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A kind of oil-soluble nanometer copper and preparation method thereof

A nano-copper, oil-soluble technology, applied in the direction of nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve the problem of lack of high-concentration, high-efficiency, high-yield preparation methods, increase the difficulty and cost of purification, The problem of low synthetic yield is to achieve the effect of reducing cost, eliminating reaction interface and simplifying production process

Active Publication Date: 2021-01-26
HENAN UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method technique is simple, productive rate is high, but still has deficiencies: 1. reactant concentration is low and causes synthetic yield not high; Difficulty and cost of purification; 3. The non-polar organic solvent accounts for 10-90% of the total volume of the reaction system. The greater the concentration of the non-polar organic solvent, the greater the risk, and it is not conducive to environmental protection
This method effectively solves the bottleneck of poor compatibility between copper nanoparticles and water phase, but its reaction system is highly alkaline (pH 9-14). If it is separated, it needs to consider the subsequent purification and wastewater treatment; , there will be impurities such as organic amines in the solution; moreover, the low concentration of the reactant makes the yield of the product low
[0005] In summary, currently, surface-modified copper nanoparticles are synthesized in a relatively low concentration reaction system, and there is a lack of high-concentration, high-efficiency, and high-yield preparation methods.
Moreover, the synthesis of surface-modified copper nanoparticles is based on the application scenario. The choice of different modifiers leads to great differences in the reaction system. For example, water-soluble nano-copper is synthesized in the water phase, and oil-soluble nano-copper is synthesized in the oil / water two-phase There is no method for synthesizing oil-soluble nano-copper in the aqueous phase system

Method used

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  • A kind of oil-soluble nanometer copper and preparation method thereof
  • A kind of oil-soluble nanometer copper and preparation method thereof
  • A kind of oil-soluble nanometer copper and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Weigh 9.8g (0.1mol) of copper hydroxide into a 250mL three-neck flask, add 50mL of deionized water and 5mL of ethanol, stir well, and add 38.5mL of diisooctyl dithiophosphoric acid (0.1mol) at 30°C, After reacting for 0.5h, a brown-green oil-soluble nano-copper intermediate emulsion was obtained; then ammonia water (mass concentration: 20%) was added to the reaction system to adjust the pH to 7. At this time, 6.1mL of hydrazine hydrate (mass concentration: 80% %, 0.1mol) was slowly added into a three-necked flask under stirring, and reacted at 30°C for 2 hours to obtain a dark reddish-brown reaction solution, which was distilled under reduced pressure to obtain oil-soluble nano-copper.

[0033] The total volume of the reaction system is about 110mL, and the yield of oil-soluble nano-copper is 41.6g (about 40mL). The particle size of oil-soluble nano-copper is 6-10nm, see the transmission electron micrograph figure 1 , the photo of the dispersion of the obtained oil-sol...

Embodiment 2

[0035] Weigh 8.0g of copper oxide (0.1mol) into a 250mL three-neck flask, add 33mL of deionized water and 6mL of methanol, stir well, and add 46.2mL of diisooctyl dithiophosphoric acid (0.12mol) at 25°C, and react 1h, the brown-green oil-soluble nano-copper intermediate emulsion was obtained; then ammonia water (mass concentration: 20%) was added to the reaction system, the pH was adjusted to 9, and the temperature was raised to 60°C. At this time, 18.4mL of formaldehyde (mass concentration 40%, 0.2mol) was slowly added into a three-necked flask under stirring, and a deep reddish brown reaction solution was obtained after 4 hours of reaction. The reaction solution was distilled under reduced pressure to obtain oil-soluble nano-copper.

[0036] The particle size of oil-soluble nano-copper is 3-7nm, and its transmission electron micrograph is shown in image 3 , the lubrication performance test results see Figure 4 . Depend on Figure 4It can be seen that oil-soluble nano-co...

Embodiment 3

[0038] Weigh 7.2g of cuprous oxide (0.05mol), 4.9g of copper hydroxide (0.05mol), 0.1mol in total, into a 250mL three-neck flask, add 40mL of deionized water, 10mL of methanol, 1mL of ether, stir well, and place at 40°C Add 45.2mL di(2-ethyl-hexyl)phosphoric acid (0.135mol) under stirring and react for 0.5h to obtain a brown oil-soluble nano-copper intermediate emulsion; then add concentrated ammonia water (mass concentration: 25% ) adjust the pH to 8, raise the temperature to 50°C, and add 12.5mL reducing agent mixture dropwise under stirring ), stirring and reacting for 4 hours to obtain a dark reddish-brown reaction liquid, and distilling the reaction liquid under reduced pressure to obtain oil-soluble nano-copper.

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Abstract

The invention belongs to the technical field of nanomaterial preparation, and in particular relates to an oil-soluble nanometer copper and a preparation method thereof. The preparation method uses high-concentration heteroatom-free copper oxides and hydroxides as precursors, and uses a one-step method to reduce the intermediates formed by copper precursors and modifiers in an aqueous system to efficiently prepare oil-soluble nano-copper, including the following Steps: 1) Mix the copper precursor and the mixed solvent evenly, and add an organic modifier at 20-80°C, and react for 0.5-3h to obtain an oil-soluble nano-copper intermediate emulsion; 2) Adjust the oil in step 1) The pH of the soluble nano-copper intermediate emulsion is 7-9, adding a reducing agent at 20-85°C for a reduction reaction of 0.5-24h to obtain an oil-soluble nano-copper reaction liquid; 3) reacting the oil-soluble nano-copper in step 2) The liquid is distilled under reduced pressure to obtain oil-soluble nano-copper. The invention is a simple, green and environment-friendly production method and recycling process, which has the characteristics of energy saving, safety and high output, and produces no three wastes at the same time.

Description

technical field [0001] The invention belongs to the technical field of nanomaterial preparation, and in particular relates to a preparation method for one-step synthesis of oil-soluble nanometer copper. Background technique [0002] At the nanoscale, materials exhibit distinct physicochemical properties from bulk materials. In recent decades, the synthesis of nanomaterials has been one of the research hotspots in the field of nanoscience and technology. Copper-based nanomaterials have attracted the attention of scientists from all over the world with their excellent performance and potential application prospects. Copper nanoparticles can replace precious metals in conductive materials, lubricating oil additives, etc., greatly reducing costs. However, nano-copper is easily oxidized and has problems such as poor stability and dispersion. Therefore, the preparation of copper nanoparticles with good dispersion and stability, and controllable shape and size has become a resea...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B22F9/24B22F1/00B82Y30/00B82Y40/00
CPCB22F9/24B82Y30/00B82Y40/00B22F1/054
Inventor 牛利永李小红田路露张治军
Owner HENAN UNIVERSITY