Biodegradable grease composition and its preparation method
A lubricating grease composition and biodegradation technology, applied in the field of lubricating grease, can solve the problems of rare and unsatisfactory lubricating grease degradation effects, and achieve excellent mechanical stability, excellent anti-oxidation effect, and simple preparation method
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[0044] The present invention also provides a preparation method of the above-mentioned compound of formula I and a method of preparing a lubricating grease composition by using the compound of formula I.
[0045] The preparation method of formula I compound comprises the steps:
[0046] (1) tartaric acid and amino acid ester hydrochloride, that is, the following formula II compound is mixed in the first solvent to carry out a reaction, that is, the first intermediate product is obtained by amidation reaction, wherein R 3 Be methyl, ethyl, tert-butyl or benzyl, for example the compound of formula II can be L-valine methyl ester hydrochloride, L-alanine methyl ester hydrochloride, L-alanine ethyl ester salt salt, L-valine ethyl ester hydrochloride, etc.
[0047]
[0048] In some embodiments, the first solvent is selected from one of dichloromethane, chloroform, acetone, ethyl acetate, N,N-dimethylformamide (DMF), dimethylsulfoxide (DMSO) and acetonitrile or more, preferably...
preparation example 1
[0070] This preparation example is used to illustrate the biodegradation accelerator of the present invention, that is, 2,2'-((2-tetradecyloxy)-1,3,2-dioxaphospholane-4,5-di Carbonyl)-diamino-dipropionic acid (see structural formula I-c) synthetic process.
[0071]
[0072] 1) Add 100mL DMF, tartaric acid (33.3mmol, 5g), L-alanine methyl ester hydrochloride (73.2mmol, 10.21g), 1-hydroxybenzotriazole (79.9mmol, 10.8 g), pyridine (8 mL), cooled to 0°C, added DCC (79.9 mmol, 16.5 g), and reacted overnight. The reaction mixture was suction-filtered, the solid was washed with 300 mL of ethyl acetate, the organic phases were combined, washed twice with saturated sodium bicarbonate solution, twice with 10% hydrochloric acid solution, once with saturated brine, dried over anhydrous magnesium sulfate for 2 h, filtered, Spin dry to obtain a white solid.
[0073] 2) Phosphorus trichloride (40mmol, 5.48g) was dissolved in 5mL of n-hexane, cooled to 4°C, triethylamine (40mmol, 4.04g) ...
Embodiment 1
[0081] In this embodiment, each raw material component is: lubricating base oil (500SN, Thailand) 828g (viscosity at 100°C is 10.9mm 2 / s), lithium hydroxide 8.3g, dodecyl hydroxystearic acid 103.5g; 2,6-di-tert-butyl-p-cresol 12g; barium petroleum sulfonate 9g; dialkyl dithiocarbamate 8g; The biodegradation accelerator 8g of preparation example 1;
[0082] First, take 500g of base oil and 103.5g of lauryl hydroxystearic acid into the fat making kettle, mix and stir evenly. When the temperature rises to 88°C, add 80.7g of lithium hydroxide aqueous solution (including 8.3g of lithium hydroxide and 72.4g of water) to carry out saponification reaction for 30min;
[0083] Then, raise the temperature to 130°C for dehydration reaction, add 12g of 2,6-di-tert-butyl-p-cresol and continue to heat up to 215°C for 15 minutes of high-temperature refining;
[0084] After high-temperature refining, add the remaining 278g of base oil and cool down to 120°C, then add 9g of barium petroleum ...
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