Organic bentonite lubricating grease and preparation method thereof

Abstract

The invention provides organic bentonite lubricating grease and a preparation method thereof. The organobentonite lubricating grease comprises the following components based on the total weight of the lubricating grease: 0.1%-5% of a benzotriazole derivative, 1%-10% of an anti-wear reagent at extreme pressure, 5%-30% of organobentonite and 60%-90% of lubricant base oil, the structure of the benzotriazole derivative is as shown in formula (I), and the definition of each group is as shown in the specification. The organobentonite lubricating grease has excellent oxidation resistance and rust resistance, also has good extreme pressure property and excellent mechanical stability, and can be qualified for harsh working conditions such as high temperature, high speed, high load, wateriness and the like.

Description

TECHNICAL FIELD

[0001] The present application relates to a kind of greases, in particular to a kind of bentonite grease with excellent antioxidant and rust-proof performance and its preparation method. BACKGROUND

[0002] Greases are necessary working media in the normal operation of mechanical equipment and the process of material manufacturing and processing. Organic bentonite grease is an important non-soap high-temperature grease obtained by thickening lubricating oil base oil with organic modified bentonite. It has a higher drop point than lithium-based grease and is more suitable for use at high temperatures. Due to its relatively simple preparation process, even without heating, and lower cost, bentonite grease is widely used in the lubrication of aircraft, automobiles, metallurgical equipment, heavy-duty equipment, and other machinery.

[0003] In recent years, with the progress of industrial technology, greases are often required to have excellent antioxidant, rust-proof, and extreme pressure performance. However, the introduction of extreme pressure additives often causes rust problems, and careful balancing of the extreme pressure and rust-proof performance of the product is often required during actual formulation development. Therefore, developing a grease with excellent antioxidant, extreme pressure, and rust-proof performance has been the direction of research and development for researchers. SUMMARY

[0004] The present application provides an organic bentonite grease and its preparation method.

[0005] The organic bentonite grease of the present application includes the following components based on the total weight of the grease: 0.1% to 5% of a benzotriazole derivative, 1% to 10% of an extreme pressure anti-wear agent, 5% to 30% of organic bentonite, and 60% to 90% of lubricating oil base oil. The structure of the benzotriazole derivative is shown in formula (I):

[0006]

[0007] In formula (I), n is an integer between 1 and 10; R1 group is selected from C 1-20 linear or branched alkylene; R2 groups in n repeating units are the same or different from each other and are each independently selected from C 1-20 linear or branched alkylene; R3 group is selected from H and C 1-20 linear or branched alkyl; A groups in n repeating units are the same or different from each other and are each independently selected from groups shown in formula (II), groups shown in formula (III);

[0008]

[0009] * in formula (II) and formula (III) represents the bonding end to formula (I);

[0010] each of the R4 group and the R5 group is independently selected from the group consisting of H and C1-6 alkyl 1-10 linear or branched alkyl group.

[0011] According to the present application, preferably, in formula (I), n is an integer between 1 and 5, the R1 group is selected from the group consisting of C1-6 alkyl and C1-6 alkoxy, the R2 group in each of the n repeating units is independently selected from the group consisting of C1-6 alkyl and C1-6 alkoxy, the R3 group is selected from the group consisting of H and C1-6 alkyl, the R4 group and the R5 group are selected from the group consisting of H and C1-6 alkyl. 1-10 linear or branched alkylene group, the R2 group in each of the n repeating units is independently selected from the group consisting of C1-6 alkyl and C1-6 alkoxy 1-10 linear or branched alkylene group, the R3 group is selected from the group consisting of H and C1-6 alkyl 1-10 linear or branched alkyl group, each of the R4 group and the R5 group is independently selected from the group consisting of H and C1-6 alkyl 1-4 linear or branched alkyl group.

[0012] According to the present application, further preferably, in formula (I), n is an integer between 1 and 3, the R1 group is selected from the group consisting of C1-6 alkyl and C1-6 alkoxy, the R2 group in each of the n repeating units is independently selected from the group consisting of C1-6 alkyl and C1-6 alkoxy, the R3 group is selected from the group consisting of H and C1-6 alkyl, the R4 group and the R5 group are selected from the group consisting of H and C1-6 alkyl. 1-8 linear or branched alkylene group, the R2 group in each of the n repeating units is independently selected from the group consisting of C1-6 alkyl and C1-6 alkoxy 1-8 linear or branched alkylene group, the R3 group is selected from the group consisting of H and C1-6 alkyl 1-8 linear or branched alkyl group, the R4 group and the R5 group are selected from the group consisting of t-butyl or the R4 group is selected from the group consisting of t-butyl and the R5 group is selected from the group consisting of H.

[0013] According to the present application, examples of the benzotriazol derivative that can be mentioned include one or more of the following structural compounds:

[0014]

[0015] According to the present application, the method for producing the benzotriazol derivative includes the following steps:

[0016] (1) reacting a compound represented by formula (α) with a peroxide;

[0017]

[0018] in formula (α), n is an integer between 1 and 10, the R1 group is selected from the group consisting of C1-6 alkyl and C1-6 alkoxy, the R2 group in each of the n repeating units is independently selected from the group consisting of C1-6 alkyl and C1-6 alkoxy, the R3 group is selected from the group consisting of H and C1-6 alkyl, the R4 group and the R5 group are selected from the group consisting of H and C1-6 alkyl. 1-20 linear or branched alkylene group; the R2 group in each of the n repeating units is the same as or different from each other, and is independently selected from the group consisting of C1-6 alkyl and C1-6 alkoxy 1-20 linear or branched alkylene group; the R3 group is selected from the group consisting of H and C1-6 alkyl 1-20 linear or branched alkyl group; the A" group in each of the n repeating units is selected from the group consisting of -CH=CH-; each of the R4 group and the R5 group is independently selected from the group consisting of H and C1-6 alkyl 1-10 linear or branched alkyl group;

[0019] (2) subjecting the reaction product of step (1) to a hydrolysis reaction;

[0020] (3) reacting the hydrolysis reaction product of step (2) with a compound represented by formula (β), and collecting the product;

[0021]

[0022] X is selected from the group consisting of OH, F, Cl, Br, I.

[0023] According to the present application, preferably, in formula (a), n is an integer between 1 and 5, the R1group is selected from the group consisting of C 1-10 linear or branched alkylene, the R2group in each of the n repeating units is independently selected from the group consisting of C 1-10 linear or branched alkylene, the R3group is selected from the group consisting of H and C 1-10 linear or branched alkyl, the R4group, the R5group is independently selected from the group consisting of C 1-4 linear or branched alkyl.

[0024] According to the present application, further preferably, in formula (a), n is an integer between 1 and 3, the R1group is selected from the group consisting of C 1-8 linear or branched alkylene, the R2group in each of the n repeating units is independently selected from the group consisting of C 1-8 linear or branched alkylene, the R3group is selected from the group consisting of H and C 1-8 linear or branched alkyl, the R4group, the R5group is selected from the group consisting of C

[0025] According to the present application, in step (1), the compound represented by formula (a) can be selected from cardanol, alkylated cardanol, which can be obtained by reacting cardanol with an alkylating agent, for example, t-butylated cardanol can be obtained by reacting cardanol with t-butyl chloride.

[0026] According to the present application, in step (1), the peroxide is preferably one or more of hydrogen peroxide, peroxyformic acid, peroxyacetic acid, peroxy sulfonic acid, meta-chloro peroxy benzoic acid, t-butyl hydroperoxide, t-butyl peroxy acetate, methyl ethyl ketone peroxide, dibenzoyl peroxide and cyclohexanone peroxide, more preferably one or more of hydrogen peroxide, peroxyformic acid, peroxyacetic acid and peroxy sulfonic acid.

[0027] According to the present application, the reaction product of step (1) can be obtained by reacting cardanol or alkylated cardanol with a peroxide, or by first reacting cardanol with a peroxide and then with an alkylating agent.

[0028] According to the present application, in step (2), the hydrolysis reaction is a hydrolysis reaction of the reaction product of step (1) with water, and the amount of water used can generally be 20% to 200% of the mass of the reaction product of step (1).

[0029] According to the present application, in step (3), the compound represented by formula (β) can be one or more selected from the group consisting of benzotriazole-5-carboxylic acid, benzotriazole-5-carbonyl fluoride, benzotriazole-5-carbonyl chloride, benzotriazole-5-carbonyl bromide and benzotriazole-5-carbonyl iodide, preferably benzotriazole-5-carboxylic acid.

[0030] According to the present application, the molar ratio between the compound represented by formula (α) and the compound represented by formula (β) is preferably 1:0.5-10:0.5-10, more preferably 1:1-5:1-5.

[0031] According to the present application, the reaction temperature of step (1) is preferably 50-100°C, more preferably 60-90°C; the reaction temperature of step (2) is preferably 50-150°C, more preferably 70-100°C; and the reaction temperature of step (3) is preferably 50-200°C, more preferably 70-160°C.

[0032] According to the present application, the reaction time of step (1), step (2) and step (3) is generally longer the better, in general, the reaction time of step (1) is preferably 1-10h, more preferably 3-5h; the reaction time of step (2) is preferably 0.5-10h, more preferably 1-3h; and the reaction time of step (3) is preferably 1-10h, more preferably 3-6h.

[0033] According to the present application, a catalyst can be added in step (1), the catalyst is preferably an acidic catalyst, for example, one or more selected from the group consisting of concentrated sulfuric acid, zinc chloride, aluminum chloride, benzene sulfonic acid and titanium acid ester, the amount of the catalyst added is preferably 0.01%-3% of the compound represented by formula (α). After the reaction of step (1) is completed, the catalyst can be removed by means of alkali washing and / or water washing.

[0034] According to the present application, a catalyst can be added in step (2), the catalyst can be selected from an acidic catalyst or an alkaline catalyst, for example, one selected from the group consisting of concentrated sulfuric acid, concentrated hydrochloric acid, concentrated nitric acid, sodium hydroxide and potassium hydroxide, preferably concentrated sulfuric acid, the amount of the catalyst added is preferably 0.5%-10% of the sum of the mass of the compound represented by formula (α) and the peroxide in step (1). After the reaction of step (2) is completed, the catalyst can be removed by means of alkali washing (if an acidic catalyst is used), acid washing (if an alkaline catalyst is used) and water washing.

[0035] According to the present application, a catalyst can be added in step (3), the catalyst is preferably an acidic catalyst, for example, one or more selected from the group consisting of concentrated sulfuric acid, zinc chloride, aluminum chloride, benzene sulfonic acid and titanium acid ester, the amount of the catalyst added is preferably 0.5%-10% of the compound represented by formula (α). After the reaction of step (3) is completed, the catalyst can be removed by means of alkali washing and / or water washing.

[0036] According to the present application, the reaction steps (1), (2), (3) can be carried out in the presence of a diluent and / or a solvent, or without using a diluent and / or a solvent.

[0037] According to the present application, the diluent can be selected from one or more of API Group I, II, III, IV and V base oils, and common commercial products or grades include 150SN, 200SN, 350SN, 500SN, 650SN, 150BS, HVI-100, HVI-150, HVI-200, HVI-350, HVI-400, HVI-500, HVI-150BS, PAO4, PAO6, PAO8, PAO10, alkylbenzene, alkylnaphthalene, etc.

[0038] According to the present application, the solvent can be selected from water, C 6-20 one or more of aromatic hydrocarbons (such as benzene, toluene, xylene and cumene), C 6-10 one or more of alkanes (such as n-hexane, cyclohexane and petroleum ether), solvent naphtha, acetone, dimethylformamide. These solvents can be used singly, or two or more in combination. The solvent can be removed after the reaction is completed, using a method known to those skilled in the art, for example under normal or reduced pressure.

[0039] According to one particular embodiment of the present application, the diluent and / or solvent can be added at any stage of the reaction steps, in an amount according to conventional use in the art, and is not particularly limited.

[0040] According to the present application, the step (1), step (2), step (3) can be carried out under the protection of an inert gas atmosphere. As the inert gas, for example, nitrogen and argon, etc. can be cited, and is not particularly limited.

[0041] According to the present application, by the aforementioned production method, as a reaction product, a single compound can be produced, or a mixture of a plurality of compounds can be produced, or a mixture of one or more compounds and the aforementioned diluent (if used) can be produced. These reaction products are all intended by the present application, and the difference in the form of existence does not affect the realization of the effect of the present application. Therefore, these reaction products are collectively referred to as benzotriazole derivatives without distinction in the context of the present specification. In view of this, according to the present application, there is no absolute necessity to further purify the reaction product, or to further separate a benzotriazole derivative of a specific structure from the reaction product. Of course, the purification or separation is preferred for further improvement of the intended effect of the present application, but is not essential to the present application. Nevertheless, as the purification or separation method, for example, a method of purifying or separating the reaction product by column chromatography or preparative chromatography can be mentioned.

[0042] According to the present application, the extreme pressure anti-wear agent can be selected from one or more of sulfurized olefins, phosphoric acid esters, phosphorous acid esters, amino thioesters, and dialkyldithiocarbamic acid salts, for example, one or more of sulfurized isobutylene, trimethylphenyl phosphate, and di-n-butyl phosphite.

[0043] According to the present application, the organobentonite can be selected from existing commercial products, for example, an organobentonite prepared using an amine-based organic cation, a polyamine, a heterocyclic amino compound, or a fatty acid amino amide as a coating agent. The organobentonite can also be prepared by a method of the prior art, for example, by first modifying bentonite to a sodium type, then adding a coating agent to adhere to the end face of the crystal structure of the bentonite, followed by filtration, washing, drying, and pulverization to obtain an organobentonite.

[0044] According to the present application, the lubricating oil base oil can be one or more of mineral oil, vegetable oil, ester synthetic oil, and poly-alpha-olefin synthetic oil, preferably a lubricating oil base oil having a kinematic viscosity at 100°C of 5 to 60 mm 2 / s, further preferably a lubricating oil base oil having a kinematic viscosity at 100°C of 5 to 30 mm 2 / s.

[0045] The production method of the organobentonite grease according to the present application includes: mixing a lubricating oil base oil and an organobentonite, and stirring until uniform; optionally adding a co-dispersant, and stirring until uniform; heating to 100 to 120°C, and maintaining for 10 to 20 minutes; adding an extreme pressure anti-wear agent and a benzotriazole derivative, and stirring until uniform, followed by grinding to obtain a grease.

[0046] According to the present application, the co-dispersant that can be optionally added can be acetone and / or ethanol.

[0047] The organic bentonite grease has excellent oxidation resistance and rust resistance, and has good extreme pressure performance and excellent mechanical stability, and can be used in high temperature, high speed, high load and other harsh working conditions. BRIEF DESCRIPTION OF DRAWINGS

[0048] Figure 1 The infrared spectrum of the product of Example 2.

[0049] Figure 2 The nuclear magnetic hydrogen spectrum of the product of Example 2. DETAILED DESCRIPTION

[0050] The application will be further described by the following examples, but not constitute a limitation to the application.

[0051] Unless otherwise specified, the percentages mentioned in the context of the application are mass percentages.

[0052] The main raw materials used are as follows:

[0053] Cardanol, Shanghai Wu Jing Chemical Technology Co., Ltd., industrial product

[0054] Zinc chloride, National Pharmaceutical Group Chemical Reagent Co., Ltd., analytical pure

[0055] Sulfuric acid, National Pharmaceutical Group Chemical Reagent Co., Ltd., analytical pure

[0056] Hydrogen peroxide (30%), National Pharmaceutical Group Chemical Reagent Co., Ltd., analytical pure

[0057] Formic acid, National Pharmaceutical Group Chemical Reagent Co., Ltd., analytical pure

[0058] Benzotriazole-5-carboxylic acid, National Pharmaceutical Group Chemical Reagent Co., Ltd., chemical pure

[0059] Tert-butyl chloride, National Pharmaceutical Group Chemical Reagent Co., Ltd., analytical pure

[0060] Acetone, National Pharmaceutical Group Chemical Reagent Co., Ltd., analytical pure

[0061] Toluene, National Pharmaceutical Group Chemical Reagent Co., Ltd., analytical pure

[0062] Dimethylformamide, National Pharmaceutical Group Chemical Reagent Co., Ltd., analytical pure

[0063] Preparation of tert-butylated cardanol of Example 1

[0064] Take 100 g of cardanol, 8 g of formic acid, 0.3 g of sulfuric acid, 200 g of hydrogen peroxide, and add them to a three-necked flask with mechanical stirring, reflux condenser and temperature control. Start stirring and heating. Maintain the reaction temperature at 70°C for 3 hours. After the reaction is complete, cool it down and obtain a transparent brownish red liquid. Filter the reaction product, wash it with 5% KOH solution, then wash it with distilled water until it is neutral. Distill the organic phase under reduced pressure at 100 Pa and 150°C for 1 hour to remove water and unreacted raw materials, and obtain a transparent orange red liquid, epoxidized cardanol.

[0065] Dissolve 35 g of epoxidized cardanol in 100 ml of acetone, and then put it into a 250 ml three-necked flask. Add 0.9 g of zinc chloride catalyst, and start stirring and heating. Maintain the reaction temperature at 60°C, slowly add 9.5 g of tert-butyl chloride dropwise into the flask, and continue the reaction for 3 hours after the addition is complete. After the reaction is complete, cool it down and obtain a transparent brownish red liquid. Filter the reaction product, wash it with 5% KOH solution, then wash it with distilled water until it is neutral. Distill it under reduced pressure at 1000 Pa and 120°C for 1 hour to remove the solvent, water and unreacted raw materials, and obtain a brownish red viscous liquid, tert-butylated epoxidized cardanol.

[0066] The example reaction formula of the above reaction is shown in the following formula.

[0067]

[0068] Example 2

[0069] Put 20 g of tert-butylated epoxidized cardanol prepared in Example 1, 0.2 g of concentrated sulfuric acid, 10 g of water and 10 g of toluene into a three-necked flask with mechanical stirring and reflux condenser. Stir and heat, and react at 85°C for 1 hour. After the reaction is complete, dissolve 12 g of benzotriazole-5-carboxylic acid in 80 g of dimethylformamide (DMF), and add it dropwise into the flask. Continue refluxing for 5 hours after the addition is complete, and stop the reaction. Wash the product with water three times, and evaporate the solvent to obtain the benzotriazole derivative W-01 of the present application, with a conversion rate of 91.3%.

[0070] The example reaction formula of the above reaction is shown in the following formula.

[0071]

[0072] Perform infrared spectroscopy and nuclear magnetic hydrogen spectrum test on the product W-01 prepared in Example 2. The infrared spectrogram is shown in Figure 1 , the analysis results are shown in Table 1, and the nuclear magnetic hydrogen spectrogram is shown in Figure 2 , the analysis results are shown in Table 2.

[0073] Table 1 Infrared analysis results of product W-01

[0074]

[0075] As can be seen from Table 1, the product W-01 has characteristic peaks such as OH stretching vibration peak, ester group C=0 stretching vibration peak, benzene ring skeleton stretching vibration peak, C-N stretching vibration peak and NH bending vibration peak, which can indicate that the synthetic product is the target compound.

[0076] Table 2 Product W-01 nuclear magnetic hydrogen spectrum analysis results

[0077]

[0078] As can be seen from Table 2, according to the attribution of each H element, it can be confirmed that the synthetic product is the target compound.

[0079] Example 3

[0080] 10 g of the t-butylated epoxy cardanol prepared in Example 1, 0.2 g of concentrated sulfuric acid, 10 g of water, and 10 g of toluene were added to a three-necked flask with mechanical stirring and a reflux condenser, stirred, heated, and reacted at 95°C for 1 h. After the reaction was completed, 12 g of benzotriazole-5-carboxylic acid was dissolved in 80 g of dimethylformamide (DMF) and added dropwise to the flask. After the dropwise addition was completed, reflux reaction was continued for 3 h, and the reaction was stopped. The product was washed with water three times, and the solvent was evaporated to obtain the benzotriazole derivative W-02 of the present application, with a conversion rate of 90.4%.

[0081] Example 4

[0082] 20 g of the t-butylated epoxy cardanol prepared in Example 1, 0.2 g of concentrated sulfuric acid, 10 g of water, and 100 g of toluene were added to a three-necked flask with mechanical stirring and a reflux condenser, stirred, heated, and reacted at 110°C for 1 h. After the reaction was completed, 50 g of benzotriazole-5-carboxylic acid was dissolved in 120 g of dimethylformamide (DMF) and added dropwise to the flask. After the dropwise addition was completed, reflux reaction was continued for 6 h, and the reaction was stopped. The product was washed with water three times, and the solvent was evaporated to obtain the benzotriazole derivative W-03 of the present application, with a conversion rate of 91.6%.

[0083] The main raw materials used in the preparation of the grease are as follows:

[0084] Organic bentonite, Hangzhou Lin'an Coating Additive Chemical Co., Ltd., industrial product

[0085] Acetone, National Pharmaceutical Group Chemical Reagent Co., Ltd., analytical pure

[0086] Ethanol, National Pharmaceutical Group Chemical Reagent Co., Ltd., analytical pure

[0087] 500N, Taishan Group, industrial product

[0088] 500SN, Fushun Petrochemical, industrial product

[0089] PAO 10, ExxonMobil Chemical, commercial product

[0090] PAO 4, ExxonMobil Chemical, commercial product

[0091] Trimcresyl phosphate, Zibo Huihua Petroleum Additives Co., Ltd., commercial product

[0092] Di-n-butyl phosphite, Zibo Huihua Petroleum Additives Co., Ltd., commercial product

[0093] Sulfurized isobutylene, Zibo Huihua Petroleum Additives Co., Ltd., commercial product

[0094] Benzotriazole, Nanjing Oubike Fine Chemical Co., Ltd., commercial product

[0095] Example I-1 of organobentonite grease

[0096] Raw material components: 500SN 734 grams (100°C viscosity of 11 mm 2 / s); organobentonite 174 grams; acetone 13 grams; sulfurized isobutylene 25.9 grams; benzotriazole derivative W-01 4.55 grams.

[0097] Add 734 grams of 500SN base oil and 174 grams of organobentonite into the grease making kettle, stir uniformly, add 13 grams of acetone, heat to 100°C, keep for 10 min, add 25.9 grams of sulfurized isobutylene, 4.55 grams of benzotriazole derivative W-01, stir uniformly, and grind three times with a three-roll mill to obtain the finished grease product.

[0098] Example I-2 of organobentonite grease

[0099] Raw material components: 500N 1073 grams (100°C viscosity of 11 mm 2 / s); organobentonite 265 grams; ethanol 27 grams; trimcresyl phosphate 33.6 grams; benzotriazole derivative W-01 6.79 grams.

[0100] Add 1073 grams of 500N base oil and 265 grams of organobentonite into the grease making kettle, stir uniformly, add 27 grams of ethanol, heat to 120°C, keep for 10 min; add 33.6 grams of trimcresyl phosphate, 6.79 grams of benzotriazole derivative W-01, stir uniformly, and grind three times with a three-roll mill to obtain the finished grease product.

[0101] Example I-3 of organobentonite grease

[0102] Raw material components: PAO 10 603 grams (100°C viscosity of 10 mm 2Organic bentonite 147 g; acetone 15 g; di-n-butyl phosphite 9.75 g; benzotriazole derivative W-02 4.73 g.

[0103] Put 603 g PAO10 base oil and 147 g organic bentonite into the grease making kettle, stir uniformly, add 15 g acetone, heat to 110°C, keep for 10 min; add 9.75 g di-n-butyl phosphite, 4.73 g benzotriazole derivative W-02, stir uniformly, grind three times by three-roll mill to obtain the finished grease product.

[0104] Example I-4 of organic bentonite grease

[0105] Raw material components: PAO4 829 g (100°C viscosity 3.9 mm 2 Organic bentonite 188 g; ethanol 18 g; trimcresyl phosphate 27.6 g; benzotriazole derivative W-03 5.37 g.

[0106] Put 829 g PAO4 base oil and 188 g organic bentonite into the grease making kettle, stir uniformly, add 18 g ethanol, heat to 100°C, keep for 10 min; add 27.6 g trimcresyl phosphate, 5.37 g benzotriazole derivative W-03, stir uniformly, grind three times by three-roll mill to obtain the finished grease product.

[0107] Comparative example D-1 of organic bentonite grease

[0108] Raw material components: 500SN 734 g (100°C viscosity 11 mm 2 Organic bentonite 174 g; acetone 13 g; sulfurized isobutylene 25.9 g.

[0109] Put 734 g 500SN base oil and 174 g organic bentonite into the grease making kettle, stir uniformly, add 13 g acetone, heat to 100°C, keep for 10 min, add 25.9 g sulfurized isobutylene, stir uniformly, grind three times by three-roll mill to obtain the finished grease product.

[0110] Comparative example D-2 of organic bentonite grease

[0111] Raw material components: 500SN 734 g (100°C viscosity 11 mm 2 Organic bentonite 174 g; acetone 13 g; sulfurized isobutylene 25.9 g; benzotriazole 4.55 g.

[0112] Into a grease making kettle, 734 g of 500SN base oil and 174 g of organic bentonite were added and stirred uniformly, 13 g of acetone was added, the temperature was raised to 100°C and maintained for 10 min, 25.9 g of sulfurized isobutylene, 4.55 g of benzotriazole were added and stirred uniformly, and the grease product was prepared by three times of three-roll milling.

[0113] The prepared grease was subjected to performance evaluation, and the evaluation items, evaluation methods and evaluation results are shown in Table 3.

[0114] Table 3

[0115]

Claims

1. An organic bentonite grease comprising, based on the total weight of the grease, 0.1-5% of a benzotriazole derivative, 1-10% of an extreme pressure anti-wear agent, 5-30% of an organic bentonite, and 60-90% of a lubricating oil base oil, wherein the benzotriazole derivative has a structure represented by Formula (I): ###0001### Formula (I) wherein * represents a bonding site for bonding to Formula (II) and Formula (III); and wherein the benzotriazole derivative comprises one or more of the following compounds: ###0002### Formula (II) Formula (III). In formula (I), n is an integer between 1 and 10; the R1group is selected from C 1-20 linear or branched alkylene; the R2groups in the n number of repeating units are the same as or different from each other and are each independently selected from C 1-20 linear or branched alkylene; the R3group is selected from H and C 1-20 linear or branched alkyl; the A groups in the n number of repeating units are the same as or different from each other and are each independently selected from a group represented by formula (II), a group represented by formula (III); Formula (II) and Formula (III) wherein * represents a bonding site for bonding to Formula (I); and wherein the benzotriazole derivative comprises one or more of the following compounds: ###0002### Formula (II) Formula (III). R4groups, R5groups are each independently selected from the group consisting of H and C 1-10 linear or branched alkyl.

2. The organobentonite grease according to claim 1, characterized in that In formula (I), n is an integer between 1 and 5, the R1groups are selected from C 1-10 linear or branched alkylene, the R2groups in n repeating units are each independently selected from C 1-10 linear or branched alkylene, the R3groups are selected from H and C 1-10 linear or branched alkyl, the R4groups, the R5groups are each independently selected from C 1-4 linear or branched alkyl.

3. The organobentonite grease according to claim 1, characterized in that In formula (I), n is an integer between 1 and 3, the R1group is selected from C 1-8 linear or branched alkylene, the R2groups in n repeat units are each independently selected from C 1-8 linear or branched alkylene, the R3group is selected from H and C 1-8 linear or branched alkyl, the R4group, the R5group are selected from tert-butyl or the R4group is selected from tert-butyl, the R5group is selected from H.

4. The organobentonite grease according to claim 1, characterized in that A method for preparing the benzotriazole derivative comprises the following steps: (1) reacting a compound represented by Formula (a) with a peroxide; (2) hydrolyzing the reaction product of step (1); (3) reacting the hydrolysis product of step (2) with a compound represented by Formula (β), and collecting the product; wherein the X group is selected from the group consisting of OH, F, Cl, Br, and I.

5. The organobentonite grease according to claim 1, characterized in that, Formula (a) wherein the compound represented by Formula (a) is selected from the group consisting of cardanol and alkylated cardanol; the peroxide is selected from the group consisting of one or more of hydrogen peroxide, peroxyformic acid, peroxyacetic acid, peroxy sulfonic acid, meta-chloro peroxybenzoic acid, t-butyl hydroperoxide, t-butyl peroxyacetate, methyl ethyl ketone peroxide, dibenzoyl peroxide, and cyclohexanone peroxide; and the compound represented by Formula (β) is selected from the group consisting of one or more of benzotriazole-5-carboxylic acid, benzotriazole-5-formic acid fluoride, benzotriazole-5-formic acid chloride, benzotriazole-5-formic acid bromide, and benzotriazole-5-formic acid iodide. The molar ratio between the compound represented by Formula (a) and the peroxide, and the compound represented by Formula (β) is 1:0.5-10:0.5-10; the reaction temperature of step (1) is 50-100°C; the reaction temperature of step (2) is 50-150°C; and the reaction temperature of step (3) is 50-200°C. In formula (a), n is an integer between 1 and 10; the R1group is selected from C 1-20 linear or branched alkylene; the R2groups in the n number of repeating units are the same or different from each other and are each independently selected from C 1-20 linear or branched alkylene; the R3group is selected from H and C 1-20 linear or branched alkyl; the A" group in the n number of repeating units is selected from CHCH; the R4group, the R5group are each independently selected from H and C 1-10 linear or branched alkyl; The extreme pressure anti-wear agent is selected from the group consisting of one or more of sulfurized olefins, phosphates, phosphites, aminothioesters, and dialkyldithiocarbamic salts; and the lubricating oil base oil is selected from the group consisting of one or more of mineral oil, vegetable oil, ester synthetic oil, and poly-alpha-olefin synthetic oil. The lubricating oil base oil and the organic bentonite are mixed and stirred until uniform; an optional dispersant aid is added and stirred until uniform; the temperature is raised to 100-120°C and maintained for 10-20 min; the extreme pressure anti-wear agent and the benzotriazole derivative are added and stirred until uniform, and the grease is ground. ​ 6. An organobentonite grease according to claim 5, characterised in that In formula (a), n is an integer between 1 and 5, the R1groups are selected from C 1-10 linear or branched alkylene, the R2groups in n repeat units are each independently selected from C 1-10 linear or branched alkylene, the R3groups are selected from H and C 1-10 linear or branched alkyl, the R4groups, the R5groups are each independently selected from C 1-4 linear or branched alkyl.

7. The organobentonite grease according to claim 5, characterized in that In formula (a), n is an integer between 1 and 3, the R1groups are selected from C 1-8 linear or branched alkylene, the R2groups in n repeat units are each independently selected from C 1-8 linear or branched alkylene, the R3groups are selected from H and C 1-8 linear or branched alkyl, the R4groups, the R5groups are selected from tert-butyl or the R4groups are selected from tert-butyl, the R5groups are selected from H.

8. The organobentonite grease according to claim 5, characterized in that, ​ 9. The organobentonite grease according to claim 5, characterized in that, ​ 10. An organobentonite grease according to one of claims 1 to 9, characterized in that ​ 11. A process for the preparation of an organobentonite grease as claimed in any one of claims 1 to 10, comprising: ​

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