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Method for simultaneously and stably dispersing laminated nanosheets and spherical nanoparticles in oily medium and application thereof

A nanoparticle and layered nanotechnology, applied in the field of materials, can solve the problems of dangerous HF, needs further development, cannot form long-term stable emulsion, etc., and achieves the effect of good anti-friction performance

Active Publication Date: 2014-12-03
SHENZHEN NANKE NEW MATERIALS TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method has the following disadvantages: firstly, the method uses very dangerous HF, and secondly, because α-ZrP has a relatively hygroscopic property, zirconium hypophosphite stripped by HF will inevitably adsorb HF, and as we all know, HF can severely corrode metal materials, therefore, zirconium hypophosphite stripped by HF cannot be used in lubricating oil
This method is safer than the method of HF stripping, but there is still a disadvantage in this method: after mixing PIBSA-PAM, α-ZrP and lubricating oil, a long-term stable emulsion cannot be formed, so the phenomenon of liquid stratification will inevitably occur. This static instability reduces the effectiveness of α-ZrP nanosheets, and there are some application problems in practice
[0004] Therefore, the research on the application of zirconium hypophosphite in lubricating oil still needs further development

Method used

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  • Method for simultaneously and stably dispersing laminated nanosheets and spherical nanoparticles in oily medium and application thereof
  • Method for simultaneously and stably dispersing laminated nanosheets and spherical nanoparticles in oily medium and application thereof
  • Method for simultaneously and stably dispersing laminated nanosheets and spherical nanoparticles in oily medium and application thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0085] Embodiment 1: the synthesis of α-zirconium hypophosphite

[0086] 8.0g ZrOCl 2 .8H 2 O and 80.0ml of H with a concentration of 3.0mol / L, 6.0mol / L, 9.0mol / L and 12.0mol / L respectively 3 PO 4 (mass fraction 85%) was placed in a three-necked glass flask, and refluxed at 100°C for 24h. After the reaction was over, the reaction product was washed three times, and the product was collected by centrifugation to obtain α-ZrP (3M) and α-ZrP respectively. (6M), the product of α-ZrP (9M) and α-ZrP (12M). Among them, α-ZrP(3M), α-ZrP(6M), α-ZrP(9M) and α-ZrP(12M) are the concentration of reactant phosphoric acid respectively 3.0mol / L, 6.0mol / L, 9.0mol / L L, the product at 12.0mol / L. Then, dry the obtained product at 65°C for 24 hours, and then grind the dried product into α-ZrP fine powder. At 25°C, the density of the obtained α-ZrP solid powder is about 2.72g.cm -3 . The obtained α-ZrP fine powder is carried out XRD experiment, the XRD spectrogram of α-ZrP (theta-ZrP of dehy...

Embodiment 2

[0087] Embodiment 2: the synthesis of θ-zirconium hypophosphite

[0088] In a beaker, 3.116g of ZrOCl 2 .8H 2 O was dissolved in 200ml of deionized water, followed by 82.19ml of H in a round bottom flask 3 PO 4 (mass fraction 85%) mixed with 117.81ml deionized water. Then, under stirring conditions, the H 3 PO 4 The round-bottomed flask of the solution was placed in a constant temperature oil bath at 94°C, when H 3 PO 4 After the solution reached equilibrium at a temperature of 94°C, the ZrOCl 2 .8H 2 O solution was added dropwise to the 3 PO 4 The solution was placed in a round-bottomed flask, and then the resulting solution was stirred at 94 °C for 48 h. After the reaction is finished, the solution is filtered, and the solid product obtained by filtering is washed with a large amount of deionized water, that is, θ-ZrP. Next, the obtained θ-ZrP was dried in a desiccator for 72 hours at room temperature, and then the dried θ-ZrP was ground into a fine powder, and t...

Embodiment 3

[0089] Embodiment 3: the synthesis of gamma-zirconium hypophosphite

[0090] NaH 2 PO 4 .H 2 O (677g, 4.91mol) dissolved in distilled water (376ml) and 85% H 3 PO 4 (182.6g, 1.58mol) in a mixed solution. The resulting solution was then refluxed for 30 min, and then the ZrOCl concentration of 1mol / L was added into the refluxed solution 2 .8H 2 O (76g) solution was 238ml, and then the obtained colloid was refluxed for 72h. Subsequently, the refluxed colloidal solution was transferred to a hydrothermal reactor, and heated to 190° C. for 120 h. After the reaction, the white precipitate was filtered out and washed with 4mol / L HCl to remove sodium ions, and then washed with 0.2mol / L HCl 3 PO 4 Wash to remove chloride ions. Finally, it was washed with deionized water to obtain γ-ZrP. Next, the obtained γ-ZrP was dried in a desiccator at room temperature for 72 hours, and then the dried γ-ZrP was ground into a fine powder, and the particle size of the obtained γ-ZrP nanoshe...

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Abstract

The invention discloses a method for simultaneously and stably dispersing laminated nanosheets and spherical nanoparticles in an oily medium and application thereof. The method comprises the following steps: (1) mixing the laminated nanosheets with oil-soluble alkylamine, so as to obtain a first mixture; (2) mixing the spherical nanoparticles with an oily medium, so as to obtain a second mixture; and (3) mixing the first mixture and the second mixture with the oily medium, so as to obtain a third mixture. By adopting the method, the spherical nanoparticles can be effectively stabilized by the nanosheets, the laminated nanosheets and the spherical nanoparticles can be simultaneously and stably dispersed in the oily medium, a solution or micro emulsion obtained through dispersion is good in stability and free of sedimentation or layering phenomenon, and the method can be implemented simply, conveniently and rapidly.

Description

technical field [0001] The invention relates to the field of materials, in particular to a method for simultaneously stably dispersing layered nanosheets and spherical nanoparticles in an oily medium and an application thereof. More specifically, it relates to a method for simultaneously and stably dispersing layered nanosheets and spherical nanoparticles in an oily medium, a mixture containing layered nanosheets and spherical nanoparticles and its use in the preparation of lubricating oil and grease. Background technique [0002] α-zirconium hypophosphite (α-ZrP, Zr(HPO 4 ) 2 ·H 2 O), a layered structure is formed by connecting the zirconium atoms with the oxygen atoms in the phosphoric acid group, 3 oxygen atoms in each phosphoric acid group participate in the formation of the layered structure, and the remaining hydroxyl group extends towards the interlayer direction of the layered structure. The interaction between α-ZrP layers is weak, and under a certain shear stres...

Claims

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Application Information

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IPC IPC(8): C10M141/06C10M161/00C10M177/00C09K23/00
CPCC10M161/00C10M177/00C10M141/06C10M2215/04C10M2201/103C10M2201/062C10M2201/065C10M2215/08C10M2201/085C10M2201/05C10N2010/14C10N2010/08C10N2010/12C10N2020/071C10N2010/06C10N2020/06C10N2030/06C10N2010/04C10N2010/16C09K23/002
Inventor 雍怀松孙大陟
Owner SHENZHEN NANKE NEW MATERIALS TECH CO LTD
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