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Application of lactam as solvent in nano-grade material preparation

A nanomaterial and lactam technology, applied in the field of nanomaterials, can solve the problems of narrow particle size distribution, affecting the subsequent application of synthetic nanoparticles, and good dispersibility.

Active Publication Date: 2013-07-17
SHANGHAI GENIUS ADVANCED MATERIAL (GRP) CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In view of the disadvantages of solid phase method, gas phase method and common liquid phase method in the prior art that are not conducive to the preparation of nanomaterials with ultrafine particle size, narrow particle size distribution and good dispersion; Subsequent application of synthetic nanoparticles, the purpose of the present invention is to provide a low-toxicity lactam as a solvent in the preparation of nanomaterials

Method used

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  • Application of lactam as solvent in nano-grade material preparation
  • Application of lactam as solvent in nano-grade material preparation
  • Application of lactam as solvent in nano-grade material preparation

Examples

Experimental program
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Effect test

Embodiment 1

[0076] Synthesis of Nano Magnesium Hydroxide by Precipitation Method Using Caprolactam as Solvent

[0077] Take 20.3g MgCl 2 ·6H 2 O was added to 100 g of molten caprolactam (caprolactam purity ≥ 80%, water content ≤ 20%), and stirred at 100°C for 30 min to fully dissolve the magnesium chloride. 10 g of ammonia water (containing 26% ammonia) was quickly added under stirring conditions, and the temperature was kept at 100° C. for 24 hours. The obtained mixture was centrifugally washed three times with deionized water, each time with 200 g of water, fully dried and pulverized to obtain nanometer Mg(OH) 2 Powder.

[0078] figure 1 It is caprolactam as the carbon nuclear magnetic resonance spectra before and after solvent use ( 13 C-NMR), the use solvent is deuterated chloroform, and caprolactam remains unchanged as the collection of spectra before and after solvent use, shows that the caprolactam solvent can be recycled. figure 2 It is the synthetic nanometer Mg(OH) of pre...

Embodiment 2

[0080] Synthesis of Nanometer Neodymium Hydroxide by Precipitation Method Using Caprolactam as Solvent

[0081] Take 10.96g Nd(NO 3 ) 3 ·6H 2 O was added to 100g of molten caprolactam (caprolactam purity ≥ 80%, moisture ≤ 20%), stirred at 200°C for 30min, and Nd(NO 3 ) 3 ·6H 2 O is fully dissolved. Add 3g NaOH quickly under stirring condition, and keep the temperature at 200°C for 24h. The obtained mixture was centrifugally washed three times with deionized water, each time with 200 g of water, fully dried and pulverized to obtain nanometer Nd(OH) 3 Powder. Figure 4 It is the transmission electron microscope (TEM) picture of the synthetic nanometer Nd(OH) powder of present embodiment method, and observation result shows that Nd(OH) 3 The powder is composed of uniformly dispersed rod-shaped nanoparticles, the average length of the nanoparticles is about 40nm, and the average diameter is about 7nm.

Embodiment 3

[0083] Synthesis of Nano-sized Aluminum Hydroxide / Yttrium Hydroxide Composite by Precipitation Method Using Caprolactam as Solvent

[0084] Take 3.83g Y(NO 3 ) 3 ·6H 2 O and 4.02g AlCl 3 9H 2 O (the molar ratio is [Y 3+ ] / [Al 3+ ]=3 / 5) was added to 100g molten caprolactam (caprolactam purity ≥ 80%, moisture ≤ 20%), stirred at 200°C for 30min, and Y(NO 3 ) 3 ·6H 2 O and AlCl 3 9H 2 O is fully dissolved. Add 8g of NaOH quickly under stirring condition, and keep the temperature at 200°C for 24h. The mixture obtained was washed three times with deionized water, 200g of water each time, fully dried and pulverized to obtain nanometer Al(OH) 3 / Y(OH) 3 Powder. Figure 5 It is the synthetic nanometer Al(OH) of present embodiment method 3 / Y(OH) 3 The TEM picture of the powder shows that the product is composed of small particles with a diameter of about 5nm.

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Abstract

Disclosed is an application of lactam as a solvent in nanomaterial preparation. The preparation method comprises a precipitation method, a sol-gel method or a high-temperature pyrolysis method. The method achieves recycling utilization of the lactam solvent, which meets the requirements of environmental protection.

Description

technical field [0001] The invention belongs to the technical field of nanometer materials, and relates to the application of a lactam as a solvent in the preparation of nanometer materials. Background technique [0002] Nanomaterials refer to materials that have at least one dimension in the three-dimensional space in the nanoscale range (1-100nm) or are composed of them as basic units. Nanoscale effects often show different melting points, magnetism, optics, thermal conductivity, and electrical conductivity from bulk materials, so they can have broad application prospects in optoelectronic materials, ceramic materials, sensors, semiconductor materials, catalytic materials, and medical treatment. [0003] At present, the methods for synthesizing nanomaterials mainly include three categories: solid-phase method, liquid-phase method and gas-phase method. Due to the large surface energy of nanomaterials, it is difficult for nanomaterials obtained by various solid-phase synthe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F5/20C01F17/00C01F7/02C01G5/00C01G5/02C01G9/02C01G9/04C01G9/08C01G3/02C01G49/08C01G49/06C01G23/053C01F5/24C01F11/46C01B19/04C01B33/12C03C17/06B22F9/24B01J23/44B82Y30/00B82Y40/00C01F7/162C01F7/785C01F17/224
CPCC01G23/053C01G5/00C01G49/06C01F5/20C01G49/08C01B33/14C01B33/12C01G9/02C01G3/02C01G23/0532C01G23/0536C01G5/02C01G9/08C01G11/00C01P2002/72C01P2002/86C01P2004/03C01P2004/04C01P2004/64C01P2006/42C01F7/34C01B19/007C01B33/18C01F5/24C01F7/162C01F11/462C01F17/224C01F7/785C01B19/04C01F5/14C22B3/04C22B11/04C22B15/0065
Inventor 夏厚胜杨桂生
Owner SHANGHAI GENIUS ADVANCED MATERIAL (GRP) CO LTD
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