Lubricating grease, preparation method and application

Abstract

The invention relates to the field of lubricating grease, and discloses lubricating grease, a preparation method and application, raw materials for preparing the lubricating grease comprise basic raw materials and additives, based on the total amount of the basic raw materials, the basic raw materials comprise 95-98 wt% of base oil and 2-5 wt% of organic acid; wherein the base oil comprises CTL base oil and poly-alpha-olefin, the mass ratio of the CTL base oil to the poly-alpha-olefin is (85-70): (15-30), and the additives comprise 5-10 wt% of a tackifier based on the total weight of the base materials, 0.2-0.8 wt% of an antioxidant based on the total weight of the base materials, 1-5 wt% of an antirust agent based on the total weight of the base materials and 1-10 wt% of an anti-wear agent based on the total weight of the base materials. The saponification alkali liquor and the organic acid are subjected to saponification reaction. According to the lubricating grease, CTL base oil and poly-alpha-olefin are adopted as base oil, the thickening agent prepared through saponification reaction of organic acid and saponification alkali liquor is further adopted for thickening, antiwear additives and other additives are added for refining, the lubricating grease is obtained, the high dropping point and good low-temperature performance and lubricity are achieved, and compared with traditional barrier gate lubricating oil, the leakage problem can be effectively solved.

Description

Technical Field

[0001] This invention relates to the field of lubricating greases, and more specifically to a lubricating grease, its preparation method, and its application. Background Technology

[0002] A barrier gate, also known as a vehicle barrier, is a specialized access control device used on roads to restrict the movement of motor vehicles. It is widely used in highway toll stations and parking lot systems to manage vehicle entry and exit. With the continuous development of the automotive industry and the increasing number of cars, the demand for barrier gates is also growing.

[0003] Typically, the mechanism of a barrier gate (mainly a planetary gear reducer) has a designed lifespan, usually 100w-200w cycles, with better ones reaching 500w cycles. This directly determines the service life of the equipment. Barrier gate reducers use metal gear transmission, which inevitably experiences wear. Therefore, regular maintenance is required, including periodic replacement of standard lubricating oil or machine oil. While lubricating oil is generally used to maintain a low wear rate, it is prone to leakage due to exposure to sunlight and rain, and its good fluidity. This not only leads to ineffective lubrication but also causes environmental pollution. Summary of the Invention

[0004] The purpose of this invention is to overcome the problem of lubricating oil leakage in existing barrier gate technologies, and to provide a lubricating grease, its preparation method, and its application. This lubricating grease has a high dropping point and an adhesion rate of over 95%, effectively solving the leakage problem caused by the use of lubricating oil.

[0005] To achieve the above objectives, the present invention provides a lubricating grease, wherein the raw materials for preparing the lubricating grease include basic raw materials and additives, wherein, based on the total amount of the basic raw materials, the basic raw materials include 95-98 wt% base oil and 2-5 wt% organic acid;

[0006] The base oil comprises CTL base oil and polyalphaolefin, wherein the mass ratio of CTL base oil to polyalphaolefin is 85-70:15-30;

[0007] The additives include: 5-10 wt% of the total amount of the base raw materials as a thickener, 0.2-0.8 wt% of the total amount of the base raw materials as an antioxidant, 1-5 wt% of the total amount of the base raw materials as a rust inhibitor, and 1-10 wt% of the total amount of the base raw materials as an anti-wear agent, as well as a saponified alkaline solution that undergoes a saponification reaction with the organic acid.

[0008] A second aspect of the present invention provides a method for preparing a lubricating grease, which is carried out according to the following method:

[0009] A portion of the base oil, along with all the organic acids and saponified alkali solution, is mixed and reacted to obtain a base oil system containing a thickener. The remaining base oil is then added and mixed. After the first cooling, a thickener is added. After the second cooling, an antioxidant is added. After the third cooling, a rust inhibitor and an anti-wear agent are added and mixed thoroughly.

[0010] The third aspect of the present invention provides the application of the lubricating grease described in the first aspect of the present invention or the lubricating grease prepared by the preparation method described in the second aspect of the present invention in a gate reducer.

[0011] The semi-fluid grease provided in this application uses CTL base oil (coal-derived oil) and polyalphaolefin as base oils, and is further thickened with a thickener obtained by saponification reaction of organic acid and saponified alkali solution. It is refined by adding anti-wear and other additives, and has a high dropping point, good low-temperature performance and lubricity. It is suitable for temperatures from -40 to 140°C and is suitable for the lubrication of planetary reducers of barrier gates. Compared with traditional barrier gate lubricating oils, it can effectively reduce leakage problems. Detailed Implementation

[0012] The endpoints and any values ​​of the ranges disclosed herein are not limited to the precise ranges or values, and these ranges or values ​​should be understood to include values ​​close to these ranges or values. For numerical ranges, the endpoint values ​​of the various ranges, the endpoint values ​​of the various ranges and individual point values, and individual point values ​​can be combined with each other to obtain one or more new numerical ranges, which should be considered as specifically disclosed herein.

[0013] The present invention provides a lubricating grease, wherein the raw materials for preparing the lubricating grease include basic raw materials and additives, wherein, based on the total amount of the basic raw materials, the basic raw materials include 95-98 wt% base oil and 2-5 wt% organic acid;

[0014] The base oil comprises CTL base oil and polyalphaolefin, wherein the mass ratio of CTL base oil to polyalphaolefin is 85-70:15-30;

[0015] The additives include: 5-10 wt% of the total amount of the base raw materials as a thickener, 0.2-0.8 wt% of the total amount of the base raw materials as an antioxidant, 1-5 wt% of the total amount of the base raw materials as a rust inhibitor, and 1-10 wt% of the total amount of the base raw materials as an anti-wear agent, as well as a saponified alkaline solution that undergoes a saponification reaction with the organic acid.

[0016] CTL base oil is a base oil synthesized via a non-petroleum route using Fischer-Tropsch synthesis technology, which converts coal-to-syngas into mixed hydrocarbons (Coal to liquid, CTL). The amount of base oil can be any value within the range of any two values ​​from 95wt%, 96wt%, 97wt%, and 98wt% of the total amount of base raw materials; the amount of organic acid can be any value within the range of any two values ​​from 2wt%, 3wt%, 4wt%, and 5wt% of the total amount of base raw materials; the amount of tackifier can be any value within the range of any two values ​​from 5wt%, 6wt%, 7wt%, 8wt%, 9wt%, and 10wt% of the total amount of base raw materials; the amount of antioxidant can be any value within the range of any two values ​​from 0.2wt%, 0.4wt%, 0.6wt%, and 0.8wt% of the total amount of base raw materials; the amount of rust inhibitor can be any value within the range of any two values ​​from 1wt%, 3wt%, and 5wt% of the total amount of base raw materials; and the amount of anti-wear agent can be any value within the range of any two values ​​from 1wt%, 3wt%, 5wt%, 7wt%, 9wt%, and 10wt% of the total amount of base raw materials.

[0017] In some embodiments of the present invention, preferably, the adhesion of the lubricating grease is not less than 95%, wherein the adhesion is tested by the following method:

[0018] Weigh 10±0.1g of grease and place it in the center of a horizontal metal disk with a diameter of 10±0.1cm. Heat the disk and stabilize the temperature at 66±1℃. Then rotate the disk at 150±10r / min for 15min. The adhesion calculation formula is as follows:

[0019] Adhesion % = [1 - (m0 - m1) / m0] × 100%, where m0 is the total weight of the metal disc and the grease placed before the test, and m1 is the total weight of the metal disc and the remaining grease on it after the test.

[0020] In some embodiments of the present invention, preferably, the dropping point of the grease is not less than 200°C.

[0021] In some embodiments of the present invention, preferably, the non-working cone penetration of the grease after being frozen at -40°C for 2 hours is not less than 75.

[0022] In some embodiments of the present invention, preferably, the organic acid includes 12-hydroxystearic acid and sebacic acid, wherein the mass ratio of 12-hydroxystearic acid to sebacic acid is 4-2:1. The two organic acids selected in this application react with saponifying alkali to generate a composite soap thickener. The mass ratio of 12-hydroxystearic acid to sebacic acid can be any value within the range of any two values ​​from 4:1, 3:1, and 2:1. The amount of saponifying alkali added is as needed. After saponification, the saponification value of the 12-hydroxystearic acid is 183-188 mg KOH / g, and the saponification value of the sebacic acid is 553-573 mg KOH / g. The saponification value of the 12-hydroxystearic acid can be any value within the range of any two values ​​from 183 mg KOH / g, 185 mg KOH / g, and 188 mg KOH / g, and the saponification value of the sebacic acid can be any value within the range of any two values ​​from 553 mg KOH / g, 563 mg KOH / g, and 573 mg KOH / g.

[0023] In some embodiments of the present invention, preferably, the saponifying alkaline solution is a lithium hydroxide solution.

[0024] In some embodiments of the present invention, preferably, the kinematic viscosity of the CTL base oil at 100°C is 6-10 mm. 2 / s, the kinematic viscosity of the polyα-olefin at 100°C is 20-40 mm² / s. 2 / s.

[0025] In some embodiments of the present invention, preferably, the kinematic viscosity of the CTL base oil at 100°C is 8-10 mm. 2 / s, the kinematic viscosity of the polyα-olefin at 100℃ is 20-30 mm. 2 / s.

[0026] CTL base oil has a kinematic viscosity of 6 mm at 100℃. 2 / s, 7mm 2 / s, 8mm 2 / s, 10mm 2 Any value within a range consisting of any two values ​​in / s. The kinematic viscosity of polyalphaolefin at 100℃ can be 20 mm. 2 / s, 25mm 2 / s, 30mm 2 / s, 35mm 2 / s, 40mm 2 Any value within the range formed by any two values ​​in / s.

[0027] In some embodiments of the present invention, preferably, the mass ratio of the CTL base oil to the polyalphaolefin is 75-70:25-30. The mass ratio of the CTL base oil to the polyalphaolefin can be any value within the range of any two values ​​from 85:15, 85:30, 70:15, 70:30, 75:25, 75:30, 70:25, and 70:30.

[0028] In some embodiments of the present invention, preferably, the CTL base oil is selected from at least one of CTL6, CTL8, and CTL10.

[0029] In some embodiments of the present invention, preferably, the polyα-olefin is selected from at least one of PAO20 and PAO40.

[0030] In some embodiments of the present invention, preferably, the tackifier is selected from one or more of polyisobutylene and polymethacrylate.

[0031] In some embodiments of the present invention, preferably, the kinematic viscosity of the polyisobutylene at 100°C is 4500-7000 mmHg. 2 / s. The kinematic viscosity of polyisobutylene at 100℃ can be 4500 mm. 2 / s, 5500mm 2 / s, 6500mm 2 / s, 7000mm 2 Any value within the range formed by any two values ​​in / s.

[0032] In some embodiments of the present invention, preferably, the number-average molecular weight of the polymethacrylate is 40,000-80,000. The number-average molecular weight of the polymethacrylate can be any value within the range of any two values ​​from 40,000, 50,000, 60,000, 70,000, to 80,000.

[0033] In some embodiments of the present invention, preferably, the antioxidant is selected from one or more of diisooctyldiphenylamine and N-phenyl-α-aniline.

[0034] In some embodiments of the present invention, preferably, the rust inhibitor is selected from one or more of benzotriazole, barium petroleum sulfonate, barium dinonylnaphthalene sulfonate, and alkenyl succinic acid.

[0035] In some embodiments of the present invention, preferably, the anti-wear agent is selected from one or more of zinc thiophosphate, aminothioester, and triphenyl thiophosphate.

[0036] A second aspect of the present invention provides a method for preparing a lubricating grease, which is carried out according to the following method:

[0037] A portion of the base oil, along with all the organic acids and saponified alkali solution, is mixed and reacted to obtain a base oil system containing a thickener. The remaining base oil is then added and mixed. After the first cooling, a thickener is added. After the second cooling, an antioxidant is added. After the third cooling, a rust inhibitor and an anti-wear agent are added and mixed thoroughly.

[0038] In some embodiments of the present invention, preferably, the process of mixing a portion of the base oil and all the organic acids and saponification alkali to obtain a base oil system containing a thickener includes: mixing 40-60 wt% of the base oil based on the total amount of base oil with all of the 12-hydroxystearic acid, adding the saponification alkali required for saponifying the 12-hydroxystearic acid for a first reaction, and then adding sebacic acid and the saponification alkali required for saponifying the sebacic acid for a second reaction, thereby obtaining a base oil system containing a thickener. The present invention uses an atmospheric pressure reaction to saponify the 12-hydroxystearic acid and sebacic acid stepwise to ensure the thickening effect of the composite soap and to guarantee the dropping point. The amount of base oil mixed with the 12-hydroxystearic acid can be any value within the range of any two values ​​from 40 wt%, 50 wt%, and 60 wt% of the total amount of base oil.

[0039] In some embodiments of the present invention, preferably, the process of adding the remaining base oil for mixing includes: after all the sucralose and the saponification alkali solution required for saponifying sucralose have been added, the system is heated to 160-170°C, the remaining base oil is added, and the temperature is further raised to 205-210°C and held at that temperature for 3-5 minutes. The system temperature when adding the base oil can be any value within the range of any two values ​​from 160°C, 165°C, and 170°C, and the holding time can be any value within the range of any two values ​​from 3 minutes, 4 minutes, and 5 minutes.

[0040] In some embodiments of the present invention, preferably, the temperature for carrying out the first reaction is 92-98°C, and the reaction time is 20-30 min. The first reaction is the saponification of 12-hydroxystearic acid, and the temperature can be any value within the range of any two values ​​formed by 92°C, 95°C, and 98°C, and the time can be any value within the range of any two values ​​formed by 20 min, 25 min, and 30 min.

[0041] In some embodiments of the present invention, preferably, the process of adding sebacic acid and the saponifying alkali solution required for saponifying sebacic acid to carry out the second reaction includes: after the first reaction is completed, the system is heated to 130-135°C, sebacic acid is added, and then the temperature is raised to 140-145°C to melt the sebacic acid, and then the temperature is lowered to 127-133°C to add the saponifying alkali solution required for saponifying sebacic acid in two batches. To ensure that the sebacic acid melts smoothly, the system needs to be initially heated, and after adding the sebacic acid, the temperature is raised to 140-145°C. To prevent the added alkali solution from vaporizing and causing a decrease in the saponification value, the system needs to be cooled before adding the alkali solution. Half of the required saponifying alkali solution is added first, at which point the system temperature will decrease, and it needs to be heated again to 127-133°C before adding the other half of the required saponifying alkali solution.

[0042] In some embodiments of the present invention, preferably, the system temperature after the first cooling is 150-160°C. The system temperature after the first cooling can be any value within the range of any two values ​​among 150°C, 155°C, and 160°C.

[0043] In some embodiments of the present invention, preferably, the system temperature after the second cooling is 110-120°C. The system temperature after the second cooling can be any value within the range of any two values ​​among 110°C, 115°C, and 120°C.

[0044] In some embodiments of the present invention, preferably, the system temperature after the third cooling is 95-105°C. The system temperature after the third cooling can be any value within the range of any two values ​​among 95°C, 100°C, and 105°C.

[0045] The third aspect of the present invention provides the application of the lubricating grease described in the first aspect of the present invention or the lubricating grease prepared by the preparation method described in the second aspect of the present invention in a gate reducer.

[0046] In some embodiments of the present invention, preferably, the ambient temperature of the application is -40°C to 140°C.

[0047] According to a particularly preferred embodiment of the present invention, the raw materials for preparing the grease include base raw materials and additives, wherein, based on the total amount of the base raw materials, the base raw materials include 96-97 wt% base oil and 3-4 wt% organic acids;

[0048] The base oil comprises CTL base oil and polyalphaolefin, wherein the mass ratio of CTL base oil to polyalphaolefin is 70-75:30-25;

[0049] The additives include: 5-10 wt% of the total amount of the base raw materials as a thickener, 0.2-0.8 wt% of the total amount of the base raw materials as an antioxidant, 1-5 wt% of the total amount of the base raw materials as a rust inhibitor, and 1-10 wt% of the total amount of the base raw materials as an anti-wear agent, as well as a saponified alkaline solution that undergoes a saponification reaction with the organic acid.

[0050] The present invention will be described in detail below through embodiments. In the following embodiments, the appearance was determined by visual inspection; the dropping point was measured using the GB / T 3497 method; the non-working cone penetration and 1 / 4 non-working cone penetration were both measured using the GB / T 269 method; corrosion was measured using the SH / T 0331 method; oil separation of the steel mesh was measured using the NB / SH / T 0324 method; dynamic evaporation was measured using the GB / T 7325 method; corrosion resistance was measured using the GB / T 5018 method; the wear scar diameter of the four-ball test was measured using the SH / T 0204 method; the maximum non-seize load and sintering load of the four balls were measured using the GB / T 3142 method; and adhesion was measured using the following method:

[0051] Weigh 10±0.1g of grease and spread it evenly in a horizontal metal pan with a diameter of 10±0.1cm. Turn on the heating and, when the temperature of the metal pan stabilizes at 66±1℃, turn on the switch. The metal pan rotates at a speed of 150±10r / min for 15min, then stops (keep heating the metal pan during rotation to maintain its temperature at 66±1℃). Weigh the metal pan before and after the test to obtain the amount of grease lost from the metal pan. The ratio of the lost amount to the total mass of grease is the loss ratio. Subtract the loss ratio from 100% to obtain the adhesion. The specific calculation formula is as follows: Adhesion % = [1-(m0-m1) / m0]×100%, where m0 is the total weight of the metal pan and the grease placed before the test, and m1 is the total weight of the metal pan and the remaining grease after the test.

[0052] Unless otherwise specified, all raw materials used in the following examples and comparative examples are commercially available. The sources and product codes of some of the raw materials used in the following examples are briefly described below.

[0053] PAO20 was purchased from Shenyang Hongcheng Fine Chemical Factory. The model is PAO20, and its kinematic viscosity at 100℃ is 20 mmHg. 2 / s;

[0054] PAO20 and PAO40 were mixed at a mass ratio of 4:6, and the resulting PAO mixture had a kinematic viscosity of 30 mmHg at 100°C. 2 / s;

[0055] PAO40 was purchased from Shenyang Hongcheng Fine Chemical Factory. The model is PAO40, and its kinematic viscosity at 100℃ is 40 mmHg. 2 / s;

[0056] CTL6 was purchased from Lu'an Chemical Group, model CTL6, with a kinematic viscosity of 6 mmHg at 100℃. 2 / s;

[0057] CTL8 was purchased from Lu'an Chemical Group. The model is CTL8, and its kinematic viscosity at 100℃ is 8 mm. 2 / s;

[0058] CTL10 was purchased from Lu'an Chemical Group. The model is CTL10, and its kinematic viscosity at 100℃ is 10 mmHg. 2 / s;

[0059] Polyisobutylene 6240 was purchased from Jinzhou Jinglian Lubricating Oil Additives Co., Ltd., model JINEX 6240, with a kinematic viscosity of 4700 mmHg at 100℃. 2 / s;

[0060] Polyisobutylene 6350 was purchased from Jinzhou Jinglian Lubricating Oil Additives Co., Ltd., model JINEX 6350, with a kinematic viscosity of 7000 mmHg at 100℃. 2 / s;

[0061] The polymethyl methacrylate is produced by Sinopec Lubricating Oil Synthetic Grease Co., Ltd., and is designated as No. 1 methyl butyl ester with a number average molecular weight of 60,000.

[0062] Diisooctyldiphenylamine was purchased from Quzhou Hengshun Chemical Co., Ltd.

[0063] N-Phenyl-α-aniline was purchased from Tianjin Yuning Chemical Co., Ltd., model T531;

[0064] Barium dinonylnaphthalenesulfonate, purchased from Suzhou Specialty Chemicals Co., Ltd., model T705;

[0065] Benzotriazole, purchased from Nantong Botao Chemical Co., Ltd., model T706;

[0066] Dodecenyl succinic acid, purchased from Dalian Guanghui Technology Co., Ltd., model T746;

[0067] The zinc thiophosphate butyrate salt, purchased from Wuxi Southern Petroleum Additives Co., Ltd., model T202;

[0068] Triphenyl thiophosphate, purchased from Shenyang Feida Chemical Oil Products Co., Ltd., model T309;

[0069] Alkyl dithiocarbamate, purchased from Jinzhou Yuchen Fine Chemical Co., Ltd., model T323.

[0070] Example 1

[0071] (1) Weigh 727.5g of CTL10 and 242.5g of PAO 20 and mix them to obtain the base oil, wherein the kinematic viscosity of CTL10 at 100℃ is 10 mm. 2 The kinematic viscosity of PAO 20 at 100℃ is 20 mm² / s. 2 / s;

[0072] (2) Weigh 390g of base oil and 22.5g of 12-hydroxystearic acid and add them to the reactor. Stir and heat to 93°C, then add lithium hydroxide alkaline solution (3.28g of lithium hydroxide monohydrate dissolved in 19.7g of deionized water). Maintain the reaction at this temperature for 20min. The saponification value of 12-hydroxystearic acid is 0.185.

[0073] (3) Continue heating to 130℃ and add 7.5g sebacic acid. Stir and heat to 140℃, then cool down to 130℃ and add lithium hydroxide alkaline solution (1.65g lithium hydroxide monohydrate dissolved in 9.9g deionized water). Stir. At this time, the system temperature has decreased. Continue heating to 130℃ and add lithium hydroxide alkaline solution (1.65g lithium hydroxide monohydrate dissolved in 9.9g deionized water) again. The saponification value of sebacic acid is 0.56.

[0074] (4) Then raise the system temperature to 160°C, add the remaining 580g of base oil, continue to raise the temperature to 205°C, keep the temperature constant for 3 minutes, stop heating and stir to cool down;

[0075] (5) Continue cooling to 160℃ and add 80g of polyisobutylene 6240. Continue cooling to 110℃ and add 3g of diisooctyl diphenylamine. Continue cooling to 100℃ and add 10g of rust inhibitor T705 and 10g of rust inhibitor T746, 20g of anti-wear agent T202 and 10g of anti-wear agent T323. Stir evenly.

[0076] (6) Grind the obtained grease three times with a three-roll mill to obtain the final product.

[0077] Example 2

[0078] (1) Weigh 724g of CTL8 and 241g of PAO 20 and mix them to obtain the base oil, wherein the kinematic viscosity of CTL8 at 100℃ is 8 mm. 2 The kinematic viscosity of PAO 20 at 100℃ is 20 mm² / s. 2 / s;

[0079] (2) Weigh 400g of base oil and 26.25g of 12-hydroxystearic acid and add them to the reactor. Stir and heat to 95°C, then add lithium hydroxide alkaline solution (3.83g of lithium hydroxide monohydrate dissolved in 23g of deionized water). Maintain the reaction at this temperature for 25min. The saponification value of 12-hydroxystearic acid is 0.185.

[0080] (3) Continue heating to 135℃ and add 8.75g sebacic acid. Stir and heat to 142℃, then cool down to 130℃ and add lithium hydroxide alkaline solution (1.93g lithium hydroxide monohydrate dissolved in 11.6g deionized water). Stir. At this time, the system temperature has decreased. Continue heating to 130℃ and add lithium hydroxide alkaline solution (1.93g lithium hydroxide monohydrate dissolved in 11.6g deionized water) again. The saponification value of sebacic acid is 0.56.

[0081] (4) Then raise the system temperature to 165°C, add the remaining 565g of base oil, continue to raise the temperature to 205°C, keep the temperature constant for 3 minutes, stop heating and stir to cool down;

[0082] (5) Continue cooling to 150℃ and add 60g of polyisobutylene 6350, continue cooling to 113℃ and add 4g of diisooctyl diphenylamine, continue cooling to 100℃ and add 3g of rust inhibitor T706, 10g of rust inhibitor T705, 10g of rust inhibitor T746, 20g of anti-wear agent T202 and 10g of anti-wear agent T309, and stir evenly;

[0083] (6) Grind the obtained grease three times with a three-roll mill to obtain the final product.

[0084] Example 3

[0085] The procedure was carried out in accordance with Example 1, except that the kinematic viscosity at 100°C was 6 mm. 2 The kinematic viscosity of CTL6 at 100°C is 20 mm / s. 2 The base oil is obtained by mixing PAO 20 at a rate of / s.

[0086] Example 4

[0087] The procedure was carried out in accordance with Example 1, except that the kinematic viscosity at 100°C was 10 mm. 2 The kinematic viscosity at CTL10 and 100°C is 30 mm³ / s. 2 The base oil is obtained by mixing PAO at a rate of / s.

[0088] Example 5

[0089] The procedure was carried out in accordance with Example 1, except that the kinematic viscosity at 100°C was 10 mm. 2 The kinematic viscosity at CTL10 and 100°C is 40 mm³ / s. 2 The base oil is obtained by mixing PAO 40 at a rate of / s.

[0090] Example 6

[0091] (1) Weigh 768g of CTL10 and 192g of PAO 40 and mix them to obtain the base oil, wherein the kinematic viscosity of CTL10 at 100℃ is 10 mm. 2 The kinematic viscosity of PAO 40 at 100℃ is 40 mm² / s. 2 / s;

[0092] (2) Weigh 400g of base oil and 30g of 12-hydroxystearic acid and add them to the reactor. Stir and heat to 95°C, then add lithium hydroxide alkaline solution (4.37g of lithium hydroxide monohydrate dissolved in 26.2g of deionized water). Maintain the reaction at this temperature for 25min. The saponification value of 12-hydroxystearic acid is 0.185.

[0093] (3) Continue heating to 130℃ and add 10g of sebacic acid. Stir and heat to 140℃, then cool down to 130℃ and add lithium hydroxide alkaline solution (2.2g of lithium hydroxide monohydrate dissolved in 13.2g of deionized water). Stir. At this time, the system temperature has decreased. Continue heating to 130℃ and add lithium hydroxide alkaline solution (2.2g of lithium hydroxide monohydrate dissolved in 13.2g of deionized water) again. The saponification value of sebacic acid is 0.56.

[0094] (4) Then raise the system temperature to 160°C, add the remaining 560g of base oil, continue to raise the temperature to 208°C, keep the temperature constant for 3 minutes, stop heating and stir to cool down;

[0095] (5) Continue cooling to 160℃ and add 70g of polyisobutylene 6240. Continue cooling to 115℃ and add 3g of diisooctyl diphenylamine. Continue cooling to 100℃ and add 3g of rust inhibitor T706 and 10g of rust inhibitor T746, 20g of anti-wear agent T202, 10g of anti-wear agent T309 and 5g of anti-wear agent T323. Stir evenly.

[0096] (6) Grind the obtained grease three times with a three-roll mill to obtain the final product.

[0097] Example 7

[0098] (1) Weigh 833g of CTL6 and 147g of PAO 20 and mix them to obtain the base oil, wherein the kinematic viscosity of CTL6 at 100℃ is 6 mm. 2 The kinematic viscosity of PAO 20 at 100℃ is 20 mm² / s. 2 / s;

[0099] (2) Weigh 588g of base oil and 16g of 12-hydroxystearic acid and add them to the reactor. Stir and heat to 98°C, then add lithium hydroxide alkaline solution (2.33g of lithium hydroxide monohydrate dissolved in 14g of deionized water). Maintain the reaction at this temperature for 30min. The saponification value of 12-hydroxystearic acid is 0.185.

[0100] (3) Continue heating to 133℃ and add 4g of sebacic acid. Stir and heat to 145℃, then cool down to 127℃ and add lithium hydroxide alkaline solution (0.88g of lithium hydroxide monohydrate dissolved in 5.3g of deionized water). Stir. At this time, the system temperature has decreased. Continue heating to 127℃ and add lithium hydroxide alkaline solution (0.88g of lithium hydroxide monohydrate dissolved in 5.3g of deionized water). The saponification value of sebacic acid is 0.57.

[0101] (4) Then raise the system temperature to 155°C, add the remaining 392g of base oil, continue to raise the temperature to 210°C, keep the temperature constant for 2 minutes, stop heating and stir to cool down;

[0102] (5) Continue cooling to 160℃ and add 100g of polyisobutylene 6240. Continue cooling to 120℃ and add 4g of N-phenyl-α-aniline. Continue cooling to 95℃ and add 20g of rust inhibitor T706 and 30g of rust inhibitor T746, 2g of anti-wear agent T202, 5g of anti-wear agent T309 and 3g of anti-wear agent T323. Stir evenly.

[0103] (6) Grind the obtained grease three times with a three-roll mill to obtain the final product.

[0104] Example 8

[0105] (1) Weigh 665g of CTL6 and 285g of PAO 40 and mix them to obtain the base oil. The kinematic viscosity of CTL6 at 100℃ is 6 mm. 2 The kinematic viscosity of PAO 40 at 100℃ is 40 mm² / s. 2 / s;

[0106] (2) Weigh 475g of base oil and 33.3g of 12-hydroxystearic acid and add them to the reactor. Stir and heat to 98°C, then add lithium hydroxide alkaline solution (4.86g of lithium hydroxide monohydrate dissolved in 29.1g of deionized water). Maintain the reaction at this temperature for 25min. The saponification value of 12-hydroxystearic acid is 0.186.

[0107] (3) Continue heating to 133℃ and add 16.7g of sebacic acid. Stir and heat to 145℃, then cool down to 133℃ and add lithium hydroxide alkaline solution (3.68g of lithium hydroxide monohydrate dissolved in 22.1g of deionized water). Stir. At this time, the system temperature has decreased. Continue heating to 133℃ and add lithium hydroxide alkaline solution (3.68g of lithium hydroxide monohydrate dissolved in 22.1g of deionized water) again. The saponification value of sebacic acid is 0.56.

[0108] (4) Then raise the system temperature to 170°C, add the remaining 475g of base oil, continue to raise the temperature to 210°C, keep the temperature constant for 2 minutes, stop heating and stir to cool down;

[0109] (5) Continue cooling to 160℃ and add 60g of polyisobutylene 6240. Continue cooling to 120℃ and add 8g of diisooctyl diphenylamine. Continue cooling to 105℃ and add 10g of rust inhibitor T706 and 10g of rust inhibitor T746, 20g of anti-wear agent T202, 30g of anti-wear agent T309 and 50g of anti-wear agent T323. Stir evenly.

[0110] (6) Grind the obtained grease three times with a three-roll mill to obtain the final product.

[0111] Example 9

[0112] The procedure was carried out in accordance with Example 2, except that the kinematic viscosity at 100°C was 8 mm. 2 The kinematic viscosity of CTL8 at 100°C is 20 mm³ / s. 2 The base oil is obtained by mixing PAO 20 at a concentration of / s, wherein the base oil comprises 679g of CTL8 and 291g of PAO 20.

[0113] Example 10

[0114] The procedure was carried out in accordance with Example 9, except that the base oil included 824.5g of CTL8 and 145.5g of PAO 20.

[0115] Comparative Example 1

[0116] As a comparison with Example 2, the main difference lies in the different proportion of total base oil (total base oil accounts for 94%), and the corresponding adjustments are made to the amounts of organic acid and saponified lye solution, as follows:

[0117] (1) Weigh 707g of CTL8 and 234g of PAO 20 and mix them to obtain the base oil, wherein the kinematic viscosity of CTL8 at 100℃ is 10 mm. 2 The kinematic viscosity of PAO 20 at 100℃ is 20 mm² / s. 2 / s;

[0118] (2) Weigh 376g of base oil and 45g of 12-hydroxystearic acid and add them to the reactor. Stir and heat to 93°C, then add lithium hydroxide alkaline solution (6.56g of lithium hydroxide monohydrate dissolved in 39.36g of deionized water). Maintain the reaction at this temperature for 20min. The saponification value of 12-hydroxystearic acid is 0.185.

[0119] (3) Continue heating to 130℃ and add 15g of sebacic acid. Stir and heat to 140℃, then cool down to 130℃ and add lithium hydroxide alkaline solution (3.31g of lithium hydroxide monohydrate dissolved in 19.86g of deionized water). Stir. At this time, the system temperature has decreased. Continue heating to 130℃ and add lithium hydroxide alkaline solution (3.31g of lithium hydroxide monohydrate dissolved in 19.86g of deionized water) again. The saponification value of sebacic acid is 0.56.

[0120] (4) Then raise the system temperature to 160°C, add the remaining 580g of base oil, continue to raise the temperature to 205°C, keep the temperature constant for 3 minutes, stop heating and stir to cool down;

[0121] (5) Continue cooling to 160℃ and add 80g of polyisobutylene 6240. Continue cooling to 110℃ and add 3g of diisooctyl diphenylamine. Continue cooling to 100℃ and add 10g of rust inhibitor T705 and 10g of rust inhibitor T746, 20g of anti-wear agent T202 and 10g of anti-wear agent T323. Stir evenly.

[0122] (6) The obtained grease was ground three times with a three-roll mill to obtain a comparison product.

[0123] Comparative Example 2

[0124] As a comparison with Example 2, the main difference lies in the different proportion of total base oil (total base oil accounts for 99%), and the corresponding adjustments are made to the amounts of organic acid and saponification alkali solution, as follows:

[0125] (1) Weigh 742.5g of CTL8 and 247.5g of PAO 20 and mix them to obtain the base oil, wherein the kinematic viscosity of CTL8 at 100℃ is 10 mm. 2 The kinematic viscosity of PAO 20 at 100℃ is 20 mm² / s. 2 / s;

[0126] (2) Weigh 396g of base oil and 7.5g of 12-hydroxystearic acid and add them to the reactor. Stir and heat to 93°C, then add lithium hydroxide alkaline solution (1.09g of lithium hydroxide monohydrate dissolved in 6.54g of deionized water). Maintain the reaction at this temperature for 20min. The saponification value of 12-hydroxystearic acid is 0.185.

[0127] (3) Continue heating to 130℃ and add 2.5g sebacic acid. Stir and heat to 140℃, then cool down to 130℃ and add lithium hydroxide alkaline solution (0.55g lithium hydroxide monohydrate dissolved in 3.3g deionized water). Stir. At this time, the system temperature has decreased. Continue heating to 130℃ and add lithium hydroxide alkaline solution (0.55g lithium hydroxide monohydrate dissolved in 3.3g deionized water) again. The saponification value of sebacic acid is 0.56.

[0128] (4) Then raise the temperature of the system to 160°C, add the remaining 580 g of base oil, continue to raise the temperature to 205°C, keep it at a constant temperature for 3 min, stop heating and stir to cool down;

[0129] (5) Continue to cool down to 160°C and add 80 g of polyisobutene 6240, continue to cool down to 110°C and add 3 g of diisooctyl diphenylamine, continue to cool down to 100°C and add 10 g of rust inhibitor T705 and 10 g of rust inhibitor T746, 20 g of anti-wear agent T202 and 10 g of anti-wear agent T323, and stir evenly;

[0130] (6) Grind the obtained grease three times with a three-roll mill to obtain the comparative product.

[0131] Take the greases prepared in Examples 1-10 and the greases prepared in Comparative Examples 1-2 as samples, observe the appearance respectively, and test the dropping point, non-worked penetration, corrosion, 1 / 4 non-worked penetration, steel mesh bleeding, dynamic evaporation, corrosion performance, four-ball test wear scar diameter, four-ball maximum non-seizure load and adhesiveness. Among them, the 1 / 4 non-worked penetration is tested after freezing the grease at -40°C for 2 h. The appearances of the greases obtained in Examples 1-11 are all uniform and smooth greases. The anti-corrosion tests at 52°C for 48 h are all qualified, and the corrosion tests on No. 45 steel at 100°C for 24 h are all qualified. The other test results are shown in Table 1.

[0132] Table 1 Test Results

[0133]

[0134] Continued Table of Table 1

[0135]

[0136]

[0137] It can be seen from Examples 1-3 that there is a contradictory relationship between the low-temperature performance and adhesiveness of the prepared grease. Considering the overall performance, when the kinematic viscosity of CTL at 100°C is 8-10 mm2 / s, the performance of the prepared grease is more excellent. Among them, especially the grease prepared in Example 2 shows particularly excellent comprehensive performance in terms of dropping point, 1 / 4 non-worked penetration, steel mesh bleeding, dynamic evaporation, adhesiveness, and maximum non-seizure load and sintering load.

[0138] Combining Examples 1, 4 and 5, it can be seen that when the kinematic viscosity of PAO at 100°C is 20-30 mm 2 / s, the comprehensive performance of the prepared grease is better.

[0139] As can be seen from Examples 2, 9 and 10, the grease produced has better overall performance when the mass ratio of CTL to PAO is in the range of 75-70:25-30.

[0140] The difference between Comparative Example 1 and Example 2 is that the total base oil content is lower and the content of organic acids is higher. The non-working penetration of the grease prepared in Comparative Example 1 is smaller than the 00 index, and the 1 / 4 non-working penetration (-40℃) is less than 75 / 0.1mm.

[0141] The difference between Comparative Example 2 and Example 2 is that the total base oil content is higher and the organic acid content is lower. The grease prepared in Comparative Example 2 has a larger non-working cone penetration, which exceeds the 00 index, and a lower dropping point. It also has greater oil separation and an adhesion of less than 90%.

[0142] When other base oils, types of organic acids, and quantities are used, the performance of the resulting grease will be worse than that of Comparative Examples 1 and 2, failing to meet the requirements. It is evident that only when the types and proportions of the total base oil and organic acids meet the requirements of this application can a grease with superior performance be obtained.

[0143] In summary, the grease of this invention maintains a consistency within the No. 1 range at a low temperature of -40°C (1 / 4 non-working depth), preventing excessive viscosity from affecting the gearbox start-up. Its dropping point is not lower than 200°C, meaning its maximum operating temperature can reach 150°C. Furthermore, this product is a No. 00 semi-fluid grease with excellent fluidity and an adhesion rate exceeding 95%, effectively solving the leakage problem associated with oil lubrication. Research has also shown that using the grease provided by this invention can extend the service life of the barrier gate mechanism.

[0144] The preferred embodiments of the present invention have been described in detail above; however, the present invention is not limited thereto. Within the scope of the inventive concept, various simple modifications can be made to the technical solutions of the present invention, including combinations of various technical features in any other suitable manner. These simple modifications and combinations should also be considered as the content disclosed in the present invention and are all within the protection scope of the present invention.

Claims

1. A lubricating grease, characterized in that, The raw materials for preparing the grease include base materials and additives, wherein, based on the total amount of the base materials, the base materials include 95-98 wt% base oil and 2-5 wt% organic acids; The base oil comprises CTL base oil and polyalphaolefin, wherein the mass ratio of CTL base oil to polyalphaolefin is 85-70:15-30; The additives include: 5-10 wt% of the total amount of the base raw materials as a thickener, 0.2-0.8 wt% of the total amount of the base raw materials as an antioxidant, 1-5 wt% of the total amount of the base raw materials as a rust inhibitor, and 1-10 wt% of the total amount of the base raw materials as an anti-wear agent, as well as a saponified alkaline solution that undergoes a saponification reaction with the organic acid.

2. The lubricating grease according to claim 1, wherein, The grease has an adhesion of not less than 95%, wherein the test method for the adhesion is as follows: Weigh 10±0.1g of lubricating grease and spread it evenly in a horizontal metal dish with a diameter of 10±0.1cm. Heat the dish until the temperature stabilizes at 66±1℃, then rotate the dish at 150±10r / min for 15min. The adhesion calculation formula is as follows: Adhesion % = [1-(m0-m1) / m0]×100%, where m0 is the total weight of the metal disc and the grease placed before the test, and m1 is the total weight of the metal disc and the remaining grease on it after the test. Preferably, the dropping point of the grease is not less than 200°C; Preferably, the non-working cone penetration of the grease after being frozen at -40°C for 2 hours is not less than 75.

3. The lubricating grease according to claim 1 or 2, wherein, The organic acids include 12-hydroxystearic acid and sebacic acid, wherein the mass ratio of 12-hydroxystearic acid to sebacic acid is 4-2:1; Preferably, the saponifying alkaline solution is a lithium hydroxide solution.

4. The lubricating grease according to any one of claims 1-3, wherein, The kinematic viscosity of the CTL base oil at 100°C is 6-10 mm. 2 / s, the kinematic viscosity of the polyα-olefin at 100°C is 20-40 mm² / s. 2 / s; Preferably, the kinematic viscosity of the CTL base oil at 100°C is 8-10 mmHg. 2 / s, the kinematic viscosity of the polyα-olefin at 100℃ is 20-30 mm. 2 / s; Preferably, the mass ratio of the CTL base oil to the polyα-olefin is 75-70:25-30; Preferably, the CTL base oil is selected from at least one of CTL6, CTL8, and CTL10; Preferably, the poly-α-olefin is selected from at least one of PAO20 and PAO40.

5. The lubricating grease according to any one of claims 1-4, wherein, The tackifier is selected from one or more of polyisobutylene and polymethacrylate; Preferably, the kinematic viscosity of the polyisobutylene at 100°C is 4500-7000 mmHg. 2 / s; Preferably, the polymethacrylate has a number-average molecular weight of 40,000-80,000; Preferably, the antioxidant is selected from one or more of diisooctyldiphenylamine and N-phenyl-α-aniline; Preferably, the rust inhibitor is selected from one or more of benzotriazole, barium petroleum sulfonate, barium dinonylnaphthalene sulfonate, and alkenyl succinic acid; Preferably, the anti-wear agent is selected from one or more of zinc thiophosphate, aminothioester, and triphenyl thiophosphate.

6. A method for preparing a lubricating grease, characterized in that... Perform the following steps: A portion of the base oil, along with all the organic acids and saponified alkali solution, is mixed and reacted to obtain a base oil system containing a thickener. The remaining base oil is then added and mixed. After the first cooling, a thickener is added. After the second cooling, an antioxidant is added. After the third cooling, a rust inhibitor and an anti-wear agent are added and mixed thoroughly.

7. The preparation method according to claim 6, wherein, The process of mixing a portion of base oil and all organic acids and saponification alkali solution to obtain a base oil system containing a thickener includes: mixing 40-60 wt% of base oil based on the total amount of base oil with all 12-hydroxystearic acid, adding saponification alkali solution required for saponifying 12-hydroxystearic acid for a first reaction, and then adding sebacic acid and saponification alkali solution required for saponifying sebacic acid for a second reaction, thereby obtaining a base oil system containing a thickener; Preferably, the process of adding the remaining base oil for mixing includes: after all the sebacic acid and the required saponification alkali solution have been added, the system is heated to 160-170°C, the remaining base oil is added, and the temperature is further increased to 205-210°C and held at that temperature for 3-5 minutes.

8. The preparation method according to claim 7, wherein, The temperature of the first reaction is 92-98℃, and the reaction time is 20-30 min; Preferably, the process of adding sebacic acid and the saponification alkali solution required for saponifying sebacic acid to carry out the second reaction includes: after the first reaction is completed, the system is heated to 130-135°C, sebacic acid is added, then the temperature is raised to 140-145°C to melt the sebacic acid, and then the temperature is lowered to 127-133°C to add the saponification alkali solution required for saponifying sebacic acid in two batches.

9. The preparation method according to any one of claims 6-8, wherein, The system temperature after the first cooling is 150-160℃; Preferably, the system temperature after the second cooling is 110-120℃; Preferably, the system temperature after the third cooling is 95-105℃.

10. The application of the lubricating grease according to any one of claims 1-5 or the lubricating grease prepared by the preparation method according to any one of claims 6-9 in a barrier gate reducer; Preferably, the ambient temperature of the application is -40°C to 140°C.

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