CN105060324A - Ultrasonic synthesis method of nano-alumina and application thereof - Google Patents

Ultrasonic synthesis method of nano-alumina and application thereof Download PDF

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CN105060324A
CN105060324A CN201510459161.1A CN201510459161A CN105060324A CN 105060324 A CN105060324 A CN 105060324A CN 201510459161 A CN201510459161 A CN 201510459161A CN 105060324 A CN105060324 A CN 105060324A
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aluminium oxide
nano aluminium
ultrasonic
synthetic method
hco
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CN105060324B (en
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程敬泉
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Hengshui University
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Abstract

The invention discloses an ultrasonic synthesis method of nano-alumina. The method includes: taking Al(NO3)3 as the raw material, using NH4HCO3 as the precipitating agent, conducting ultrasonic treatment and then performing calcination to prepare a precursor, thus obtaining nano-alumina. According to the ultrasonic synthesis method of nano-alumina provided by the invention, the ultrasonic parameters are controlled to affect the shape, performance and other characteristics of the synthesized nano-alumina. The method promotes the further development of ultrasonic chemical preaparation of nano-materials, and injects new vitality to nanotechnologies.

Description

The ultrasonic synthetic method of nano aluminium oxide and application thereof
Technical field
The invention belongs to chemical material field, be specifically related to a kind of ultrasonic synthetic method and application thereof of nano aluminium oxide.
Background technology
At present, the technology of preparing of domestic and international nano aluminium oxide can be divided into solid phase method, vapor phase process and liquid phase method three major types.Solid phase method is simple to operate, but the particle diameter generating particle is difficult to control; Vapor phase process facility investment is large, and complicated operation, thus the application of liquid phase method is more extensive.In liquid phase method, the precipitator method many employings inorganic raw material, cost is low, and production unit and technique are simple, and particle purity is high, and granularity is little, narrow diameter distribution, is therefore that one has emulative method.
In recent years, the research of ultrasonic technique in novel material synthesis is very active, acoustic cavitation (acousticcavitation) process is a kind of highly effective technology preparing nano material, and the special physics that acoustic cavitation causes, chemical environment are that people prepare nano material and provide important approach.
Pei little Miao etc. take hexamethylenetetramine as precipitation agent, and under have studied ultrasonic field, sol-gel method prepares nanometer Al 2o 3the technique of powder, has carried out scanning electron microscope (SEM) to product, X-ray diffraction (XRD) has been analyzed and sreen analysis.Experimental result shows, hyperacoustic introducing can significantly improve the performance of powder.The presoma that supersound process is crossed has obtained 1100 DEG C of calcinings for 2 hours reunites less, and median size is at the α-Al of about 30nm 2o 3powder.
Wang Yajuan etc. are with aluminum nitrate and volatile salt for raw material, and the method utilizing ultrasonic wave to be combined with precipitated phase, has obtained the alumina ultrafine powder that median size is (12 ± 2) nm.Through XRD, TG and DTA experimental analysis, precipitation knows that its chemical constitution is NH 4al (OH) 2cO 3, this is deposited in 475K and starts to be decomposed into aluminum oxide, is almost converted into θ-Al completely at 1273K 2o 3.
Ultrasonic cavitation greatly can improve the speed of inhomogeneous reaction, and Jie realized between inhomogeneous reaction thing sees Homogeneous phase mixing, the diffusion process of accelerated reaction thing and product, promotes the generation of solid cenotype, controls size and the distribution of particle.Compare with traditional method in the mass transfer of ultrasonic wave between the heterogeneous interface of strengthening and there is obvious advantage and distinctive feature.The new trend that chemical reaction or transmittance process are chemistry and chemical field is in recent years strengthened by the efficient coupling of different technologies.Such as laser technology, high-gravity technology, plasma technique, microwave technology etc. have relevant research report in the preparation of nano material, feature for concrete system designs the optimum combination between these technology, likely reaches the object of anticipation with less cost.At present, market has had plant-scale ultrasonic wave generating apparatus, this is ultrasonic technique is used for mass-producing preparation that is ultra-fine and nano-powder material to lay the foundation, and ultrasonic technique has vast potential for future development in this respect.
Nano aluminium oxide crystalline phase is stable, hardness is high, good stability of the dimension, can be widely used in various paint, play effect that is wear-resisting, Hardening.The hardness of paint generally increases along with the increase of nano aluminium oxide addition, and wear resistance can reach optimum value when the certain addition of nano aluminium oxide, and mechanical property ratio uses common aluminum oxide to strengthen 8-10 doubly.
In recent years, the research of ultrasonic technique in novel material synthesis is very active, is a kind of effective technology preparing nano material.The special physics that acoustic cavitation causes, chemical environment are that the preparation of nano material provides important channel.Ultrasonic wave effectively can promote the generation of solid cenotype, controls the size of particle and distribution, and particle size is little and be evenly distributed.Ultrasonic cavitation produces localized hyperthermia's high pressure, and its shockwave produced and microjet have porphyrization, can stop the formation of hydrogen bond, reaches the object preventing from reuniting.
Under ultrasonic field effect, add a certain amount of dispersion agent, utilize chemical precipitation method to prepare the nano aluminium oxide of certain pattern, size tunable, added in paint, the paint for production excellent property provides new thinking.
Summary of the invention
An object of the present invention is to overcome the deficiencies in the prior art, provides a kind of ultrasonic synthetic method of nano aluminium oxide.
The invention provides a kind of ultrasonic synthetic method of nano aluminium oxide, with Al (NO 3) 3for raw material, NH 4hCO 3for precipitation agent, calcine after supersound process, prepare presoma, obtain nano aluminium oxide.
Further, Al (NO is got 3) 3solution, adds PEG300, mixes, and obtains mixing solutions; NH is added in described mixing solutions 4hCO 3solution, measure pH value, supersound process, filters after ageing, discards filtrate, washing precipitation, and after drying, calcining, with stove naturally cooling, obtains nano aluminium oxide.
Further, Al (NO is got 3) 3solution, adds PEG300, and vigorous stirring mixes, and obtains mixing solutions; Separately get NH isopyknic with described mixing solutions 4hCO 3solution, by described mixing solutions and described NH 4hCO 3solution is placed in 40 DEG C of water-bath constant temperature 15min respectively, then rapid in described NH 4hCO 3solution adds in described mixing solutions and mixes, and measure pH value, supersound process, filters after ageing 24h, discard filtrate, washing precipitation, and after drying, calcining, with stove naturally cooling, obtains nano aluminium oxide.
Further, described Al (NO 3) 3with NH 4hCO 3mol ratio be 1:3.
Further, described supersound process parameter is frequency 20kHz, power 100w, ultrasonication time 30-90 minute.
Further, described pH < 9.10.
Further, the method for described washing precipitation is for respectively to wash once with dehydrated alcohol and ammoniacal liquor respectively.
Further, the condition of described oven dry is 100 DEG C of oven dry 1h.
Further, the temperature of described calcining is 500-900 DEG C, and the time of calcining is 1.5h.
Further, described nano aluminium oxide is bar-shaped γ-Al 2o 3.
The present invention also provides a kind of above-mentioned nano aluminium oxide preparing the application in paint.
Beneficial effect of the present invention is: the ultrasonic synthetic method of nano aluminium oxide of the present invention, by the feature such as nano aluminium oxide pattern, performance of synthesizing the control effect of ultrasound parameter, promotion sonochemical method is prepared further developing of nano material, for nanosecond science and technology inject new vitality.Add in paint by nano aluminium oxide of the present invention, the production for the paint of excellent property provides new thinking.
Accompanying drawing explanation
Figure 1 shows that the infrared spectra of ultrasonic synthetic method three embodiments of nano aluminium oxide of the present invention;
Figure 2 shows that the XRD figure of ultrasonic synthetic method three embodiments of nano aluminium oxide of the present invention;
Figure 3 shows that the SEM figure of the embodiment of the present invention 3.
Embodiment
Hereafter will describe the specific embodiment of the invention in detail in conjunction with concrete accompanying drawing.It should be noted that the combination of technical characteristic or the technical characteristic described in following embodiment should not be considered to isolated, they can mutually be combined thus be reached better technique effect.
Embodiment one
Al (the NO of preparation 0.1mol/L 3) 3the NH of solution and 0.3mol/L 4hCO 3solution.Get the Al (NO of the 0.1mol/L prepared 3) 3solution, adds a small amount of PEG300, vigorous stirring, mixes, obtain mixing solutions; Separately get the NH of isopyknic 0.3mol/L with mixing solutions 4hCO 3solution, by mixing solutions and NH 4hCO 3solution is placed in 40 DEG C of water-bath constant temperature 15min respectively, then rapid in NH 4hCO 3solution adds in mixing solutions and mixes, and measures pH=8.08, at frequency 20kHz, and in the ultrasonic field of power 100w ultrasonic 30 minutes.After ultrasonic end, remove sample, filter, discard filtrate, use dehydrated alcohol and each washing precipitation of ammoniacal liquor respectively once after ageing 24h, dry 1h for 100 DEG C, put into crucible, design temperature is 500 DEG C, and calcining 1.5h, with stove naturally cooling, obtains bar-shaped γ-Al 2o 3and coacervate.
Embodiment two
Al (the NO of preparation 0.1mol/L 3) 3the NH of solution and 0.3mol/L 4hCO 3solution.Get the Al (NO of the 0.1mol/L prepared 3) 3solution, adds a small amount of PEG300, vigorous stirring, mixes, obtain mixing solutions; Separately get the NH of isopyknic 0.3mol/L with mixing solutions 4hCO 3solution, by mixing solutions and NH 4hCO 3solution is placed in 40 DEG C of water-bath constant temperature 15min respectively, then rapid in NH 4hCO 3solution adds in mixing solutions and mixes, and measures pH=8.08, at frequency 20kHz, and in the ultrasonic field of power 100w ultrasonic 30 minutes.After ultrasonic end, remove sample, filter, discard filtrate, use dehydrated alcohol and each washing precipitation of ammoniacal liquor respectively once after ageing 24h, dry 1h for 100 DEG C, put into crucible, design temperature is 700 DEG C, and calcining 1.5h, with stove naturally cooling, obtains bar-shaped γ-Al 2o 3and coacervate.
Embodiment three
Al (the NO of preparation 0.1mol/L 3) 3the NH of solution and 0.3mol/L 4hCO 3solution.Get the Al (NO of the 0.1mol/L prepared 3) 3solution, adds a small amount of PEG300, vigorous stirring, mixes, obtain mixing solutions; Separately get the NH of isopyknic 0.3mol/L with mixing solutions 4hCO 3solution, by mixing solutions and NH 4hCO 3solution is placed in 40 DEG C of water-bath constant temperature 15min respectively, then rapid in NH 4hCO 3solution adds in mixing solutions and mixes, and measures pH=8.08, at frequency 20kHz, and in the ultrasonic field of power 100w ultrasonic 30 minutes.After ultrasonic end, remove sample, filter, discard filtrate, use dehydrated alcohol and each washing precipitation of ammoniacal liquor respectively once after ageing 24h, dry 1h for 100 DEG C, put into crucible, design temperature is 900 DEG C, and calcining 1.5h, with stove naturally cooling, obtains bar-shaped γ-Al 2o 3.
Design temperature is 900 DEG C, and calcining 1.5h, with stove naturally cooling, obtains bar-shaped γ-Al 2o 3; And 500 DEG C and 700 DEG C bar-shaped except having, also have coacervate, also can find out XRD figure only have 900 DEG C for γ-Al 2o 3; And the crystal formation more complicated of 500 DEG C and 700 DEG C, guess is the rising along with calcining temperature, Al 2o 3crystal formation there occurs conversion, 900 DEG C become γ-Al 2o 3.
As shown in Figure 1, at 400-1000cm -1have a wide absorption band in wave-number range, this is the characteristic absorption band of nano aluminium oxide.Calcine 500 DEG C, 700 DEG C as seen from the figure, produce characteristic absorbance all herein with 900 DEG C, compare with document and be not difficult to find out that low temperature can prepare nano aluminium oxide under ultrasonic field.At 1600-1000cm -1interval three stronger absorption peaks, lay respectively at 1394cm -1, 1516cm -1, 1635cm -1left and right.The absorption of sample peak intensity of differing temps calcination processing is different.Owing to have employed ultrasonic technique, prepare the nano aluminium oxide crystal that particle diameter is less.Nano alumina surface atom occupies sizable ratio, and comes to life perpendicular to the outstanding key vertical telescopic vibration on surface, and the bands of a spectrum relevant with longitudinal acoustical mode are strengthened.Meanwhile, the nanometer Al that sintering temperature can obtain different crystal forms is controlled 2o 3.700 DEG C of sample 1390cm in Fig. 1 -1and 1520cm -1absorption intensity obviously weaken, illustrate and mainly obtain nanocluster to only have the outstanding key chattering of nano aluminium oxide effectively could produce absorption band, and the outstanding key of surface atom is more, and band intensity is larger.Contrast 500 DEG C and 900 DEG C of samples can find, when calcining temperature is respectively 500 DEG C and 900 DEG C, absorption peak strength increases, and the composition minimizing of nanocluster is described, and infer with this, aluminum oxide experienced by the transformation of pattern 700 DEG C time, and degree of crystallization slightly increases.
As shown in Figure 2, calcine 1.5 hours for 500 DEG C, precursor has been converted into amorphous γ-Al 2o 3, three diffraction peaks the strongest 67.037 ° in figure, 45.679 °, 37.016 ° of corresponding d values are respectively: 0.13949,0.19345 and 0.24255 and standard PDF card in γ-Al 2o 3card (29-63) goodness of fit better.When 700 DEG C, the diffraction peak of 37.016 ° is more obvious, and the diffraction peak at 67.037 ° and 45.679 ° places is more sharp-pointed, and illustrate that calcining temperature raises, crystallization degree strengthens.The crystal formation comparatively single and γ-Al that particle diameter is less is obtained when 900 DEG C 2o 3, conform to results of IR.
As shown in Figure 3, compare for 1:3 in the amount of aluminium salt and precipitant material, prepare presoma under the condition of pH < 9.10,900 DEG C of calcining precursor 1.5h are act on 30min in the ultrasonic field of 20kHz can obtain comparatively homogeneous rod-like nano aluminum oxide in frequency.
The nano aluminium oxide taken a morsel adds silane coupling agent and carries out surface modification, ultrasonic disperse in emulsion monomer, pre-emulsification 30min.Get 1/6 pre-emulsion, drip initiator and pre-emulsion under water-bath 65 DEG C of-70 DEG C of conditions, reaction 3h, be warming up to 95 DEG C, constant temperature 30min, adjustment pH is 8-9, discharging.Emulsion is milky white band blue phase stiff fluid, evenly not stratified.
In deionized water, add spices, wetting agent, tensio-active agent, film coalescence aid is uniformly dispersed in high speed homogenization agitator high speed.Add a certain proportion of talcum powder, titanium dioxide, calcium carbonate high-speed stirring evenly, drip proper quantity of defoaming agent, change stirring at low speed into, add emulsion, mould inhibitor, thickening material after stirring, dispersed with stirring is even, filters discharging.Coating appearance is white stiff fluid, mensuration viscosity is 120-200s, solid content >40%, surface drying time 7min, actual drying time 24h, 25 DEG C of water resistance test >96h are without whiting, place after 2 months without caking, do not affect use after stirring, again detect, indices is all qualified.
The ultrasonic synthetic method of nano aluminium oxide of the present invention, by the feature such as nano aluminium oxide pattern, performance of synthesizing the control effect of ultrasound parameter, prepares further developing of nano material by promotion sonochemical method, for nanosecond science and technology inject new vitality.Add in paint by nano aluminium oxide of the present invention, the production for the paint of excellent property provides new thinking.
Although give some embodiments of the present invention, it will be understood by those of skill in the art that without departing from the spirit of the invention herein, can change embodiment herein.Above-described embodiment is exemplary, should using embodiment herein as the restriction of interest field of the present invention.

Claims (10)

1. a ultrasonic synthetic method for nano aluminium oxide, is characterized in that, with Al (NO 3) 3for raw material, NH 4hCO 3for precipitation agent, calcine after supersound process, prepare presoma, obtain nano aluminium oxide.
2. the ultrasonic synthetic method of nano aluminium oxide as claimed in claim 1, is characterized in that, get Al (NO 3) 3solution, adds PEG300, mixes, and obtains mixing solutions; NH is added in described mixing solutions 4hCO 3solution, measure pH value, supersound process, filters after ageing, discards filtrate, washing precipitation, and after drying, calcining, with stove naturally cooling, obtains nano aluminium oxide.
3. the ultrasonic synthetic method of nano aluminium oxide as claimed in claim 2, is characterized in that, get Al (NO 3) 3solution, adds PEG300, and vigorous stirring mixes, and obtains mixing solutions; Separately get NH isopyknic with described mixing solutions 4hCO 3solution, by described mixing solutions and described NH 4hCO 3solution is placed in 40 DEG C of water-bath constant temperature 15min respectively, then rapid in described NH 4hCO 3solution adds in described mixing solutions and mixes, and measure pH value, supersound process, filters after ageing 24h, discard filtrate, washing precipitation, and after drying, calcining, with stove naturally cooling, obtains nano aluminium oxide.
4. the ultrasonic synthetic method of the nano aluminium oxide as described in any one of claim 1-3, is characterized in that, described Al (NO 3) 3with NH 4hCO 3mol ratio be 1:3.
5. the ultrasonic synthetic method of nano aluminium oxide as claimed in claim 4, it is characterized in that, described supersound process parameter is frequency 20kHz, power 100w, ultrasonication time 30-90 minute.
6. the ultrasonic synthetic method of nano aluminium oxide as claimed in claim 5, is characterized in that, described pH < 9.10.
7. the ultrasonic synthetic method of nano aluminium oxide as claimed in claim 6, it is characterized in that, the method for described washing precipitation is for respectively to wash once with dehydrated alcohol and ammoniacal liquor respectively.
8. the ultrasonic synthetic method of nano aluminium oxide as claimed in claim 7, is characterized in that, the condition of described oven dry is 100 DEG C dries 1h.
9. the ultrasonic synthetic method of nano aluminium oxide as claimed in claim 8, it is characterized in that, the temperature of described calcining is 500-900 DEG C, and the time of described calcining is 1.5h.
10. the ultrasonic synthetic method of the nano aluminium oxide as described in claim 1-3, any one of 5-9, is characterized in that, described nano aluminium oxide is bar-shaped γ-Al 2o 3.
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CN106799500A (en) * 2017-01-05 2017-06-06 天津大学 The preparation method of ultrafine tungsten powder
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CN106799500A (en) * 2017-01-05 2017-06-06 天津大学 The preparation method of ultrafine tungsten powder
CN106799500B (en) * 2017-01-05 2019-03-29 天津大学 The preparation method of ultrafine tungsten powder
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CN108558373A (en) * 2018-06-13 2018-09-21 宣城晶瑞新材料有限公司 A kind of preparation and application of novel nano alumina ceramic material
CN117843020A (en) * 2024-01-04 2024-04-09 兰州兰石中科纳米科技有限公司 Preparation method of nano alumina powder

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