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Preparation method of fluorinated cellulose nanocrystalline lubricating grease thickening agent

A cellulose and nanocrystalline technology, applied in the field of materials, can solve the problems of weak fluorine base oil affinity, limited lubricating performance, and low oil content

Active Publication Date: 2021-10-29
WUHAN UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the traditional fluorine grease mostly uses polytetrafluoroethylene (PTFE) micron particles as the thickener, which has weak affinity with fluorine base oil, usually requires a larger mass fraction, lower oil content, and poor lubricating performance. Limited; while PTFE nanoparticles have better performance, but the preparation cost is higher

Method used

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  • Preparation method of fluorinated cellulose nanocrystalline lubricating grease thickening agent
  • Preparation method of fluorinated cellulose nanocrystalline lubricating grease thickening agent
  • Preparation method of fluorinated cellulose nanocrystalline lubricating grease thickening agent

Examples

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preparation example Construction

[0027] The preparation process of fluorinated cellulose nanocrystals of the present invention is as follows:

[0028]

[0029] Concrete preparation process is as follows:

[0030] 1) Disperse cellulose nanocrystals in N,N-dimethylformamide (DMF), add 4-dimethylaminopyridine (DMAP) and triethylamine (TEA), and ultrasonically disperse to obtain a suspension; the fiber The purity of the plain nanocrystal is higher than 97wt%, the crystallinity is 54%~88%, the length is 100~300nm, and the diameter is 10~20nm; the mass ratio of the amount of cellulose nanocrystal, 4-dimethylaminopyridine and triethylamine is 1:( 2~3): (1~2);

[0031] 2) Slowly add 2-bromoisobutyryl bromide (BiBB) solution dropwise to the obtained suspension under an inert atmosphere, heat up to 70-90°C for 24-36 hours after dropping, and centrifuge, wash and dialyze to obtain CNC-Br powder; The amount of 2-bromoisobutyryl bromide is 13 to 17 times the mass of cellulose nanocrystals;

[0032] 3) The obtained C...

Embodiment 1

[0037] A preparation method of a fluorinated cellulose nanocrystalline grease thickener and its application in fluorine grease, comprising the following steps:

[0038] (1) Weigh 1g of cellulose nanocrystal (CNC) and disperse it into a 250ml flask equipped with 120ml N,N-dimethylformamide (DMF), add 2.4g 4-dimethylaminopyridine (DMAP) and 1.32g Triethylamine (TEA) was ultrasonically dispersed in a cell pulverizer with 200W power for 10min to obtain a suspension;

[0039] (2) Under an inert atmosphere, 15 g of 2-bromoisobutyryl bromide (BiBB) was slowly added dropwise to the obtained suspension, and the temperature was raised to 70° C. for 24 h. After the reaction, it was centrifuged and washed twice with ethanol and deionized water, put into a dialysis bag and dialyzed for 3 days to obtain about 0.8 g of CNC-Br powder;

[0040] (3) Disperse 0.8g of CNC-Br powder into a 250ml flask containing 120ml of DMF, add 0.2g of copper bromide, 0.7g of N,N,N,N,N-pentamethyldiethylenetria...

Embodiment 2

[0047] The difference between this example and Example 1 is that the doping amount of fluorinated cellulose nanocrystals in step (5) is 20 wt%, and other steps, reagents and parameters are the same as in Example 1. In this embodiment, fluorine grease with higher viscosity can be obtained, which is used in heavy-load or low-speed working conditions. The fluorinated grafting of cellulose nanocrystals in this implementation case was confirmed by infrared spectroscopy and transmission electron microscope analysis; the friction and wear properties of the obtained grease were confirmed by a four-ball friction test (ASTMD266).

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Abstract

The invention discloses a preparation method of a fluorinated cellulose nanocrystal lubricating grease thickening agent. The method comprises the following steps: dispersing cellulose nanocrystal into N, N-dimethylformamide, adding 4-dimethylaminopyridine and triethylamine, and carrying out ultrasonic dispersion to obtain a suspension; slowly dropwise adding a 2-bromoisobutyryl bromide solution into the obtained suspension in an inert atmosphere, heating to 70-90 DEG C after dropwise adding, reacting for 24-36 hours, centrifuging, washing and dialyzing to obtain CNC-Br powder; dispersing the CNC-Br powder into N, N-dimethylformamide, adding copper bromide, N, N, N, N, N-pentamethyldiethylenetriamine, cuprous chloride and a monomer with a fluorine-containing group, removing oxygen in a reaction system, and carrying out an atom transfer radical polymerization reaction in an inert atmosphere; and removing impurities, and drying the extracted product to obtain the product. According to the preparation method, surface hydroxyl groups of the cellulose nanocrystals are replaced by Br-containing ester groups, and then monomers with fluorine-containing groups are added, so that fluorinated chains grow on the surfaces of the cellulose nanocrystals for grafting, and the lubricating grease thickening agent with excellent performance is obtained.

Description

technical field [0001] The invention belongs to the technical field of materials, and in particular relates to a preparation method of a fluorinated cellulose nanocrystal lubricating grease thickener. Background technique [0002] In industrial production, there will be friction between parts among the connection mechanism, power unit and transmission mechanism of many mechanical equipment. These friction and wear are considered to be one of the main factors causing energy consumption, material loss and mechanical equipment failure. According to statistics, friction consumes 1 / 3 of the world's primary energy, about 80% of mechanical parts fail due to wear, and more than 50% of mechanical equipment's vicious accidents are caused by lubrication failure. It can be seen that, The loss caused by friction and wear is very astonishing. Therefore, strengthening the lubrication of mechanical equipment will improve the friction resistance of friction pairs and the reliability of mecha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F251/02C08F220/24C10M147/04C10N30/06
CPCC08F251/02C10M147/04C10M2209/126C10N2030/06C10N2060/08C10N2020/06C08F220/24Y02P20/10
Inventor 李克葛月林宁俸颢
Owner WUHAN UNIV OF TECH
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