CN112522017B - Composite barium-based lubricating grease and preparation method thereof - Google Patents
Composite barium-based lubricating grease and preparation method thereof Download PDFInfo
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- CN112522017B CN112522017B CN201910876070.6A CN201910876070A CN112522017B CN 112522017 B CN112522017 B CN 112522017B CN 201910876070 A CN201910876070 A CN 201910876070A CN 112522017 B CN112522017 B CN 112522017B
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
- C10M169/06—Mixtures of thickeners and additives
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M117/00—Lubricating compositions characterised by the thickener being a non-macromolecular carboxylic acid or salt thereof
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
- C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
- C10M2205/028—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers containing aliphatic monomers having more than four carbon atoms
- C10M2205/0285—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers containing aliphatic monomers having more than four carbon atoms used as base material
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/02—Hydroxy compounds
- C10M2207/023—Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings
- C10M2207/026—Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings with tertiary alkyl groups
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2207/121—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms
- C10M2207/122—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms monocarboxylic
- C10M2207/1225—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms monocarboxylic used as thickening agent
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
- C10M2207/126—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids monocarboxylic
- C10M2207/1265—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids monocarboxylic used as thickening agent
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/14—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings
- C10M2207/141—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings monocarboxylic
- C10M2207/1415—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings monocarboxylic used as thickening agent
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
- C10M2215/06—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to carbon atoms of six-membered aromatic rings
- C10M2215/064—Di- and triaryl amines
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Lubricants (AREA)
Abstract
The invention relates to the technical field of lubricating grease, in particular to composite barium-based lubricating grease and a preparation method thereof. The lubricating grease comprises base oil and a thickening agent, wherein the thickening agent is prepared from composite acid and barium hydroxide, and the composite acid comprises stearic acid, terephthalic acid and acetic acid. By optimizing the formula of the lubricating grease (especially compounding the composite acid in the thickening agent), the lubricating grease has good performances of extreme pressure wear resistance, high temperature resistance, mechanical stability, salt water resistance, adhesion, corrosion resistance and the like, is a multi-effect lubricating grease, and has wide application prospect. The preparation method can well exert the performance of each component in the formula, thereby further improving the performance of each aspect of the lubricating grease; and the process is simple, the cost is low, and the popularization and the application of the lubricating grease are convenient.
Description
Technical Field
The invention relates to the technical field of lubricating grease, in particular to composite barium-based lubricating grease and a preparation method thereof.
Background
The composite barium-base lubricating grease is made up by using composite barium soap thickened base oil produced by reaction of two or more than two acids and barium hydroxide, and possesses excellent mechanical stability and colloid stability, and its characteristics of resisting extreme pressure, resisting wear, resisting high temp., resisting water and long service life are used as one of the lubricating grease varieties with good development prospect. In recent years, with the development of modern industry in China, more rigorous requirements on the performance of lubricating grease are put forward in the industries of bearings, metallurgy, automobiles, textile, printing and dyeing and the like. Ordinary greases have difficulty meeting such demanding lubrication requirements.
The preparation method of the composite barium grease is mentioned in many patents at home and abroad, such as: US2417433A and US2033148 describe in detail the preparation method of barium complex grease; CN1160754A adopts one-step saponification compounding process, and uses C 16 -C 20 The reactant of the fatty acid, the sebacic acid and the barium hydroxide is a thickening agent, and the viscosity is 15-30mm at 100 DEG C 2 Mineral oil/s base oil, aromatic amine and lithium salicylateThe composite is an antioxidant, and is prepared by adding an antirust agent and a filler, and the composite barium-based lubricating grease has excellent high temperature property, oxidation stability, water resistance and extreme pressure wear resistance, and is multi-effect lubricating grease; CN105219504A introduces a preparation method of a composite barium composition, the lubricating grease is applied to a high-speed motor main shaft bearing, a reactant of a mixture of stearic acid and acetic acid and barium hydroxide is used as a thickening agent, II-class hydrogenated mineral oil is used as base oil, and amines and phenols are used as antioxidants, and the lubricating grease is prepared by adopting a special refining process.
Most of the above patents adopt two kinds of acid and barium hydroxide as thickeners, and the prepared grease has poor shear stability and colloid stability, and cannot meet the requirements of certain specific grease using conditions.
Disclosure of Invention
In order to solve the technical problems, the invention provides a multi-effect composite barium-based lubricating grease and a preparation method thereof.
The invention aims to provide composite barium-based lubricating grease which comprises base oil and a thickening agent, wherein the thickening agent is prepared from composite acid and barium hydroxide, and the composite acid comprises stearic acid, terephthalic acid and acetic acid.
In the research and development process, the thickening agent obtained by reacting the barium hydroxide and the composite acid formed by compounding stearic acid, terephthalic acid and acetic acid is found to have better high temperature resistance, water resistance and extreme pressure wear resistance when being applied to lubricating grease, and can also give consideration to shear stability and colloid stability, so that the thickening agent is suitable for more grease using working conditions.
Preferably, the composite acid consists of stearic acid, terephthalic acid and acetic acid; preferably, the molar ratio of stearic acid, terephthalic acid and acetic acid is 1.3-0.5.
Under the above proportion, the shear stability and colloid stability of the grease are further improved.
In order to further improve various performances of the lubricating grease, the invention researches the base oil and the additive which have better compounding effect with the thickening agent to obtain the following preferred technical scheme:
preferably, the base oil is a polyalphaolefin synthetic oil.
Preferably, the poly-alpha-olefin synthetic oil has a kinematic viscosity at 40 ℃ of 20 to 50mm 2 /s。
Preferably, the grease further comprises an antioxidant, and the antioxidant comprises an amine antioxidant and a phenol antioxidant.
Preferably, the amine antioxidant is diisooctyl diphenylamine.
Preferably, the phenolic antioxidant is 2,6-di-tert-butyl-p-cresol.
Preferably, the antioxidant consists of diisooctyl diphenylamine and 2,6-di-tert-butyl-p-cresol; preferably, the weight ratio of the diisooctyldiphenylamine to the 2,6-di-tert-butyl-p-cresol is 1.8-1.2; more preferably 1:1.
as a preferable scheme of the invention, the lubricating grease is prepared from the following raw materials in parts by weight:
base oil: 65-85 parts;
a thickening agent: 15-35 parts;
antioxidant: 0.1-2 parts;
the base oil is poly-alpha olefin synthetic oil;
the thickening agent is prepared from composite acid and barium hydroxide, wherein the composite acid is composed of stearic acid, terephthalic acid and acetic acid with the molar ratio of 1;
the antioxidant consists of diisooctyl diphenylamine and 2,6-di-tert-butyl-p-cresol in the weight ratio of 1.8-1.2.
By combining the preferred embodiments of the present invention, an embodiment with better effects can be obtained.
The second purpose of the invention is to provide a method for preparing the lubricating grease, which comprises the following steps:
(1) Mixing part (preferably 2/3 mass) of the base oil with stearic acid, terephthalic acid, acetic acid and heating to 85-95 deg.C;
(2) Adding excessive barium hydroxide aqueous solution for saponification for 1.5-2h;
(3) Heating to 180-200 deg.C after saponification, and refining for 10-20min;
(4) After refining, adding the rest base oil, cooling to 80-100 ℃, and adding an antioxidant.
The invention searches for the optimal preparation method of the lubricating grease, and finds that the lubricating grease prepared by the method can well exert the performance of each component in the formula, so that the performance of each aspect of the lubricating grease is further improved.
Preferably, the method further comprises: and (5) grinding for 3 times by a three-roller machine.
The invention has the following beneficial effects:
(1) By optimizing the formula of the lubricating grease (especially compounding the composite acid in the thickening agent), the lubricating grease has good performances of extreme pressure wear resistance, high temperature resistance, mechanical stability, salt water resistance, adhesion, corrosion resistance and the like, is a multi-effect lubricating grease, and has wide application prospect.
(2) The preparation method can well exert the performance of each component in the formula, thereby further improving the performance of each aspect of the lubricating grease; and the process is simple, the cost is low, and the popularization and the application of the lubricating grease are convenient.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example 1
Firstly, 595.2g of base oil is added into a reaction kettle, 227.2g of stearic acid, 39.8g of terephthalic acid and 4.8g of acetic acid are added, the molar ratio of stearic acid to terephthalic acid to acetic acid is 1.3. After the saponification reaction is finished, the temperature is raised to the maximum refining temperature of 200 ℃, the refining is continued for 15min, after the refining is finished, the heating is closed, the rest 297.6g of base oil is added, when the temperature is cooled to be below 100 ℃, 13.1g of diisooctyl diphenylamine antioxidant and 13.1g of 2,6-di-tert-butyl-p-cresol are added, and the lubricating grease is ground for 3 times through a three-roller machine.
Example 2
Firstly, 643.7g of base oil is added into a reaction kettle, 227.2g of stearic acid, 39.8g of terephthalic acid and 9.6g of acetic acid are added, the molar ratio of stearic acid to terephthalic acid to acetic acid is 1.3. After the saponification reaction is finished, the temperature is raised to the maximum refining temperature of 200 ℃, the refining is continued for 15min, after the refining is finished, the heating is closed, the rest 321.8g of base oil is added, when the temperature is cooled to be below 100 ℃, 14.0g of antioxidant diisooctyl diphenylamine and 14.0g of 2,6-di-tert-butyl-p-cresol are added, and the lubricating grease is ground for 3 times through a three-roller machine.
Example 3
Firstly, 702.7g base oil is added into a reaction kettle, 227.2g stearic acid, 53.1g terephthalic acid and 4.8g acetic acid are added, the molar ratio of stearic acid to terephthalic acid to acetic acid is 1: 0.1, the temperature is raised to 90 ℃, 136.5g barium hydroxide and a proper amount of water are prepared to obtain a barium hydroxide aqueous solution, the barium hydroxide aqueous solution is poured into the reaction kettle, and saponification reaction is carried out for 1.5-2 hours. After the saponification reaction is finished, the temperature is raised to the maximum refining temperature of 200 ℃, the refining is continued for 15min, after the refining is finished, the heating is closed, the rest 351.3g of base oil is added, when the temperature is cooled to be below 100 ℃, 15.1g of diisooctyl diphenylamine antioxidant and 15.1g of 2,6-di-tert-butyl-p-cresol are added, and the lubricating grease is ground for 3 times through a three-roller machine.
Example 4
Firstly, 722.5g of base oil is added into a reaction kettle, 227.2g of stearic acid, 53.1g of terephthalic acid and 9.6g of acetic acid are added, the molar ratio of stearic acid to terephthalic acid to acetic acid is 1.4. After the saponification reaction is finished, the temperature is raised to the maximum refining temperature of 200 ℃, the refining is continued for 15min, after the refining is finished, the heating is closed, the rest 361.2g of base oil is added, when the temperature is cooled to be below 100 ℃, 15.5g of diisooctyl diphenylamine antioxidant and 15.5g of 2,6-di-tert-butyl-p-cresol are added, and the lubricating grease is ground for 3 times through a three-roller machine.
Example 5
Firstly, 721.0g of base oil is added into a reaction kettle, 227.2g of stearic acid, 66.4g of terephthalic acid and 4.8g of acetic acid are added, the molar ratio of stearic acid to terephthalic acid to acetic acid is 1.5. After the saponification reaction is finished, heating to the maximum refining temperature of 200 ℃ for 15min, stopping heating after refining is finished, adding the rest 360.4g of base oil, cooling to the temperature below 100 ℃, adding 15.7g of diisooctyl diphenylamine serving as an antioxidant and 15.7g of 2,6-di-tert-butyl-p-cresol into the mixture, and grinding the lubricating grease for 3 times by a three-roller machine.
Example 6
Firstly, 768.7g of base oil is added into a reaction kettle, 227.2g of stearic acid, 66.4g of terephthalic acid and 9.6g of acetic acid are added, the molar ratio of stearic acid to terephthalic acid to acetic acid is 1.5. After the saponification reaction is finished, the temperature is raised to the maximum refining temperature of 200 ℃, the refining is continued for 15min, after the refining is finished, the heating is closed, the rest 384.3g of base oil is added, when the temperature is cooled to be below 100 ℃, 16.5g of diisooctyl diphenylamine antioxidant and 16.5g of 2,6-di-tert-butyl-p-cresol are added, and the lubricating grease is ground for 3 times through a three-roller machine.
The parts by weight of the grease components in examples 1-6 are shown in Table 1.
TABLE 1
Comparative example 1
This comparative example differs from example 1 in that: terephthalic acid was replaced with an equal amount of azelaic acid.
Comparative example 2
Comparative example 2 differs from example 1 in that: terephthalic acid was replaced with an equal amount of sebacic acid.
Test examples
The performance of the grease compositions of examples 1-6, reference (foreign brand composite barium-based grease), comparative example 1 and comparative example 2 were tested, and the test methods and test results are shown in table 2.
TABLE 2
The following conclusions can be drawn from the relevant data of tables 1 and 2:
the difference value between the penetration and the penetration is less than that of like products in the market, so that the product has good shearing stability;
(1) The difference value between the penetration degree and the penetration degree is smaller than that of like products in the market, so that the product has good shearing stability;
(2) The dropping point and steel mesh oil separation test shows that the product has better high temperature resistance and colloid stability;
(3) As can be seen by a corrosivity test and a water spraying test, the product has better corrosion resistance and water resistance;
(4) The extreme pressure performance test shows that the product has good extreme pressure wear resistance.
Although the invention has been described in detail hereinabove by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that many modifications and improvements can be made thereto based on the invention. Accordingly, it is intended that all such modifications and alterations be included within the scope of this invention as defined in the appended claims.
Claims (12)
1. The composite barium-based lubricating grease comprises base oil and a thickening agent, and is characterized in that the thickening agent is prepared from composite acid and barium hydroxide, wherein the composite acid is composed of stearic acid, terephthalic acid and acetic acid in a molar ratio of 1.3-0.5.
2. The grease of claim 1, wherein the base oil is a polyalphaolefin synthetic oil.
3. The grease of claim 2, wherein the polyalphaolefin synthetic oil has a kinematic viscosity at 40 ℃ of 20 to 50mm 2 /s。
4. The grease of any one of claims 1~3 wherein the grease further comprises an antioxidant, the antioxidant comprising an amine antioxidant and a phenolic antioxidant.
5. Grease according to claim 4, characterized in that the aminic antioxidant is diisooctyldiphenylamine.
6. The grease of claim 4, wherein the phenolic antioxidant is 2,6-di-tert-butyl-p-cresol.
7. The grease of claim 4, wherein the antioxidant consists of diisooctyldiphenylamine and 2,6-di-tert-butyl-p-cresol.
8. The grease of claim 7, wherein the weight ratio of diisooctyldiphenylamine to 2,6-di-tert-butyl-p-cresol is 1.
9. The grease of claim 7, wherein the weight ratio of diisooctyldiphenylamine to 2,6-di-tert-butyl-p-cresol is 1:1.
10. the grease of any one of claims 1~3 and 5~9, prepared from the following raw materials in parts by weight:
base oil: 65-85 parts of a base;
a thickening agent: 15-35 parts;
antioxidant: 0.1-2 parts;
the base oil is poly-alpha olefin synthetic oil;
the thickening agent is prepared from composite acid and barium hydroxide, wherein the composite acid is composed of stearic acid, terephthalic acid and acetic acid with the molar ratio of 1;
the antioxidant consists of diisooctyl diphenylamine and 2,6-di-tert-butyl-p-cresol in a weight ratio of 1 to 1.8-1.2.
11. The lubricating grease of claim 4, wherein the lubricating grease is prepared from the following raw materials in parts by weight:
base oil: 65-85 parts;
thickening agent: 15-35 parts;
antioxidant: 0.1-2 parts;
the base oil is poly-alpha olefin synthetic oil;
the thickening agent is prepared from composite acid and barium hydroxide, wherein the composite acid is composed of stearic acid, terephthalic acid and acetic acid with the molar ratio of 1;
the antioxidant consists of diisooctyl diphenylamine and 2,6-di-tert-butyl-p-cresol in a weight ratio of 1.8 to 1.2.
12. Method for preparing a grease according to any of claims 1 to 11, comprising the steps of:
(1) Mixing part of base oil with stearic acid, terephthalic acid and acetic acid, and heating to 85-95 deg.C;
(2) Adding excessive barium hydroxide aqueous solution for saponification for 1.5-2h;
(3) Heating to 180-200 deg.C after saponification, and refining for 10-20min;
(4) After refining, adding the rest base oil, cooling to 80-100 ℃, and adding an antioxidant.
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