CN115806851B - Grease composition with radiation resistance and preparation method thereof - Google Patents

Grease composition with radiation resistance and preparation method thereof Download PDF

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CN115806851B
CN115806851B CN202111074986.3A CN202111074986A CN115806851B CN 115806851 B CN115806851 B CN 115806851B CN 202111074986 A CN202111074986 A CN 202111074986A CN 115806851 B CN115806851 B CN 115806851B
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grease composition
base oil
acid
extreme pressure
total weight
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CN115806851A (en
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郑会
刘欣阳
庄敏阳
陈靖
何懿峰
李朝宇
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Sinopec Research Institute of Petroleum Processing
China Petroleum and Chemical Corp
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Sinopec Research Institute of Petroleum Processing
China Petroleum and Chemical Corp
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Abstract

The invention relates to the field of lubricating grease, and discloses a lubricating grease composition with radiation resistance and a preparation method thereof. The lubricating grease composition comprises base oil, a thickening agent and optional additives, wherein the weight ratio of the base oil is 1:0.3-3 of alkyl naphthalene and alkyl diphenyl ether, and the additive is at least one selected from the group consisting of a structure improver, an antioxidant, an antirust agent and an extreme pressure agent. The method of preparing the grease composition comprises: mixing part of base oil, water, acid and lithium precursor with a structure improver for saponification reaction, heating for refining, and then mixing with the rest of base oil and optional other additives, wherein the other additives are at least one selected from antioxidants, rust inhibitors and extreme pressure agents. The invention also discloses the lubricating grease composition prepared by the method. The lubricating grease composition disclosed by the invention has long service life, excellent radiation resistance, extreme pressure property, oxidation resistance, corrosion resistance and rust resistance, and can meet the lubricating requirement of a radiated working condition.

Description

Grease composition with radiation resistance and preparation method thereof
Technical Field
The invention relates to the field of lubricating grease, in particular to a lubricating grease composition with radiation resistance and a preparation method thereof.
Background
At present, greenhouse gas emission reduction and CO (carbon monoxide) are being promoted worldwide 2 The emission reduction demand promotes the development of clean energy, and nuclear power has certain advantages in the clean energy, and is one of important measures for stimulating internal needs and promoting economic development. The golden period of nuclear power construction and nuclear power industry development is coming, and the nuclear power industry enters a development stage of batch and industrialization, so that the prospect is better and better.
Because of the special working condition of the nuclear power station, the grease used is required to have excellent radiation resistance, and a great deal of researches are carried out on the radiation resistant grease by students at home and abroad. US3083160a reports the use of carbon black to thicken mineral oils and to add thickeners to prepare a radiation resistant grease. The composite lithium soap for CN1197838A is used for thickening mineral oil, and antioxidant, extreme pressure antiwear agent, antirust preservative and the like are added to develop the lubricating grease for the anti-radiation bearing and the lubricating grease for the anti-radiation gearbox.
With the development of nuclear power plants, new requirements are put forward on lubricating grease for nuclear power equipment, and general mineral oil-based lubricating oil cannot meet the use requirements. CN107805534A is thickened by polyurea powder to obtain alkyl diphenyl ether, and polytetrafluoroethylene, silicon dioxide and zinc oxide are added to prepare the special anti-radiation high-low temperature lubricating grease for the nuclear pump. The grease has excellent high and low temperature resistance, stability, long service life, oxidation resistance, ageing resistance and radiation resistance, and simultaneously has better extreme pressure abrasion resistance. CN105018208A adopts poly-alpha-olefin and metallocene PAO synthetic base oil as base oil, the thickening agent adopts toluene diisonitrile acid ester and calcium acetate, and simultaneously additives such as antioxidant, antirust agent, extreme pressure antiwear agent, adhesive agent and the like are added, and the prepared lubricating grease composition has excellent high temperature resistance, water spray resistance, pumping performance and extreme pressure performance. The CN104119993A is a mechanical lubricant prepared from perfluoropolyether oil and polytetrafluoroethylene, and has excellent high-temperature resistance, corrosion resistance, flame resistance and acid-base resistance and radiation resistance.
In the existing anti-radiation lubricating grease, the problems of short service life, small anti-radiation dosage, poor extreme pressure abrasion resistance, poor colloid stability and the like still exist, and the lubricating requirement of the working condition of high radiation dosage in the nuclear power station is difficult to meet.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provides a lubricating grease composition with radiation resistance and a preparation method thereof.
In order to achieve the above object, according to one aspect of the present invention, there is provided a grease composition having radiation resistance, the grease composition comprising a base oil, a thickener and optionally an additive, wherein the base oil is a mixture of 1:0.3-3 of alkyl naphthalene and alkyl diphenyl ether, wherein the additive is at least one selected from the group consisting of a structure improver, an antioxidant, an antirust agent and an extreme pressure agent.
In a second aspect, the present invention provides a method of preparing a grease composition, the method comprising: mixing part of base oil, water, acid and lithium precursor with a structure improver for saponification reaction, heating for refining, and then mixing the mixture with the rest of base oil and optional other additives, wherein the other additives are at least one selected from antioxidants, rust inhibitors and extreme pressure agents.
In a third aspect the present invention provides a grease composition obtainable by the method according to the second aspect.
The lubricating grease composition disclosed by the invention has long service life, and has excellent anti-radiation performance, extreme pressure performance, oxidation resistance, corrosion resistance and rust resistance, and can meet the lubricating requirement of a radiated working condition.
In the most preferred embodiment of the present invention, by blending a specific base oil, thickener, structure improver, antioxidant, rust inhibitor and extreme pressure agent in a specific ratio, a grease composition having a longer life, excellent extreme pressure performance, colloid stability and oxidation stability can be obtained.
Detailed Description
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
In a first aspect, the invention provides a grease composition with radiation resistance, which comprises base oil, a thickening agent and optional additives, and is characterized in that the weight ratio of the base oil is 1:0.3-3 of alkyl naphthalene and alkyl diphenyl ether, wherein the additive is at least one selected from the group consisting of a structure improver, an antioxidant, an antirust agent and an extreme pressure agent.
According to the present invention, preferably, the weight ratio between the alkyl naphthalene and the alkyl diphenyl ether is 1:0.4-2.1.
According to the invention, the base oil is preferably present in an amount of 70 to 92 wt.%, more preferably 78 to 90 wt.%, based on the total weight of the grease composition.
According to the invention, the lubricating base oil is a mixed oil of alkyl naphthalene and alkyl diphenyl ether, the alkyl naphthalene base oil preferably having a kinematic viscosity of 10 to 30mm at 100 DEG C 2 And/s. The alkyl diphenyl ether base oil preferably has a kinematic viscosity of 10-20mm at 100 DEG C 2 Lubricating base oil/s. The "kinematic viscosity" test method was GB/T30515.
According to the invention, the thickener is preferably used in an amount of 5 to 20 wt.%, more preferably 8 to 15 wt.%, based on the total weight of the grease composition.
According to a preferred embodiment of the invention, the thickener used is a composite lithium-based thickener, produced by the reaction of an acid with lithium hydroxide, said acid being a mixed acid of a high-molecular acid and a low-molecular acid. The high molecular acid is C12-C20 fatty acid and/or C12-C20 hydroxy fatty acid, and can be one or more of lauric acid, palmitic acid, stearic acid and 12-hydroxy stearic acid, preferably stearic acid and 12-hydroxy stearic acid; the low molecular acid is C2-C11 organic acid, and can be one or more of acetic acid, propionic acid, oxalic acid, adipic acid, azelaic acid, sebacic acid and terephthalic acid, preferably one or more of sebacic acid, azelaic acid, adipic acid and terephthalic acid. Wherein the molar ratio of the high molecular acid to the low molecular acid is preferably 1:0.3-1. The molar ratio of the total amount of the high-molecular acid and the low-molecular acid to lithium hydroxide is preferably stoichiometric, wherein the amount of lithium hydroxide may also be in excess of 1 to 10% by weight. The amount of water in the aqueous solution of lithium hydroxide is generally 0.1 to 10 times by weight, preferably 0.5 to 5 times by weight, the amount of lithium hydroxide used, in order to allow the saponification reaction to proceed smoothly. Although water is used in the obtaining of the thickener, water will eventually be removed from the grease composition.
According to the invention, the content of the structure improving agent is preferably 0.1 to 5 wt.%, more preferably 0.2 to 0.8 wt.%, based on the total weight of the grease composition.
According to the invention, the structure-improving agent is preferably silica. The particle size of the silica is preferably in the range of 1-100 nm.
According to the invention, the antioxidant is preferably present in an amount of 0.1 to 3 wt.%, more preferably 0.5 to 1.5 wt.%, based on the total weight of the grease composition.
According to the present invention, the antioxidant is preferably an aromatic amine type antioxidant, and may be, for example, one or more of diphenylamine, diisooctyldiphenylamine, β -naphthylamine, N-phenyl- α -naphthylamine, N-phenyl- β -naphthylamine, N-isopropyl-N '-phenyl-p-phenylenediamine, N-cyclohexyl-N' -phenyl-p-phenylenediamine, N '-di- β -naphthylp-phenylenediamine, and N, N' -di-sec-butyl-p-phenylenediamine.
According to the present invention, the rust inhibitor is preferably contained in an amount of 0.1 to 10% by weight, more preferably 0.5 to 5% by weight, based on the total weight of the grease composition.
According to the invention, the rust inhibitor is preferably an organic sulfonate type rust inhibitor, such as one or more of barium petroleum sulfonate, sodium petroleum sulfonate, barium dinonyl naphthalene sulfonate, zinc dinonyl naphthalene sulfonate, and zinc naphthenate.
According to the invention, the extreme pressure agent is preferably present in an amount of 1 to 10 wt.%, more preferably 2 to 5 wt.%, based on the total weight of the grease composition.
According to the invention, the extreme pressure agent is preferably a solid extreme pressure agent with a layered structure, such as at least one of molybdenum disulfide, tungsten disulfide, graphite, graphene and fullerene.
According to the present invention, preferably, the weight ratio between the antioxidant, the rust inhibitor and the extreme pressure agent is 1:1-5:2-8, more preferably 1:2-4:3-6.
According to the invention, the grease composition consists of only the above components.
According to the present invention, by blending a preferable base oil, a thickener, a structure improver, an antioxidant, a rust inhibitor, and an extreme pressure agent in a preferable ratio, a grease composition having more excellent performance can be obtained.
The grease of the present invention can be produced in a conventional manner as long as it contains the above-mentioned components. However, preferably, the saponification reaction is performed in the presence of a structure improver and the thickener is synthesized in situ, and the saponification reaction performed in the presence of the structure improver can further improve the colloidal stability of the grease while shortening the saponification time. Accordingly, in a second aspect, the present invention provides a method of preparing a grease composition, the method comprising: mixing part of base oil, water, acid and lithium precursor with a structure improver for saponification reaction, heating for refining, and then mixing the mixture with the rest of base oil and optional other additives, wherein the other additives are at least one selected from antioxidants, rust inhibitors and extreme pressure agents.
Preferably, the preparation method of the grease composition comprises the following steps: mixing part of base oil, a structure improver, high molecular acid and low molecular acid, heating to 80-95 ℃, adding aqueous solution of lithium hydroxide for saponification reaction, heating to 190-220 ℃ for high-temperature refining, adding the rest of base oil, cooling to 100-120 ℃, adding necessary additives, and grinding into grease to obtain a finished product. Wherein the saponification reaction time is preferably 0.2-1.5 hours, and the refining time is preferably 5-20 minutes.
Those skilled in the art can obtain the amounts of the various raw materials used in the preparation method of the second aspect according to the contents of the base oil, the thickener and the additive, and are not described herein.
In a third aspect, the present invention provides a grease composition obtainable by the method according to the second aspect.
The present invention will be described in detail by examples. The performance evaluations in the following examples and comparative examples were performed as follows:
the higher the value, the better the high temperature performance is indicated by using the GB/T3498 method for measuring the dropping point;
the cone penetration is measured by using a GB/T269 method, and the smaller the value is, the thicker the grease is;
the method of GB/T5018 is adopted for measuring the corrosion resistance;
determination of four-ball machine test P D The SH/T0202 method is adopted, the larger the value is, the better the extreme pressure performance is;
the corrosion performance of the copper sheet is measured by using a GB/T7326 method;
the method of NB/SH/T0324 is adopted for measuring the oil separation performance of the steel mesh, and the smaller the value is, the less the oil separation is;
the oxidation resistance (oxidation stability) is measured by adopting an SH/T0325 method, and the smaller the value is, the better the oxidation stability is;
the longer the value, the longer the life is measured by SH/T0773 method;
the saponification reaction time is measured by the time required for visual inspection of the materials in the fat-making kettle to become completely fat-like;
the sources of the main raw materials used are shown in Table 1.
TABLE 1
Example 1
The raw material components are as follows: alkyl diphenyl ether base oil AD12 42kg; alkyl naphthalene AN15 kg; 8.2kg of 12-hydroxystearic acid; azelaic acid 1.5kg; 1.9kg of lithium hydroxide monohydrate; 0.2kg of silicon dioxide; 0.8kg of diphenylamine; 2.4kg of barium petroleum sulfonate; molybdenum disulfide 2.6kg
Adding 60kg of mixed base oil, 0.2kg of silicon dioxide, 8.2kg of 12-hydroxystearic acid and 1.5kg of azelaic acid into a lipid preparation kettle, heating and stirring, heating to 80 ℃, adding lithium hydroxide aqueous solution (containing 1.9kg of lithium hydroxide and 5kg of water) for saponification reaction for 0.2h, and heating to 190 ℃ for high-temperature refining for 20min; after the rest mixed base oil is added and cooled to 105 ℃, 1kg of diphenylamine, 2.4kg of barium petroleum sulfonate and 2.4kg of molybdenum disulfide are added, the mixture is stirred and cooled to room temperature, and the mixture is ground for 2 times by a three-roller mill to form grease. The product properties are shown in Table 2.
The contents of the respective components in the grease obtained in this example are calculated from the amounts of the materials charged are shown in Table 2.
Example 2
The raw material components are as follows: 15 kg of alkyl diphenyl ether base oil AD; alkyl naphthalene AN 23.1 kg; 8.7kg of 12-hydroxystearic acid; 2.9kg of sebacic acid; 2.6kg of lithium hydroxide monohydrate; 0.4kg of silicon dioxide; 0.5kg of diisooctyl diphenylamine; 2kg of petroleum sodium sulfonate; tungsten disulfide 3kg
Adding 62kg of mixed base oil, 0.4kg of silicon dioxide, 8.7kg of 12-hydroxystearic acid and 2.9kg of sebacic acid into a fat preparation kettle, heating and stirring, heating to 90 ℃, adding lithium hydroxide aqueous solution (containing 2.6kg of lithium hydroxide and 13kg of water) for saponification reaction for 0.5h, and heating to 200 ℃ for high-temperature refining for 10min; after the rest mixed base oil is added and cooled to 115 ℃, 0.5kg of diisooctyl diphenylamine, 2kg of petroleum sodium sulfonate and 3kg of tungsten disulfide are added, the mixture is stirred and cooled to room temperature, and the mixture is ground for 2 times by a three-roller machine to form grease. The product properties are shown in Table 2.
The contents of the respective components in the grease obtained in this example are calculated from the amounts of the materials charged are shown in Table 2.
Example 3
The raw material components are as follows: alkyl diphenyl ether base oil AD12 55kg; 30 kg of alkyl naphthalene AN; 6.8kg of stearic acid; 2.8kg of adipic acid; 2.8kg of lithium hydroxide monohydrate; 0.6kg of silicon dioxide; 1.2kg of beta-naphthylamine; 3kg of barium dinonyl naphthalene sulfonate; graphite 4.2kg
Adding 60kg of mixed base oil, 0.6kg of silicon dioxide, 6.8kg of stearic acid and 2.8kg of adipic acid into a lipid preparation kettle, heating and stirring, heating to 85 ℃, adding lithium hydroxide aqueous solution (containing 2.8kg of lithium hydroxide and 10kg of water) for saponification reaction for 0.3h, and heating to 205 ℃ for high-temperature refining for 15min; after the rest mixed base oil is added and cooled to 110 ℃, 1.2kg of beta-naphthylamine, 3kg of barium dinonyl naphthalene sulfonate and 4.2kg of graphite are added, the mixture is stirred and cooled to room temperature, and the mixture is ground for 2 times by a three-roller machine to form grease. The product properties are shown in Table 2.
The contents of the respective components in the grease obtained in this example are calculated from the amounts of the materials charged are shown in Table 2.
Example 4
The raw material components are as follows: alkyl diphenyl ether base oil AD15 kg; alkyl naphthalene AN23 kg; 7.3kg of stearic acid; 4.2kg of terephthalic acid; 3.4kg of lithium hydroxide monohydrate; 0.8kg of silicon dioxide; 1.5kg of N-phenyl-beta-naphthylamine; 3kg of zinc dinonyl naphthalene sulfonate; graphene 4.7kg
Adding 60kg of mixed base oil, 0.8kg of silicon dioxide, 7.3kg of stearic acid and 4.2kg of terephthalic acid into a fat preparation kettle, heating and stirring, heating to 95 ℃, adding lithium hydroxide aqueous solution (containing 3.4kg of lithium hydroxide and 10kg of water) for saponification reaction for 0.5h, and heating to 205 ℃ for high-temperature refining for 10min; after the rest mixed base oil is added and cooled to 110 ℃, 1.5kg of N-phenyl-beta-naphthylamine, 3kg of zinc dinonyl naphthalene sulfonate and 4.7kg of graphene are added, the mixture is stirred and cooled to room temperature, and the mixture is ground for 2 times by a three-roller machine to form grease. The product properties are shown in Table 2.
The contents of the respective components in the grease obtained in this example are calculated from the amounts of the materials charged are shown in Table 2.
Example 5
Grease was prepared as in example 1, except that the amount of diphenylamine used was 1kg; the dosage of the barium petroleum sulfonate is 4kg; the molybdenum disulfide was used in an amount of 0.8kg. The product performance test results and the contents of the components in the grease obtained in this example are shown in Table 2.
Example 6
Grease was prepared as in example 2, except that the amount of diisooctyldiphenylamine used was 1kg; the dosage of the petroleum sodium sulfonate is 3.5kg; the amount of tungsten disulfide used was 1kg. The product performance test results and the contents of the components in the grease obtained in this example are shown in Table 2.
Example 7
Grease was prepared as in example 3, except that the amount of beta-naphthylamine was 1kg; the dosage of the barium dinonyl naphthalene sulfonate is 1kg; the amount of graphite was 7kg. The product performance test results and the contents of the components in the grease obtained in this example are shown in Table 2.
Example 8
Grease was prepared as in example 4, except that 1kg of N-phenyl- β -naphthylamine was used; the dosage of zinc dinonyl naphthalene sulfonate is 6kg; the amount of graphene was 1.2kg. The product performance test results and the contents of the components in the grease obtained in this example are shown in Table 2.
Example 9
Grease was prepared as in example 1, except that no silica was added, as follows:
the raw material components are as follows: alkyl diphenyl ether base oil AD12 42kg; alkyl naphthalene AN15 kg; 8.2kg of 12-hydroxystearic acid; azelaic acid 1.5kg; 1.9kg of lithium hydroxide monohydrate; 1kg of diphenylamine; 3kg of barium petroleum sulfonate; molybdenum disulfide 4kg
Adding 60kg of mixed base oil, 8.2kg of 12-hydroxystearic acid and 1.5kg of azelaic acid into a lipid preparation kettle, heating and stirring, heating to 80 ℃, adding lithium hydroxide aqueous solution (containing 1.9kg of lithium hydroxide and 5kg of water) for saponification reaction for 1.5h, and heating to 190 ℃ for refining for 20min; adding the rest mixed base oil, cooling to 105 ℃, adding 1kg of diphenylamine, 3kg of barium petroleum sulfonate and 4kg of molybdenum disulfide, stirring, cooling to room temperature, and grinding for 2 times by a three-roller machine to form grease. The product properties are shown in Table 2.
The contents of the respective components in the grease obtained in this example are calculated from the amounts of the materials charged are shown in Table 2.
Comparative example 1
A grease was prepared as in example 1, except that both the alkyl diphenyl ether base oil AD12 and the alkyl naphthalene AN15 were replaced with 500SN base oil. The product performance test results and the contents of the components in the grease obtained in this example are shown in Table 2.
Example 10
Grease was prepared as in example 2, except that the antioxidants, rust inhibitors and extreme pressure agents were replaced, specifically as follows:
the raw material components are as follows: 15 kg of alkyl diphenyl ether base oil AD; alkyl naphthalene AN 23.1 kg; 8.7kg of 12-hydroxystearic acid; 2.9kg of sebacic acid; 2.6kg of lithium hydroxide monohydrate; 0.4kg of silicon dioxide; 0.5kg of 2, 6-di-tert-butyl-4-methylphenol; 2kg of benzotriazole; potassium metaborate 3kg
Adding 62kg of mixed base oil, 0.4kg of silicon dioxide, 8.7kg of 12-hydroxystearic acid and 2.9kg of sebacic acid into a fat preparation kettle, heating and stirring, heating to 90 ℃, adding lithium hydroxide aqueous solution (containing 2.6kg of lithium hydroxide and 13kg of water) for saponification reaction for 0.5h, and heating to 200 ℃ for high-temperature refining for 10min; after the rest mixed base oil is added and cooled to 115 ℃, 0.5kg of 2, 6-di-tert-butyl-4-methylphenol, 2kg of benzotriazole and 3kg of potassium metaborate are added, stirred and cooled to room temperature, and ground for 2 times by a three-roll mill to form grease. The product properties are shown in Table 2.
The contents of the respective components in the grease obtained in this example are calculated from the amounts of the materials charged are shown in Table 2.
TABLE 2
Example 11
The raw material components are as follows: alkyl diphenyl ether base oil AD12 50kg; 30 kg of alkyl naphthalene AN; 15.4kg of organic bentonite; acetone 0.2kg; 0.6kg of silicon dioxide; 1kg of 2, 6-di-tert-butyl-4-methylphenol; 6kg of benzotriazole;
firstly, adding 55kg of mixed base oil, 0.6kg of silicon dioxide and 15.4kg of organic bentonite into a fat preparation kettle, heating and stirring, heating to 40 ℃, adding acetone, dispersing for 1h, heating to 105 ℃, and carrying out high-temperature refining for 15min; after the rest mixed base oil is added and cooled to 110 ℃, 1kg of 2, 6-di-tert-butyl-4-methylphenol and 6kg of benzotriazole are added, the mixture is stirred and cooled to room temperature, and the mixture is ground for 2 times by a three-roller machine to form grease. The results of the product performance test are shown in Table 3.
Example 12
The raw material components are as follows: alkyl diphenyl ether base oil AD12 50kg; 30 kg of alkyl naphthalene AN; 8.5kg of calcium hydroxide; 4.5kg of acetic acid; 3kg of sebacic acid; 0.6kg of silicon dioxide; 1kg of potassium metaborate; 6kg of benzotriazole;
adding 55kg of mixed base oil, 0.6kg of silicon dioxide and 17kg of calcium hydroxide emulsion (8.5 kg of calcium hydroxide and 8.5kg of water) into a fat manufacturing kettle, heating and stirring, heating to 40 ℃, adding 4.5kg of acetic acid, heating to 90 ℃, adding 3kg of sebacic acid, performing saponification reaction for 1h, and heating to 205 ℃ for refining for 15min; after the rest mixed base oil is added and cooled to 1100 ℃, 1kg of 2,6 potassium metaborate and 6kg of benzotriazole are added, the mixture is stirred and cooled to room temperature, and the mixture is ground for 2 times by a three-roller machine to form grease. The results of the product performance test are shown in Table 3.
Example 13
The raw material components are as follows: alkyl diphenyl ether base oil AD12 50kg; 30 kg of alkyl naphthalene AN; 15.4kg of organic bentonite; acetone 0.2kg; 0.6kg of silicon dioxide; 1kg of 2, 6-di-tert-butyl-4-methylphenol; 1kg of potassium metaborate;
firstly, adding 55kg of mixed base oil, 0.6kg of silicon dioxide and 15.4kg of organic bentonite into a fat preparation kettle, heating and stirring, heating to 40 ℃, adding acetone, dispersing for 1h, heating to 105 ℃, and carrying out high-temperature refining for 15min; after the rest mixed base oil is added and cooled to 110 ℃, 1kg of 2, 6-di-tert-butyl-4-methylphenol and 1kg of potassium metaborate are added, the mixture is stirred and cooled to room temperature, and the mixture is ground for 2 times by a three-roller machine to form grease. The results of the product performance test are shown in Table 3.
Example 14
Grease was prepared as in example 2, except that silicon dioxide was added together with tungsten disulfide (saponification was not performed in the presence of silicon dioxide), and the time for saponification was 1.5h. The results of the product performance test are shown in Table 3.
Example 15
Grease was prepared as in example 2, except that the amount of silica used was 2kg and the saponification time was 0.5h. The results of the product performance test are shown in Table 3.
Comparative example 2
Grease was prepared as in example 2, except that both alkyl naphthalene and alkyl diphenyl ether were replaced with poly-alpha-olefins (PAO synthetic base oils, source Shanghai Nake lubricating technologies Co.). The results of the product performance test are shown in Table 3.
Comparative example 3
A grease was prepared as in example 2, except that the amount of alkyl naphthalene was 13.1kg and the amount of alkyl diphenyl ether was 69kg. The results of the product performance test are shown in Table 3.
TABLE 3 Table 3
From the above results, it can be seen that examples 1 to 4 employing the preferred embodiment of the present invention have longer life, superior colloid stability, extreme pressure property, and oxidation stability. From the results of examples 1-4, examples 5-8 and example 10, it can be seen that the specific antioxidants, rust inhibitors and extreme pressure agents are compounded in a specific ratio to have a synergistic effect, so that the grease product has excellent anti-radiation performance, rust resistance, extreme pressure performance, colloid stability and oxidation resistance. It can be seen from examples 1-4 and examples 11-13 that base oils, thickeners and additives were compounded in specific kinds and amounts to obtain greases with better properties. It can be seen from examples 1 to 4 and examples 14 to 15 that the saponification reaction is carried out in the presence of a specific amount of silica to obtain a grease having more excellent properties, and that the saponification reaction in the presence of silica can further improve the colloidal stability of the grease while shortening the saponification time.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.

Claims (10)

1. A grease composition with radiation resistance, comprising a base oil, a thickener and optionally additives, characterized in that the base oil is in a weight ratio of 1:0.3-3 of alkyl naphthalene and alkyl diphenyl ether, wherein the additive is at least one selected from the group consisting of a structure improver, an antioxidant, an antirust agent and an extreme pressure agent.
2. The grease composition of claim 1, wherein the weight ratio of alkyl naphthalene to alkyl diphenyl ether is 1:0.4-2.1;
and/or the base oil is present in an amount of 70 to 92 wt.%, based on the total weight of the grease composition.
3. The grease composition according to claim 1 or 2, wherein the base oil is present in an amount of 78-90 wt.%, based on the total weight of the grease composition;
and/or the alkyl naphthalene has a kinematic viscosity at 100 ℃ of 10-30mm 2 /s;
And/or the kinematic viscosity of the alkyl diphenyl ether at 100 ℃ is 10-20mm 2 /s。
4. The grease composition according to claim 1, wherein the thickener is used in an amount of 5-20 wt%, based on the total weight of the grease composition;
and/or, the content of the structure improver is 0.1-5 wt% based on the total weight of the lubricating grease composition;
and/or, the antioxidant is present in an amount of 0.1 to 3 wt.%, based on the total weight of the grease composition;
and/or, the rust inhibitor is contained in an amount of 0.1 to 10 wt% based on the total weight of the grease composition;
and/or, the extreme pressure agent is present in an amount of 1 to 10 wt.%, based on the total weight of the grease composition;
and/or the weight ratio of the antioxidant, the rust inhibitor and the extreme pressure agent is 1:1-5:2-8.
5. The grease composition of claim 4, wherein the thickener is used in an amount of 8-15 wt%, based on the total weight of the grease composition;
and/or, the content of the structure improver is 0.2-0.8 wt% based on the total weight of the lubricating grease composition;
and/or, the antioxidant is present in an amount of 0.5 to 1.5 wt.%, based on the total weight of the grease composition;
and/or, the rust inhibitor is present in an amount of 0.5 to 5 wt.%, based on the total weight of the grease composition;
and/or, the extreme pressure agent is present in an amount of 2 to 5 wt.%, based on the total weight of the grease composition;
and/or the weight ratio of the antioxidant, the rust inhibitor and the extreme pressure agent is 1:2-4:3-6.
6. The grease composition of claim 1, 4 or 5, wherein the thickener is a complex lithium-based thickener;
and/or, the structure modifier is selected from silica;
and/or the antioxidant is selected from aromatic amine type antioxidants;
and/or, the rust inhibitor is selected from organic sulfonate type rust inhibitors;
and/or the extreme pressure agent is selected from solid extreme pressure agents having a layered structure.
7. The grease composition of claim 1, wherein the thickener is generated by the reaction of an acid with lithium hydroxide, the acid being a mixed acid of a high molecular acid and a low molecular acid; wherein the high molecular acid is C12-C20 fatty acid and/or C12-C20 hydroxy fatty acid; the low molecular acid is C2-C11 organic acid.
8. The grease composition of claim 1, 4 or 5, wherein the structure modifier is selected from silica having a particle size in the range of 1-100 nm;
and/or the antioxidant is selected from at least one of diphenylamine, diisooctyldiphenylamine, beta-naphthylamine, N-phenyl-alpha-naphthylamine, N-phenyl-beta-naphthylamine, N-isopropyl-N '-phenyl-p-phenylenediamine, N-cyclohexyl-N' -phenyl-p-phenylenediamine, N '-di-beta-naphthyl-p-phenylenediamine and N, N' -di-sec-butyl-p-phenylenediamine;
and/or the rust inhibitor is selected from at least one of barium petroleum sulfonate, sodium petroleum sulfonate, barium dinonyl naphthalene sulfonate, zinc dinonyl naphthalene sulfonate and zinc naphthenate;
and/or the extreme pressure agent is selected from at least one of molybdenum disulfide, tungsten disulfide, graphite, graphene and fullerene.
9. A method of preparing a grease composition, the method comprising: mixing part of base oil, water, acid and lithium precursor with a structure improver for saponification reaction, heating for refining, and then mixing the mixture with the rest of base oil and optional other additives, wherein the other additives are at least one selected from antioxidants, rust inhibitors and extreme pressure agents.
10. A grease composition made by the method of claim 9.
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US6673750B2 (en) * 2001-02-22 2004-01-06 Ntn Corporation Lubricating composition

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JPH10279974A (en) * 1997-04-02 1998-10-20 Nippon Oil Co Ltd Grease composition
CN1197838A (en) * 1997-04-09 1998-11-04 中国石油化工总公司 Lubricating grease for gear box in nuclear power station
CN112375607A (en) * 2020-11-25 2021-02-19 青岛中科润美润滑材料技术有限公司 Tetraurea lubricating grease composition and preparation method thereof

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