that obtains;
(3) mixture that step (2) is obtained is put into flash dryer, and flash distillation in 150-250 ℃, oven dry, pulverizing obtain the nano-scale oxidized zinc powder of 96-99 ﹪, and the powder granule diameter is 50-100nm, and powder whiteness is more than 8 grades.Zinc hydroxide almost all is converted into zinc oxide in the high temperature flash distillation.
The further improvement project of the present invention is, said zinc salt is one or more mixtures (can arbitrary proportion mix) in zinc sulfate, zinc nitrate or the zinc chloride.
The present invention further improvement project is, said alkaline solution is sodium hydroxide or potassium hydroxide solution or both mixed solutions (can arbitrary proportion mix), and its concentration is 25-50 ﹪.
Particulate size and percent crystallinity improve with the raising of temperature in time in the reaction process.
The present invention compared with prior art has the following advantages:
(1) nano-scale oxidized zinc powder of preparation is a single crystal structure, and structure is circular entity; Purity high (high energy reach 99%), grain diameter little (single particle TEM is at 50 ~ 100 nm).Temperature of reaction is low, and the reaction times is short, and powder whiteness is more than 8 grades.
(2) nano-scale oxidized zinc powder of preparation has good active, is specially adapted to the rubber tyre industry.
(3) this operational path material is cheap and easy to get, production technique is simple, working condition is gentle, do not produce pollution, easy to operate, be easy to realize suitability for industrialized production.
Description of drawings
Fig. 1 is the transmission electron micrograph synoptic diagram of nano-scale oxidized zinc powder.Show its particle size about 75nm, be shaped as irregular spherical.
Fig. 2 is the X-ray diffraction spectrum diagram intention of nano-scale oxidized zinc powder.Do not find the diffraction peak of other impurity in the spectrogram.
Embodiment
Embodiment 1
(1) solution of zinc sulfate of preparation 1.5mo/L and 30% sodium hydroxide solution; Under 70 ℃ of water bath condition; Sodium hydroxide solution with 30% slowly adds in the solution of zinc sulfate; Making solution PH is 11 (PH is not less than 11 in the reaction process), 400 rev/mins of stirring velocitys, and obtain the deposition of zinc hydroxide and zinc oxide after 1 hour 70 ℃ of reactions;
(2) filtering separation obtains solid hydrogen zinc oxide and zinc oxide mixture, with the solid mixture that obtains with distilled water wash 7 ~ 8 times, in filtered liq till the sulfate radical-free ion;
(3) solid mixture that step (2) is obtained is put into flash dryer, and flash distillation in 200 ℃, oven dry, pulverizing obtain the nano-scale oxidized zinc powder of 97 ﹪, and the powder granule diameter is 75nm, and powder whiteness is 8.5 grades.
Embodiment 2
(1) (both proportionings can be arbitrarily for zinc sulfate, the zinc chloride mixing solutions of preparation 1.0mo/L; Be 1:1 in the present embodiment) and 35% potassium hydroxide solution, under 60 ℃ of water bath condition; Potassium hydroxide solution with 35% slowly adds in zinc sulfate, the zinc chloride mixing solutions; Making solution PH is 12,400 rev/mins of stirring velocitys, and obtain the deposition of zinc hydroxide and zinc oxide after 1 hour 60 ℃ of reactions;
(2) filtering separation obtains solid hydrogen zinc oxide and zinc oxide mixture, with the solid mixture that obtains with distilled water wash 7 ~ 8 times, in filtered liq till the sulfate radical-free ion;
(3) solid mixture that step (2) is obtained is put into flash dryer, and flash distillation in 180 ℃, oven dry, pulverizing obtain the nano-scale oxidized zinc powder of 95 ﹪, and the powder granule diameter is 75nm, and powder whiteness is 8.5 grades.
Embodiment 3
(1) zinc nitrate, the zinc chloride mixing solutions (both proportioning 1:1) of preparation 2.0mo/L; With 35% sodium hydroxide, potassium hydroxide solution; Under 80 ℃ of water bath condition, the sodium hydroxide with 35%, potassium hydroxide solution slowly add in zinc nitrate, the liquor zinci chloridi, and making solution PH is 12; 400 rev/mins of stirring velocitys, and obtain the deposition of zinc hydroxide and zinc oxide after 1.5 hours 80 ℃ of reactions;
(2) filtering separation obtains solid hydrogen zinc oxide and zinc oxide mixture, with the solid mixture that obtains with distilled water wash 7 ~ 8 times, in filtered liq till the sulfate radical-free ion;
(3) solid mixture that step (2) is obtained is put into flash dryer, and flash distillation in 250 ℃, oven dry, pulverizing obtain the nano-scale oxidized zinc powder of 99 ﹪, and the powder granule diameter is 95nm, and powder whiteness is 8.5 grades.
Claims (3)
1. the chemical prepn process of a nano-scale oxidized zinc powder is characterized in that comprising the following steps:
(1) zinc solution concentration is adjusted into 0.5-2.0mol ∕ L, is heated to 20-80 ℃, it is 11-12 that the adding alkaline solution makes the PH of zinc solution, and after 1-2 hour, obtains the deposition of zinc hydroxide and zinc oxide in reaction under the 20-80 ℃ of condition;
(2) filtering separation obtains solid hydrogen zinc oxide and zinc oxide mixture, and zinc hydroxide and zinc oxide mixture are washed, and in washings, does not contain till the zinc salt negatively charged ion;
(3) solid mixture that step (2) is obtained is put into flash dryer, and flash distillation in 150-250 ℃, oven dry, pulverizing obtain the nano-scale oxidized zinc powder of 96-99 ﹪, and the powder granule diameter is 50-100nm, and powder whiteness is more than 8 grades.
2. the chemical prepn process of a kind of nano-scale oxidized zinc powder as claimed in claim 1, it is characterized in that: said zinc salt is one or more mixtures in zinc sulfate, zinc nitrate or the zinc chloride.
3. the chemical prepn process of a kind of nano-scale oxidized zinc powder as claimed in claim 1, it is characterized in that: said alkaline solution is sodium hydroxide or potassium hydroxide solution or both mixed solutions, and its concentration is 25-50 ﹪.
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
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CN104085913A (en) * | 2014-06-11 | 2014-10-08 | 南通昊友食品添加剂有限公司 | Production method of food grade high-purity zinc oxide |
CN104276593A (en) * | 2014-11-03 | 2015-01-14 | 苏州市泽镁新材料科技有限公司 | Method for preparing nano zinc carbonate |
CN104445362A (en) * | 2014-11-03 | 2015-03-25 | 苏州市泽镁新材料科技有限公司 | Preparation method of nano zinc carbonate |
CN104445366A (en) * | 2014-11-10 | 2015-03-25 | 西北大学 | Method for synthesizing spindlelike ZnO nanomaterial by adopting microwave-assisted extraction process |
CN106145172A (en) * | 2016-06-29 | 2016-11-23 | 青岛惠城环保科技股份有限公司 | A kind of water purification agent and preparation method thereof |
CN106517302A (en) * | 2016-10-29 | 2017-03-22 | 乐山凯亚达光电科技有限公司 | Preparation method of nanoscale zinc oxide crystals |
CN106986371A (en) * | 2017-04-07 | 2017-07-28 | 魏周宏 | A kind of method for preparing nanometer Zinc oxide powder |
CN107381617A (en) * | 2017-02-23 | 2017-11-24 | 江西金泰化工股份有限公司 | A kind of isooctyl acid produces catalyst recycling technique |
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CN101514480A (en) * | 2009-02-25 | 2009-08-26 | 太原理工大学 | Method for preparing white needle-shaped six-edge mono-crystalline nano-zinc oxide |
CN101613121A (en) * | 2009-07-16 | 2009-12-30 | 聊城大学 | A kind of preparation method of ellipsoid-shaped zinc oxide |
CN101823758A (en) * | 2010-05-14 | 2010-09-08 | 常宁市湘江化工有限责任公司 | Novel method for producing nanometer grade zinc carbonate and zinc oxide |
US20110300061A1 (en) * | 2010-06-04 | 2011-12-08 | Indian Institute Of Technology Bombay | Polymer-mediated synthesis of ZnO nanostructures |
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CN101514480A (en) * | 2009-02-25 | 2009-08-26 | 太原理工大学 | Method for preparing white needle-shaped six-edge mono-crystalline nano-zinc oxide |
CN101613121A (en) * | 2009-07-16 | 2009-12-30 | 聊城大学 | A kind of preparation method of ellipsoid-shaped zinc oxide |
CN101823758A (en) * | 2010-05-14 | 2010-09-08 | 常宁市湘江化工有限责任公司 | Novel method for producing nanometer grade zinc carbonate and zinc oxide |
US20110300061A1 (en) * | 2010-06-04 | 2011-12-08 | Indian Institute Of Technology Bombay | Polymer-mediated synthesis of ZnO nanostructures |
Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104085913A (en) * | 2014-06-11 | 2014-10-08 | 南通昊友食品添加剂有限公司 | Production method of food grade high-purity zinc oxide |
CN104276593A (en) * | 2014-11-03 | 2015-01-14 | 苏州市泽镁新材料科技有限公司 | Method for preparing nano zinc carbonate |
CN104445362A (en) * | 2014-11-03 | 2015-03-25 | 苏州市泽镁新材料科技有限公司 | Preparation method of nano zinc carbonate |
CN104445366A (en) * | 2014-11-10 | 2015-03-25 | 西北大学 | Method for synthesizing spindlelike ZnO nanomaterial by adopting microwave-assisted extraction process |
CN104445366B (en) * | 2014-11-10 | 2016-05-04 | 西北大学 | The method of the synthetic spindle flower-like structure ZnO nano material of a kind of microwave abstracting |
CN106145172A (en) * | 2016-06-29 | 2016-11-23 | 青岛惠城环保科技股份有限公司 | A kind of water purification agent and preparation method thereof |
CN106517302A (en) * | 2016-10-29 | 2017-03-22 | 乐山凯亚达光电科技有限公司 | Preparation method of nanoscale zinc oxide crystals |
CN107381617A (en) * | 2017-02-23 | 2017-11-24 | 江西金泰化工股份有限公司 | A kind of isooctyl acid produces catalyst recycling technique |
CN106986371A (en) * | 2017-04-07 | 2017-07-28 | 魏周宏 | A kind of method for preparing nanometer Zinc oxide powder |
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Application publication date: 20120704 |