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Liquid phase nano powder body and preparation method of nano particle agglutinative structure material

A nano-powder and nano-particle technology, which is applied in the direction of nano-structure manufacturing, chemical methods for making liquids react with liquids, nano-technology, etc., can solve the problems that are not conducive to equipment maintenance and cleaning parameter regulation, hard agglomeration of nanoparticles is difficult to eliminate, and difficult Effectively control particle size and other issues, achieve the effect of improving equipment maintenance and cleaning performance, eliminating hard agglomeration, and being suitable for large-scale production

Inactive Publication Date: 2003-03-05
UNIV OF SCI & TECH LIAONING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the preparation of nanoparticles and materials with nanoparticle aggregation structure by this process has the advantages of simple operation, low cost and high yield, it is recognized that this method has three disadvantages: ① difficult to control the particle size; ② difficult to control the particle size very small; ③ hard agglomeration between nanoparticles of powder is difficult to eliminate
The disadvantage of this method is: a carrier solution that has nothing to do with the chemical reaction is added, and the reactant solution is added in a periodic intermittent pulse. These measures complicate the operation.
The disadvantage of this method is: the solution relies on supergravity to pass through the packed bed, and the strength to quickly form a fresh interface between the two reactants is not enough, so it is difficult to effectively control the particle size
[0005] In the CN01106279.7 patent application, the applicant has provided a non-stirred tank method: the reaction solution is continuously fed into the dynamic, fast and orderly mixed reaction precipitator of the micro-liquid mass, and the micro-liquid mass is quickly mixed in the form of turbulent flow. Reaction and precipitation, the reaction zone is arranged in an orderly manner along the direction of the liquid flow, the precipitation slurry continuously flows out of the mixed reaction precipitation equipment, enters the cleaning and filtration process, and then performs other post-processing links (such as drying, heat treatment, crushing, etc.), this method The prepared nanoparticles have a small and uniform particle size, and the hard agglomeration between particles is eliminated. The disadvantage of this method is that a dynamic rotor is used, which is not conducive to equipment maintenance and cleaning and the simplification of parameter regulation.

Method used

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  • Liquid phase nano powder body and preparation method of nano particle agglutinative structure material
  • Liquid phase nano powder body and preparation method of nano particle agglutinative structure material
  • Liquid phase nano powder body and preparation method of nano particle agglutinative structure material

Examples

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Effect test

Embodiment 1

[0031] Embodiment 1: Weigh 773.4 grams of zirconium oxychloride (ZrOCl 2 ·8H 2 O, molecular weight 322.25, purity ≥ 99%), made into ZrOCl with a concentration of 0.8mol / L 2 3000ml aqueous solution is called A solution. Another 375ml ammonia water (NH 3 Concentration is 25%) add twice distilled water, add the ethanol (95%) 2100ml that is used as dispersant again, be mixed with 3000ml aqueous solution, be called B solution. The temperature is room temperature 20°C, according to figure 1 Process flow, let A and B solutions pass through Figure 2-a The tubular jet mixer is used for mixing, reaction and precipitation, and the pH value is adjusted with ammonia water, and the final pH value is 7-8. The inner diameter of the tubular jet mixer is 10mm, the inner diameter of the injection hole is 1mm, the flow rates of A and B solutions are both 200L / h, and the injection inlet pressure of A solution is 100kg / cm 2 . The slurry containing the precipitate enters the continuous proc...

Embodiment 2

[0032] Embodiment 2: weigh 333.6 grams of ZnCl 2 , add secondary water to make ZnCl 2 3000ml of an aqueous solution with a concentration of 0.8mol / L is called A solution, and the temperature is 70°C. Get 375ml of ammonia water (25%), then add 900ml of ethanol (95%) used as a dispersant to prepare NH 3 Concentration is 3000ml of ethanol aqueous solution of 0.8mol / L, temperature is 30 ℃. according to figure 1 Process flow, let A and B solutions pass through Figure 2-a The tubular jet mixer is used for mixing, reaction and precipitation, and the pH value is adjusted with ammonia water so that the final pH value is 7-8. The inner diameter of the mixing reactor is 10mm, the inner diameter of the injection hole is 1mm, the flow rate of each solution entering the mixing reactor is 150L / h, and the inlet pressure of the injection solution is 90kg / cm 2 . The slurry containing the precipitate enters the continuous processing equipment for cleaning and filtration, and then undergoe...

Embodiment 3

[0033] Embodiment 3: weigh 441.6 grams of BaCl 2 , add secondary water, add 900ml ethanol, and prepare BaCl 2 3000ml of an aqueous solution with a concentration of 0.6mol / L is called A solution at a temperature of 20°C. Weigh 156.6 g NH 4 HCO 3 , add secondary water, get 180ml ammoniacal liquor (25%), add the 1200ml ethanol (95%) that is used as dispersant again, be mixed with B solution 3000ml, temperature 20 ℃. according to figure 1 Process flow, let A and B solution be fed continuously Figure 2-a Tube jet mixer for mixing, reaction and precipitation. Adjust the amount of ammonia water in liquid B so that the pH value of the mixed sedimentation liquid is 7-8. The inner diameter of the tubular jet mixer is 10mm, the inner diameter of the jet hole is 1mm, and the inlet pressure of the jet solution is 100kg / cm 2 , the flow rate of each solution is 160L / h. The slurry containing the precipitate enters the continuous processing equipment for cleaning and filtration, and t...

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Abstract

The present invention discloses a nano powder body and nano particle aggregative structure material preparation method. Said method can regulate and control grain size of nano particle, can make saidmaterial possess uniform grain size, good dispersion property and high yield. Its equipment is simple, and consumption is less. Said method mainly includes the following steps: continuously feeding reactant solution into quickly-mixing reaction precipitation equipment, and continuously discharging the precipitate-contained slurry material from said equipment, then making the slurry material undergo the processes of cleaning, filtering or ageing, cleaning and filtering, drying, heat treatment, pulverizing and packaging. Said method can be used for producing various nano powder body and nano particle aggregative structure materials.

Description

technical field [0001] The invention relates to a liquid-phase chemical reaction precipitation method for preparing nanoparticle powder and a material with nanoparticle aggregation structure. Background technique [0002] The common process characteristics of the liquid phase precipitation method are: using a stirred tank for the mixed reaction, at least one reactant solution is gradually added by dropping, inflowing or spraying over a long period of time. Although the preparation of nanoparticles and materials with nanoparticle aggregation structure by this process has the advantages of simple operation, low cost and high yield, it is recognized that this method has three disadvantages: ① difficult to control the particle size; ② difficult to control the particle size ③ The hard agglomeration between the nanoparticles of the powder is difficult to eliminate. The root cause of the disadvantage of the stirred tank process is that one of the reactant solutions is added for to...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J19/00C01F11/18B01F3/08C01G1/02C01G9/00C01G25/02
CPCY10S977/775C01G1/02C01P2006/22C01P2004/64B82Y30/00C01P2004/03C01P2004/52Y10S977/773Y10S977/777B82B3/00B82Y40/00
Inventor 周英彦高首山王开明温传庚李晓奇
Owner UNIV OF SCI & TECH LIAONING
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