CN103274671A - Preparation method for alpha-alumina balls - Google Patents
Preparation method for alpha-alumina balls Download PDFInfo
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- CN103274671A CN103274671A CN2013101424073A CN201310142407A CN103274671A CN 103274671 A CN103274671 A CN 103274671A CN 2013101424073 A CN2013101424073 A CN 2013101424073A CN 201310142407 A CN201310142407 A CN 201310142407A CN 103274671 A CN103274671 A CN 103274671A
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Abstract
The invention discloses a preparation method for alpha-alumina balls. The preparation method is characterized by comprising the steps of weighing deionized water and aluminium isopropoxide according to a molar ratio of the deionized water to aluminium isopropoxide being 50-150 : 1; weighing nitric acid according to a molar ratio of the nitric acid to aluminium isopropoxide being 0.15-0.25 : 1; mixing aluminium isopropoxide and the deionized water, hydrolyzing, adding the nitric acid; reacting for 1-10 hours; putting the obtained materials into a drying oven; drying the obtained material to get a gel; dropping the gel in a flask of a rotary evaporator; controlling rotary speed, evaporation temperature and evaporation time of the rotary evaporator to prepare alumina gel balls; putting the alumina gel balls in the drying oven to dry the alumina gel balls; and sintering the alumina gel balls to obtain the alpha-alumina balls. The preparation method employs a sol-gel method to form the balls; synthetic process is green, environment-friendly and simple; operations are safe; and the preparation method can realize industrialization easily. The prepared alpha-alumina balls can be used as an adsorbent, a desiccant, a catalyst, a carrier and the like in the fields such as medicines, chemical engineering, environment protection, etc.
Description
Technical field
The invention belongs to the preparation of the oxide compound of aluminium, relate to a kind of preparation method of Alpha-alumina ball.The Alpha-alumina ball of the present invention's preparation can be used as sorbent material, siccative and catalyzer or carrier etc. and is widely used in fields such as medicine, chemical industry, environmental protection.
Background technology
Along with the raising of fast development of social economy and people's living standard, also more and more higher to the service requirements of material.Stupalith is acknowledged as to have: advantage such as high strength, high rigidity and good wear resistance and erosion resistance, have incomparable characteristics such as metallic substance, organic polymer material, and in numerous industries, bringing into play indispensable effect.And ceramic microsphere is because its unique microsphere particle advantage makes ceramic microsphere be widely used in fields such as military project, medicine, chemical industry, environmental protection, nuclear technique.From the sixties in last century so far, more and more deep to the research of ceramic microsphere, it is abundant that its preparation method also is tending towards.The preparation method of at present existing multiple ceramic microsphere, as inverse suspension polymerization method, oily newborn method, polymerization-induce methods such as colloid aggregation method, air-flow polishing, method of fusion, sol-gel method, microballoons such as TiO2, ZrO2, SiO2, SiC, B4C, UO2, Al2O3 have been prepared by these methods.Inverse suspension polymerization method, oily newborn method, polymerization-induce the ceramic microsphere particle diameter of method preparations such as colloid aggregation method too little and wayward, the microballoon balling-up efficient of air-flow polishing preparation is low, it is not high to be difficult to scale operation, energy utilization rate, the method of fusion power consumption is high, the balling-up temperature range is wayward, easily form the low microballoon of sphericity, microspherulite diameter is bigger than normal, and the alumina balls size of traditional sol-gel method preparation is too little.
Alumina ceramic material since characteristics such as it is high temperature resistant, resistance to chemical attack, wear-resisting, thermal conductivity height receive much concern always.Be widely used at surfacecti proteon layer material, optical material, catalyzer and aspects such as carrier, semiconductor material thereof.In the prior art, Hou Chunlou adopts gel aluminium hydroxide as raw material, prepare aluminum oxide micro-sphere with special agglomeration technique device, but prepared alumina balls is the gama-alumina ball, and test used agglomeration technique device complexity, the microsphere particle abrasion of gained are bigger.Zhu Hongfa utilizes spray drying process to make gama-alumina microsphere, and the spray drying unit that this method relates to is complicated, and power consumption is high, and the microspherulite diameter of gained is less, and mostly about tens microns, and size distribution is inhomogeneous.The alumina-ceramic ball major part of Sheng Chaning all is to use the method for fusion blowing and balling in the market, and the required high temperature of its fusing causes power consumption height, complex technical process.
Summary of the invention
Purpose of the present invention is intended to overcome deficiency of the prior art, based on sol-gel method, provides that a kind of raw material is inexpensive, technology is simple, operational safety, easily realize the preparation method of the Alpha-alumina ball of suitability for industrialized production.
Content of the present invention is: a kind of preparation method of Alpha-alumina ball, its feature part is to comprise the following steps:
A, batching: by deionized water: aluminum isopropylate is that the mol ratio of 50~150:1 is removed ionized water and (solid material) aluminum isopropylate, and by nitric acid: aluminum isopropylate is that the mol ratio of 0.15~0.25:1 is got (peptizing agent) nitric acid;
B, prepared in reaction colloidal sol: aluminum isopropylate is mixed, is hydrolyzed with deionized water behind 1~5h, add nitric acid and react 1~10h again, obtain reacting rear material, the baking oven of reacting rear material being put into temperature again and be 80 ℃~110 ℃ dries by the fire 24~72h, makes (stable transparent) colloidal sol;
C, preparation gel ball: (for example: round-bottomed flask colloidal sol is added dropwise to the flask of (can be added dropwise to by syringe or other prior art mode) rotatory evaporator, or other container) in, the speed of rotation of control rotatory evaporator is that 10~150r/min, vaporization temperature are 60 ℃~95 ℃, after evaporation time is 3~12h, make the alumina gel ball;
D, preparation Alpha-alumina ball: with the alumina gel ball put into temperature be 80 ℃~110 ℃ baking oven through 12~48h oven dry after, through calcining (calcining in the High Temperature Furnaces Heating Apparatus), namely make Alpha-alumina ball product again.
In the content of the present invention: the temperature of the described hydrolysis of step a is 70~95 ℃ preferably.
In the content of the present invention: the program of the described calcining of steps d is preferably: the alumina gel ball after will drying is warming up to 400~500 ℃ with the speed of 2~10 ℃/min, speed with 3~10 ℃/min is warming up to 900~1000 ℃ then, speed with 2~6 ℃/min is warming up to 1050~1200 ℃ at last, is incubated 100~300min down at 1050~1200 ℃ again.
In the content of the present invention: there is Shanghai Yarong Biochemical Instrument Plant etc. in the manufacturing enterprise of described rotatory evaporator, is existing commercially available prod.
The particle size distribution range of the Alpha-alumina ball that the preparation method of Alpha-alumina ball of the present invention makes is that 0.1-2mm, crystal formation are α-Al2O3.
Compared with prior art, the present invention has following characteristics and beneficial effect:
(1) adopts the present invention, owing to can not dissolve each other between the out of phase liquid (oil phase and water), contact at the interface two, molecule is because being subjected to force unbalance, have higher energy than interior molecules, in order to reduce surface energy, it is that shrink on the free surface that the surface tension of liquid is tried hard to; So splash in the silicone oil colloidal sol since the surface tension effects of liquid exist with spherical state, thereby form water in oil micro emulsion grain; This micro emulsion grain has just obtained prepared Alpha-alumina ball through subsequent drying and calcination process;
(2) adopt the present invention, cost of material is cheap, does not add organic solvent or toxic substance in the balling-up process, and the waste liquid of generation is convenient to handle; Processing unit is simple, the operation environmental protection, and green safety, production cost is low; Can obtain particle size range at α-Al2O3 ball of 0.1-2mm by regulating solidification value;
(3) α-Al2O3 ball of the present invention's preparation, a step balling-up, technology is simple; Sintering process is finished under air atmosphere, need not to control sintering atmosphere, and sintering temperature is easy to control, and step is simple, and production cost is lower, easily realizes suitability for industrialized production;
(4) the present invention has effectively overcome the deficiency of alumina-ceramic ball technology of preparing in the prior art, and preparation technology is simple, and operation is easy, and operation is practical easily; The Alpha-alumina ball of preparation can be used as sorbent material, siccative and catalyzer or carrier etc. and is widely used in fields such as medicine, chemical industry, environmental protection.
Description of drawings
Fig. 1 is the micro-Electronic Speculum figure of the Alpha-alumina ball that makes; Resulting α-Al2O3 spherolite footpath is about 1mm as known in the figure, surperficial smoother, sphericity height;
Fig. 2 is the X ray diffracting spectrum of the Alpha-alumina ball that makes; The ball that obtains as known in the figure is the perfect α of crystal formation-Al2O3 ball.
Embodiment
Embodiment given below intends so that the invention will be further described; but can not be interpreted as it is limiting the scope of the invention; the person skilled in art to some nonessential improvement and adjustment that the present invention makes, still belongs to protection scope of the present invention according to the content of the invention described above.
Embodiment 1:
A kind of preparation method of Alpha-alumina ball comprises the following steps:
A, batching: by deionized water: the mol ratio of aluminum isopropylate is that the proportional of 100:1 is removed ionized water, aluminum isopropylate, and according to nitric acid: the mol ratio of aluminum isopropylate is that the ratio of 0.25:1 is measured nitric acid;
B, prepared in reaction colloidal sol: be dissolved in aluminum isopropylate in the deionized water and hydrolysis 3h in 85 ℃ water-bath environment, and then move in the baking oven after splashing into the nitric acid of measuring, reaction 2h, under 80 ℃ temperature, leave standstill 72h, obtain the alumina sol of stable transparent;
C, preparation gel ball: alumina sol is splashed in the flask of rotatory evaporator with syringe, the control speed of rotation is that 40r/min, vaporization temperature are 85 ℃, obtains gel ball after evaporation 12h solidifies;
D, preparation Alpha-alumina ball: gel ball put into put into High Temperature Furnaces Heating Apparatus after the baking oven oven dry and calcine, heating schedule is: with the speed of 4 ℃/min be warming up to 500 ℃, then with the speed of 4 ℃/min be warming up to 1000 ℃, again be warming up to 1150 ℃ with the speed of 5 ℃/min after, under 1150 ℃ temperature, be incubated 3h, namely make α-Al2O3 ball.
Embodiment 2:
A kind of preparation method of Alpha-alumina ball comprises the following steps:
A, batching: by deionized water: aluminum isopropylate is that the mol ratio of 50~150:1 is removed ionized water and (solid material) aluminum isopropylate, and by nitric acid: aluminum isopropylate is that the mol ratio of 0.15~0.25:1 is got (peptizing agent) nitric acid;
B, prepared in reaction colloidal sol: aluminum isopropylate is mixed, is hydrolyzed with deionized water behind 1~5h, add nitric acid and react 1~10h again, obtain reacting rear material, the baking oven of reacting rear material being put into temperature again and be 80 ℃~110 ℃ dries by the fire 24~72h, makes (stable transparent) colloidal sol;
C, preparation gel ball: (for example: round-bottomed flask colloidal sol is added dropwise to the flask of (can be added dropwise to by syringe or other prior art mode) rotatory evaporator, or other container) in, the speed of rotation of control rotatory evaporator is that 10~150r/min, vaporization temperature are 60 ℃~95 ℃, after evaporation time is 3~12h, make the alumina gel ball;
D, preparation Alpha-alumina ball: with the alumina gel ball put into temperature be 80 ℃~110 ℃ baking oven through 12~48h oven dry after, through calcining, namely make Alpha-alumina ball product again.
Embodiment 3:
A kind of preparation method of Alpha-alumina ball comprises the following steps:
A, batching: by deionized water: aluminum isopropylate is that the mol ratio of 100:1 is removed ionized water and (solid material) aluminum isopropylate, and by nitric acid: aluminum isopropylate is that the mol ratio of 0.2:1 is got (peptizing agent) nitric acid;
B, prepared in reaction colloidal sol: aluminum isopropylate is mixed, is hydrolyzed with deionized water behind the 3h, add nitric acid and react 5h again, obtain reacting rear material, the baking oven of reacting rear material being put into temperature again and be 90 ℃ dries by the fire 48h, makes (stable transparent) colloidal sol;
C, preparation gel ball: (for example: round-bottomed flask colloidal sol is added dropwise to the flask of (can be added dropwise to by syringe or other prior art mode) rotatory evaporator, or other container) in, the speed of rotation of control rotatory evaporator is that 80r/min, vaporization temperature are 80 ℃, after evaporation time is 7h, make the alumina gel ball;
D, preparation Alpha-alumina ball: with the alumina gel ball put into temperature be 90 ℃ baking oven through the 30h oven dry after, through calcining, namely make Alpha-alumina ball product again.
Embodiment 4:
A kind of preparation method of Alpha-alumina ball comprises the following steps:
A, batching: by deionized water: aluminum isopropylate is that the mol ratio of 50:1 is removed ionized water and (solid material) aluminum isopropylate, and by nitric acid: aluminum isopropylate is that the mol ratio of 0.15:1 is got (peptizing agent) nitric acid;
B, prepared in reaction colloidal sol: aluminum isopropylate is mixed, is hydrolyzed with deionized water behind the 1h, add nitric acid and react 1h again, obtain reacting rear material, the baking oven of reacting rear material being put into temperature again and be 80 ℃ dries by the fire 72h, makes (stable transparent) colloidal sol;
C, preparation gel ball: (for example: round-bottomed flask colloidal sol is added dropwise to the flask of (can be added dropwise to by syringe or other prior art mode) rotatory evaporator, or other container) in, the speed of rotation of control rotatory evaporator is that 10r/min, vaporization temperature are 60 ℃, after evaporation time is 12h, make the alumina gel ball;
D, preparation Alpha-alumina ball: with the alumina gel ball put into temperature be 80 ℃ baking oven through the 48h oven dry after, through calcining, namely make Alpha-alumina ball product again.
Embodiment 5:
A kind of preparation method of Alpha-alumina ball comprises the following steps:
A, batching: by deionized water: aluminum isopropylate is that the mol ratio of 150:1 is removed ionized water and (solid material) aluminum isopropylate, and by nitric acid: aluminum isopropylate is that the mol ratio of 0.25:1 is got (peptizing agent) nitric acid;
B, prepared in reaction colloidal sol: aluminum isopropylate is mixed, is hydrolyzed with deionized water behind the 5h, add nitric acid and react 10h again, obtain reacting rear material, the baking oven of reacting rear material being put into temperature again and be 110 ℃ dries by the fire 24h, makes (stable transparent) colloidal sol;
C, preparation gel ball: (for example: round-bottomed flask colloidal sol is added dropwise to the flask of (can be added dropwise to by syringe or other prior art mode) rotatory evaporator, or other container) in, the speed of rotation of control rotatory evaporator is that 150r/min, vaporization temperature are 95 ℃, after evaporation time is 3h, make the alumina gel ball;
D, preparation Alpha-alumina ball: with the alumina gel ball put into temperature be 110 ℃ baking oven through the 12h oven dry after, through calcining, namely make Alpha-alumina ball product again.
Embodiment 6~12:
A kind of preparation method of Alpha-alumina ball comprises the following steps:
A, batching: by deionized water: aluminum isopropylate is that the mol ratio of 50~150:1 is removed ionized water and (solid material) aluminum isopropylate, and by nitric acid: aluminum isopropylate is that the mol ratio of 0.15~0.25:1 is got (peptizing agent) nitric acid;
The concrete mol ratio of each feed composition sees the following form among each embodiment:
Annotate: go up the numerical value " 60 " that embodiment is numbered under 6 in the table and represent deionized water: the mol ratio of aluminum isopropylate is 60:1, and numerical value " 0.17 " expression nitric acid: the mol ratio of aluminum isopropylate is 0.17:1, the numerical value under other embodiment numbers and the like.
B, prepared in reaction colloidal sol: aluminum isopropylate is mixed, is hydrolyzed with deionized water behind the 3h, add nitric acid and react 5h again, obtain reacting rear material, the baking oven of reacting rear material being put into temperature again and be 95 ℃ dries by the fire 48h, makes (stable transparent) colloidal sol;
C, preparation gel ball: (for example: round-bottomed flask colloidal sol is added dropwise to the flask of (can be added dropwise to by syringe or other prior art mode) rotatory evaporator, or other container) in, the speed of rotation of control rotatory evaporator is that 70r/min, vaporization temperature are 75 ℃, after evaporation time is 6h, make the alumina gel ball;
D, preparation Alpha-alumina ball: with the alumina gel ball put into temperature be 90 ℃ baking oven through the 26h oven dry after, through calcining, namely make Alpha-alumina ball product again.
Embodiment 13: a kind of preparation method of Alpha-alumina ball, the temperature of the described hydrolysis of step a are 95 ℃, and other omits with arbitrary among the embodiment 2~12.
Embodiment 14: a kind of preparation method of Alpha-alumina ball, the temperature of the described hydrolysis of step a are 90 ℃, and other omits with arbitrary among the embodiment 2~12.
Embodiment 15: a kind of preparation method of Alpha-alumina ball, the temperature of the described hydrolysis of step a are 70 ℃, and other omits with arbitrary among the embodiment 2~12.
Embodiment 16: a kind of preparation method of Alpha-alumina ball, the temperature of the described hydrolysis of step a are 75 ℃, and other omits with arbitrary among the embodiment 2~12.
Embodiment 17: a kind of preparation method of Alpha-alumina ball, the temperature of the described hydrolysis of step a are 80 ℃, and other omits with arbitrary among the embodiment 2~12.
Embodiment 18:
A kind of preparation method of Alpha-alumina ball, the program of the described calcining of steps d is: the alumina gel ball after will drying is warming up to 400~500 ℃ with the speed of 2~10 ℃/min, speed with 3~10 ℃/min is warming up to 900~1000 ℃ then, speed with 2~6 ℃/min is warming up to 1050~1200 ℃ at last, be incubated 100~300min down at 1050~1200 ℃ again, other omits with arbitrary among the embodiment 2~17.
Embodiment 19:
A kind of preparation method of Alpha-alumina ball, the program of the described calcining of steps d is: the alumina gel ball after will drying is warming up to 400 ℃ with the speed of 2 ℃/min, speed with 3 ℃/min is warming up to 900 ℃ then, speed with 2 ℃/min is warming up to 1050 ℃ at last, be incubated 300min down at 1050 ℃ again, other omits with arbitrary among the embodiment 2~17.
Embodiment 20:
A kind of preparation method of Alpha-alumina ball, the program of the described calcining of steps d is: the alumina gel ball after will drying is warming up to 500 ℃ with the speed of 10 ℃/min, speed with 10 ℃/min is warming up to 1000 ℃ then, speed with 6 ℃/min is warming up to 1200 ℃ at last, be incubated 100min down at 1200 ℃ again, other omits with arbitrary among the embodiment 2~17.
Embodiment 21:
A kind of preparation method of Alpha-alumina ball, the program of the described calcining of steps d is: the alumina gel ball after will drying is warming up to 450 ℃ with the speed of 6 ℃/min, speed with 6 ℃/min is warming up to 950 ℃ then, speed with 4 ℃/min is warming up to 1100 ℃ at last, be incubated 150min down at 1100 ℃ again, other omits with arbitrary among the embodiment 2~17.
Embodiment 22:
A kind of preparation method of Alpha-alumina ball, the program of the described calcining of steps d is: the alumina gel ball after will drying is warming up to 430 ℃ with the speed of 3 ℃/min, speed with 4 ℃/min is warming up to 930 ℃ then, speed with 3 ℃/min is warming up to 1080 ℃ at last, be incubated 140min down at 1080 ℃ again, other omits with arbitrary among the embodiment 2~17.
Embodiment 23:
A kind of preparation method of Alpha-alumina ball, the program of the described calcining of steps d is: the alumina gel ball after will drying is warming up to 480 ℃ with the speed of 8 ℃/min, speed with 8 ℃/min is warming up to 980 ℃ then, speed with 5 ℃/min is warming up to 1170 ℃ at last, be incubated 260min down at 1170 ℃ again, other omits with arbitrary among the embodiment 2~17.
In above-described embodiment: there is Shanghai Yarong Biochemical Instrument Plant etc. in the manufacturing enterprise of described rotatory evaporator, is existing commercially available prod.
In above-described embodiment: each raw material that adopts is the commercially available prod.
In above-described embodiment: in the percentage that adopts, do not indicate especially, be quality (weight) percentage; Described quality (weight) part can all be gram or kilogram; Described mole is the expression amount of substance, and symbol is mol.
In above-described embodiment: the processing parameter in each step (temperature, time, speed, speed of rotation etc.) and each amounts of components numerical value etc. are scope, and any point is all applicable.
The not concrete same prior art of narrating of technology contents in content of the present invention and above-described embodiment.
The invention is not restricted to above-described embodiment, content of the present invention is described all can implement and have described good result.
Claims (3)
1. the preparation method of an Alpha-alumina ball is characterized in that comprising the following steps:
A, batching: by deionized water: aluminum isopropylate is that the mol ratio of 50~150:1 is removed ionized water and aluminum isopropylate, and by nitric acid: aluminum isopropylate is that the mol ratio of 0.15~0.25:1 is got nitric acid;
B, prepared in reaction colloidal sol: aluminum isopropylate is mixed, is hydrolyzed with deionized water behind 1~5h, add nitric acid and react 1~10h again, obtain reacting rear material, the baking oven of reacting rear material being put into temperature again and be 80 ℃~110 ℃ dries by the fire 24~72h, makes colloidal sol;
C, preparation gel ball: colloidal sol is added dropwise in the flask of rotatory evaporator, the speed of rotation of control rotatory evaporator is that 10~150r/min, vaporization temperature are 60 ℃~95 ℃, after evaporation time is 3~12h, makes the alumina gel ball;
D, preparation Alpha-alumina ball: with the alumina gel ball put into temperature be 80 ℃~110 ℃ baking oven through 12~48h oven dry after, through calcining, namely make Alpha-alumina ball product again.
2. by the preparation method of the described Alpha-alumina ball of claim 1, it is characterized in that: the temperature of the described hydrolysis of step a is 70~95 ℃.
3. press the preparation method of claim 1 or 2 described Alpha-alumina balls, it is characterized in that: the program of the described calcining of steps d is: the alumina gel ball after will drying is warming up to 400~500 ℃ with the speed of 2~10 ℃/min, speed with 3~10 ℃/min is warming up to 900~1000 ℃ then, speed with 2~6 ℃/min is warming up to 1050~1200 ℃ at last, is incubated 100~300min down at 1050~1200 ℃ again.
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CN104163444A (en) * | 2014-07-18 | 2014-11-26 | 西南科技大学 | Alpha-alumina hollow ball preparation method |
CN112429755A (en) * | 2020-11-18 | 2021-03-02 | 山东物华新材料科技有限公司 | Preparation method of water treatment active alumina ball |
CN112427007A (en) * | 2020-11-18 | 2021-03-02 | 山东物华新材料科技有限公司 | Preparation method of activated alumina ball adsorbent |
CN114773036A (en) * | 2022-04-18 | 2022-07-22 | 天津大学 | Low-density composite ceramic ball for fluidized bed and preparation method and application thereof |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN112429755A (en) * | 2020-11-18 | 2021-03-02 | 山东物华新材料科技有限公司 | Preparation method of water treatment active alumina ball |
CN112427007A (en) * | 2020-11-18 | 2021-03-02 | 山东物华新材料科技有限公司 | Preparation method of activated alumina ball adsorbent |
CN114773036A (en) * | 2022-04-18 | 2022-07-22 | 天津大学 | Low-density composite ceramic ball for fluidized bed and preparation method and application thereof |
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