CN1394670A - Preparation method of nano-grade powder by using spray homogeneous precipitation process - Google Patents
Preparation method of nano-grade powder by using spray homogeneous precipitation process Download PDFInfo
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- CN1394670A CN1394670A CN 02133557 CN02133557A CN1394670A CN 1394670 A CN1394670 A CN 1394670A CN 02133557 CN02133557 CN 02133557 CN 02133557 A CN02133557 A CN 02133557A CN 1394670 A CN1394670 A CN 1394670A
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Abstract
The method for preparing nano particles by utilizing homogeneous reaction to produce precipitation includes the following steps: pressurizing precipitant liquor or solution and compound liquor or solution, and spraying them and making them into controlled fine-small liquid drops; them making the fine-small liquid drops and correspondent compound liquor or solution and precipitant gas and precipitant liquor or solution produce chemical reaction to produce microparticle precipitate. As compared with other homogeneous precipitation methods said invention can obtain the nano-grade powder body with uniform grain size and higher controlability.
Description
The present invention relates to the synthetic high-purity nm powder of liquid phase chemical, but particularly relate to precipitation from homogeneous solution, utilize the precipitation row to nanometer grade powder.
Known in precipitation from homogeneous solution, be that making it increases lentamente, makes the precipitation reaction in the solution be in poised state by the precipitating reagent concentration in the control solution, occur equably thereby be deposited in the solution, obtain nanometer powder.As Shi Jianlin is the precipitation from homogeneous solution agent with urea, makes urea resolve into the ammonia precipitation process agent about 70 ℃.What here to point out so is, 70 ℃ of temperature add the heat that chemical synthesis produces, and is difficult to avoid the very near produced simultaneously adjacent precipitation particulate of distance to form and reunites, and the particle size that draws like this is uncontrollable, and influences the uniformity of particulate; And use precipitating reagent aspect raw material single, this just determine terrible go out nano material can not diversity.
The purpose of this invention is to provide a kind of, can homogeneous precipitation, and it is controlled to obtain particle size, has uniform and stable property, and be fit to a kind of homogeneous precipitation method of different precipitating reagents.
Precipitating reagent liquid or compound liquid, and fine drop is sprayed in their even dilute solution high-pressure rotary or gap, again with corresponding compounds liquid or homogeneous solution, precipitating reagent gas, and precipitating reagent liquid or homogeneous solution chemical reaction generation particulate deposits, can obtain powder particle of uniform size.
According to the present invention, use material to be:
Component (A) is the solute of being sprayed; Component (B) is and the corresponding chemical reactant of component (A), and component (C) be a component (A) and the sediment of component (B) reaction generation, and component (D) is component (A) solvent, and is as follows:
1. low volatility precipitating reagent (A) or they
Low liquid or the solution boiling point of being defined as of indication volatility is not less than 80 ℃ and is preferably and is not less than 100 ℃ in the above
Technological process of the present invention is:
(1) with (A) liquid or it and homogeneous solution (D) (being less than or equal to saturated concentration).Pressurization rotation or gap spraying (swing circle or off time fall into 1/3 of (B) liquid level time for being not less than droplet naturally from shower nozzle, mainly are to avoid droplet reunion and reaction heat that adjacent precipitation particulate is met again), mist particle diameter d is controlled to be
(μ m micron) V
DBe (D) solvent volume under the normal temperature and pressure, V
ABe (A) solute volume under the normal temperature and pressure.Because have only relative molecular weight now, there is not the average molecular volume, here can be roughly with atom number ratio in the unimolecule, for calculating nano particle volume ratio parameter.Draw top formula former because, be unit with 0.1 micron diameter particle volume, solute (A) volume is divided scale parameter
Divide solvent (D) volume with this ratio
Drawing the droplet volume so is that top ratio is added 1 0.1 micron diameter particle volume
(μ m) because (A) solid particle is bigger, density is sparse, and (A) volume is divided into 0.1 micron diameter particle, and with the average division that calculates, the 0.1 micron diameter particle that draws, it is much bigger to draw particle volume than pragmatize branch, so by top predication method,
(μ m) is bigger than mist particle diameter in the practical operation, requirement of the present invention
(μ m) so in the droplet that draws of practical operation solute (A) after sloughing solvent (D), particle diameter just inevitable less than
(μ m) is again because after reaction in the product, because the molecular structure difference, the sediment size also just with droplet in solute (A) volume variant, so be calculation of parameter reaction front and back with atom number ratio in the unimolecule roughly here, the particulate volume ratio just draws formula
(μ m micron)
(2) make (1) to produce droplet and in (B) gas that constantly charges into or (B) liquid that is constantly stirring or solution, react, generate sediment (C).
(3) droplet as with gas reaction, generate directly low temperature drying or fall into (C) insoluble solvent that is stirring of sediment, refilter drying.
(4) if sediment is a gained nano particle predecessor, need calcining just can produce, then in (B) solvent, add materials such as surfactant, obtain the predecessor colloidal particle, be convenient to drying, calcining.
Nanometer sediment proposed by the invention is to reach less than 100 nanometers according to mean particle dia at first to determine mist particle diameter less than 0.1 micron
(μ m micron) thus the particle diameter that obtains less than 100 nanometers.Preferred ingredient of the present invention (A) and only can react the material of producing precipitation with component (B) is if add other component then only comprise their solvent and nano-particle surface modifier and the material that can generate colloidal state that makes predecessor be convenient to calcine in preferred ingredient; And in interpolation, must not influence the original chemistry before (A) component and (B) component reaction.The sediment that generates adopts well-known low temperature drying or freeze-drying.
The present invention (A) solution concentration is equal to or less than their saturated concentration at normal temperatures and pressures, and (B) component is satisfied with complete reaction (A) component.
Mention low this notion of volatility in the present invention, major limitation (A) component liquid or their solution boiling point are more than or equal to 80 ℃, are preferably more than to equal 100 ℃.
The present invention can be applicable to produce the nano_scale particle that can generate precipitation in any chemical reaction, obtains controlled amount, uniform and stable particulate.
The following stated embodiment describes the present invention in detail
Embodiment 1, preparation CaCo
3Nano-powder
Under the normal temperature and pressure, with 1 part of calcium hydroxide uniform dissolution (every part is same volume) in 8 parts of water, again with the pressurization of this solution with rotating spraying (swing circle be droplet from shower nozzle fall into naturally the water surface time 1/3), sparge and constantly charge into CO
2In the reactor of gas, the bottom is the aqueous solution that is stirring, and adjusts pressure or shower nozzle spray eye, make mist particle diameter be smaller or equal to
(μ m) ≈ 0.208 μ m lime water fine drop and CO
2Gas reaction generates water-fast CaCO
3Powder with the sedimentation and filtration drying, obtains the calcium carbonate nano particle less than 0.1 micron.If spray particle diameter is more little, obtain deposit C aCO
3Particle is thin more.
Embodiment 2 preparation nano TiO 2 powder predecessors
Under the normal temperature and pressure, with 2 parts of titanium tetrachloride uniform dissolution (every part is same volume) in 8 parts of water, again with this homogeneous solution pressurization rotating spraying, (swing circle be droplet from shower nozzle fall into naturally the liquid level time 1/3) sparge the reactor that fills excessive ammonia solution and react, adjust pressure or shower nozzle spray eye, make mist particle diameter be controlled to be smaller or equal to
The precipitation that (μ m) ≈ 0.203 μ m draws is the titanium dioxide fine particles drying, the predecessor of calcining.
Embodiment 3 preparation ZrO
2-Y
2O
3Receive the placate powder
Under the normal temperature and pressure with 2 parts of ZrOCI
2.8H
2O and YCI
3Uniform dissolution is (every part is same volume) in 10 parts of water, again this homogeneous solution is sparged with rotary nozzle in the solution that fills excessive ammonia (swing circle be droplet from shower nozzle fall into naturally the liquid level time 1/3), adjust pressure or shower nozzle spray eye, the control mist particle diameter be smaller or equal to
(μ m) ≈ 0.276 μ m with this predecessor in solution, colloidal sol and gel, dry, calcining makes ZrO
2-Y
2O
3Nano-powder.
Claims (8)
1, (A) component liquid or it and (D) the homogeneous solution spraying of component, generates precipitation (C) component, produce nano particle with (B) component liquid or its homogeneous solution interaction energy.
2, described according to claim 1, the spraying of (A) component is satisfied condition to (A) component solution boiling point is more than or equal to 80 ℃, be preferably more than to equal 100 ℃.
3, described according to claim 1, (A) component spraying mist particle diameter smaller or equal to
4, described according to claim 1, (A) component adopts rotation or gap spraying, and swing circle and off time are for to fall into 1/3 of (B) liquid level time more than or equal to droplet naturally from shower nozzle.
5,,,, adopt low temperature drying or freeze drying to crossing filter cake (C) for preventing hard aggregation according to the described nano particle of claim 1.
6, according to described in the claim 1-5, any precipitating reagent of using, when satisfying claim 2, liquid-liquid phase and liquid-gas phase, reaction generates sediment, all can utilize the present invention to produce nanoparticle or its predecessor.
7, according to described in the right 1-3, mist particle diameter
In the scope, the d value is more little, and it is more little to obtain diameter of nano particles.
8, according to described in the 1-3,7, in droplet size one regularly, in the saturated concentration range, solute (A) concentration is more little in solvent (D) for solute (A), and it is more little to obtain diameter of nano particles.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 02133557 CN1394670A (en) | 2002-08-01 | 2002-08-01 | Preparation method of nano-grade powder by using spray homogeneous precipitation process |
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| CN 02133557 CN1394670A (en) | 2002-08-01 | 2002-08-01 | Preparation method of nano-grade powder by using spray homogeneous precipitation process |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107057090A (en) * | 2017-04-27 | 2017-08-18 | 万华化学集团股份有限公司 | A kind of preparation method of nylon powder |
-
2002
- 2002-08-01 CN CN 02133557 patent/CN1394670A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107057090A (en) * | 2017-04-27 | 2017-08-18 | 万华化学集团股份有限公司 | A kind of preparation method of nylon powder |
| CN107057090B (en) * | 2017-04-27 | 2019-07-23 | 万华化学集团股份有限公司 | A kind of preparation method of nylon powder |
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Addressee: Luo Haonan Document name: Notice of publication of application for patent for invention |
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