CN113637515B - Low-noise composite calcium sulfonate-based lubricating grease composition and preparation method thereof - Google Patents

Low-noise composite calcium sulfonate-based lubricating grease composition and preparation method thereof Download PDF

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CN113637515B
CN113637515B CN202110843542.5A CN202110843542A CN113637515B CN 113637515 B CN113637515 B CN 113637515B CN 202110843542 A CN202110843542 A CN 202110843542A CN 113637515 B CN113637515 B CN 113637515B
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calcium
sulfonate
oil
grease composition
low
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CN113637515A (en
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储友双
周钰
姜增鸿
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China Petroleum and Chemical Corp
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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
    • 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
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/087—Boron oxides, acids or salts
    • 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
    • C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
    • C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
    • C10M2203/1006—Petroleum or coal fractions, e.g. tars, solvents, bitumen 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
    • 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
    • C10M2207/021—Hydroxy compounds having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms
    • 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
    • C10M2207/021—Hydroxy compounds having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/022—Hydroxy compounds having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms containing at least two hydroxy 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
    • C10M2207/123—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms polycarboxylic
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    • 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
    • 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
    • C10M2207/144—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings containing hydroxy groups
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    • 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
    • C10M2207/28—Esters
    • C10M2207/282—Esters of (cyclo)aliphatic oolycarboxylic acids
    • C10M2207/2825—Esters of (cyclo)aliphatic oolycarboxylic acids 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
    • C10M2207/28—Esters
    • C10M2207/283—Esters of polyhydroxy compounds
    • C10M2207/2835—Esters of polyhydroxy compounds 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
    • C10M2207/28—Esters
    • C10M2207/285—Esters of aromatic polycarboxylic acids
    • C10M2207/2855—Esters of aromatic polycarboxylic acids 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
    • C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/04—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
    • C10M2219/046—Overbasedsulfonic acid salts
    • C10M2219/0466—Overbasedsulfonic acid salts used as thickening agents
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/12—Inhibition of corrosion, e.g. anti-rust agents or anti-corrosives
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/02—Bearings
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
    • C10N2050/10—Semi-solids; greasy

Abstract

The invention provides a low-noise composite calcium sulfonate-based lubricating grease composition and a preparation method thereof. The lubricating grease composition is prepared from the following components in percentage by mass: high-base number synthetic calcium alkyl benzene sulfonate 18-35%; 1-5% of transforming agent; 0.1 to 3 percent of calcium hydroxide; 0.1 to 4 percent of composite acid; 30-60% of deeply refined mineral base oil; 5-10% of ester oil; 5-20% of olefin synthetic oil; the calcium alkyl benzene sulfonate in the high-base number synthetic calcium alkyl benzene sulfonate comprises the following components in a weight ratio of 1: (0.05-0.3) long-chain linear calcium alkylbenzene sulfonate and calcium dodecylbenzene sulfonate. The composite calcium sulfonate-based lubricating grease provided by the invention has good silencing performance in small and medium-sized bearings, and simultaneously has excellent extreme pressure wear resistance and antirust performance, and has structural stability of long-period storage.

Description

Low-noise composite calcium sulfonate-based lubricating grease composition and preparation method thereof
Technical Field
The invention relates to the technical field of lubricating grease, in particular to a low-noise composite calcium sulfonate-based lubricating grease composition and a preparation method thereof.
Background
With the rapid development of the manufacturing industry, the bearing industry has also made a great technical progress, the processing precision of the bearing is also gradually improved, the requirements on the noise, the service life and the like of the bearing are higher and higher, and the problems of the noise and the service life of the bearing cannot be completely solved by the optimized design of the bearing. The lubricating grease is used as the fifth major part of the bearing, and the development and preparation of the lubricating grease capable of reducing the running noise characteristic of the rolling bearing have important significance in meeting the requirements of the bearing industry. Silent bearing greases in the industry are still dominated by lithium-based low noise greases and polyurea-based low noise greases.
The grant publication No. CN102021069B provides a lithium-based low-noise bearing lubricating grease which takes naphthenic oil and ester oil as base oil, the lubricating grease has good vibration noise reduction performance, the vibration value can be reduced by 2-5 decibel values, and meanwhile indexes such as high-temperature performance, low-temperature performance and the like of the lubricating grease reach a better index range, and a finished product of the lubricating grease also has a transparent appearance.
Grant publication No. CN100572510 provides a heat-resistant lithium grease composition, which uses polymerized lipid oil to prepare higher fatty acid lithium soap bearing grease, which is used for small-sized motors, especially motor bearings of household appliances such as air conditioners, motor bearings of image equipment such as blowers, and the like.
The grant publication No. CN107338095B provides a low-noise lubricating grease which is prepared by mixing lithium soap lubricating grease and polyurea lubricating grease, adding an auxiliary dispersant and an antioxidant, and then performing a high-temperature mixing process, and has excellent low-noise performance, good mechanical stability and excellent lubricating life, and the maximum service temperature can reach 150 ℃.
In summary, the low noise bearing grease in the industry is mainly focused on lithium-based grease and polyurea-based grease, but as the requirements of the bearing industry on the mute bearing grease are higher and higher, for example, the mute bearing is involved in more and more sizes and the lubricating conditions are more and more demanding, the lithium-based low noise grease and the polyurea-based low noise grease are gradually unable to meet the requirements at the same time.
Compared with other thickeners, the composite calcium sulfonate thickener has various performances of excellent mechanical stability, colloid stability, extreme pressure abrasion resistance, water resistance, rust resistance and the like, is called one of the most potential greases in the twenty-first century, represents the development direction of the grease, and is a typical representative of intensive technology in the grease industry. The product is widely applied to high-temperature, high-humidity and high-load equipment such as rolling mill bearings, continuous casting machine roller bearings and the like in the steel industry. At present, the research on the low-noise performance of the composite calcium sulfonate thickener is less, and the invention is especially provided in order to meet the higher requirements of the bearing industry on lubricating grease.
Disclosure of Invention
The invention aims to provide a low-noise composite calcium sulfonate-based lubricating grease composition and a preparation method thereof. The composite calcium sulfonate-based lubricating grease provided by the invention has good silencing performance in small and medium-sized bearings, and also has excellent extreme pressure abrasion resistance, long-period storage stability and antirust performance.
The invention provides the following technical scheme:
a low-noise composite calcium sulfonate-based lubricating grease composition is prepared from the following components in percentage by mass:
high-base number synthetic calcium alkyl benzene sulfonate 18-35%;
1-5% of transforming agent;
0.1 to 3 percent of calcium hydroxide;
0.1 to 4 percent of composite acid;
30-60% of deeply refined mineral base oil;
5-10% of ester oil;
5-20% of olefin synthetic oil;
the calcium alkyl benzene sulfonate in the high-base number synthetic calcium alkyl benzene sulfonate comprises the following components in a weight ratio of 1: (0.05-0.3) long-chain linear calcium alkylbenzene sulfonate and calcium dodecylbenzene sulfonate.
According to the invention, a large number of experiments show that the silence performance of the obtained lubricating grease product is obviously improved by taking the long-chain linear calcium alkylbenzene sulfonate and the calcium dodecylbenzene sulfonate which are in a specific ratio as raw materials, and the lubricating grease product also has excellent extreme pressure wear resistance, long-period storage stability and antirust performance.
According to some preferred embodiments of the present invention, the total base number of the overbased synthetic calcium alkylbenzene sulfonate is from 360 to 425mgKOH/g.
The high-alkali-value synthetic calcium alkyl benzene sulfonate needs to be diluted by base oil, and the base oil accounts for 40-60% of the total weight.
According to some preferred embodiments of the present invention, the long-chain linear calcium alkylbenzene sulfonate is calcium benzene sulfonate with an alkyl side chain having carbon atoms in the range of 20 to 24.
According to some preferred embodiments of the invention, the conversion agent is a C4-C8 alcohol compound or a C2-C4 acid compound; the C4-C8 alcohol compound is preferably at least one of n-hexanol, n-pentanol, hexanediol, 1,2-hexanediol, octanediol and 2,3-butanediol; the C2-C4 acid compound is preferably at least one of acetic acid and propionic acid;
the composite acid is one or two selected from salicylic acid, sebacic acid, stearic acid and boric acid.
According to some preferred embodiments of the present invention, the deeply refined mineral base oil used in the present invention is a mineral base oil of the type that is shipped at 40 ℃The dynamic viscosity is 200-480mm 2 /s。
According to some preferred embodiments of the present invention, the ester oil used in the present invention is selected from any one of trimellitate, pentaerythritol ester, and dioctyl sebacate.
According to some preferred embodiments of the invention, the olefin synthetic oil used in the invention is polymerized from C8, C10 and C12 olefins, and has a kinematic viscosity at 100 ℃ of 8-20mrn 2 /s。
According to some preferred embodiments of the present invention, the grease composition further comprises 0.2-2.0% by mass of an antioxidant, and the antioxidant is diphenylamine. The invention discovers that the antioxidant with the content is added, so that the antioxidant performance of the lubricating grease product is obviously improved on the basis of ensuring the original performance of the lubricating grease product.
The invention also provides a preparation method of the low-noise composite calcium sulfonate-based lubricating grease composition, which comprises the steps of completing crystal conversion by a conversion agent in the highly refined mineral base oil, compounding, adding olefin synthetic oil for quenching at high temperature, finally adding the antioxidant and the ester oil, and uniformly mixing.
Specifically, the method comprises the following steps:
(1) Adding high-base-number synthetic calcium alkyl benzene sulfonate, deep refined mineral base oil and water accounting for 10-20% of the total weight of the high-base-number synthetic calcium alkyl benzene sulfonate into a normal-pressure reaction kettle according to a specified weight ratio, mixing, wherein the weight of the water is not counted into the total weight, and stirring and heating to 85-95 ℃;
(2) Adding a transforming agent, stirring, controlling the temperature to be 85-95 ℃ and transforming for 1-2 hours, so that the calcium carbonate is completely transformed into a calcite crystal form from an amorphous crystal form;
(3) Controlling the temperature to 85-95 ℃, adding calcium hydroxide, stirring for 30-60 minutes, adding composite acid, diluting the calcium hydroxide with 1-3 times of water in advance, counting the weight of the water, controlling the temperature, and keeping for 30-60 minutes;
(4) Heating to 150-160 deg.C, controlling heating time for 2-4 hr, keeping the temperature at the highest temperature for 10-15min, adding olefin synthetic oil, and quenching to form soap fiber structure;
(5) And (3) when the temperature is reduced to below 150 ℃, adding an antioxidant, finally adding ester oil, adjusting to the cone penetration of a specified mark by three-roll oil rolling, and filling to obtain a finished product.
The composite calcium sulfonate-based lubricating grease composition provided by the invention has the following advantages:
1) The composite calcium sulfonate-based lubricating grease composition greatly reduces the content of high-base-number synthetic calcium alkyl benzene sulfonate in the lubricating grease, and meanwhile, the high-base-number synthetic calcium alkyl benzene sulfonate fiber is finer, and the size of calcium carbonate crystals in the high-base-number synthetic calcium alkyl benzene sulfonate is more uniform, so that the silencing performance is greatly improved.
2) The composite calcium sulfonate-based lubricating grease composition optimizes the base oil formula combination, brings good low-speed oil separation characteristic of the lubricating grease, and greatly reduces the phenomenon of excessive starting noise.
3) The composite calcium sulfonate-based lubricating grease composition effectively improves the stability of colloid after long-term placement, and does not generate the phenomenon of large oil distribution of lubricating grease.
4) The composite calcium sulfonate-based lubricating grease composition has good extreme pressure anti-wear performance, can effectively reduce the running resistance of equipment, reduces the abrasion of mechanical equipment during running, and has excellent performance in a mute test under the condition that a medium-sized bearing is added with a certain load.
5) The composite calcium sulfonate-based lubricating grease composition has excellent antirust performance and can protect lubricating equipment for a long time.
Detailed Description
The present invention is further illustrated by the following examples, which are intended to be illustrative, not limiting and are not intended to limit the scope of the invention. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art, and the raw materials added in the examples are commercially available conventional raw materials unless otherwise specified.
In the following examples and comparative examples, 150BS was used as the deeply refined mineral base oil; PAO8 for olefin synthetic oil separation; ester oil is trimellitate; diphenylamine is used as the antioxidant.
Example 1
The low-noise composite calcium sulfonate-based lubricating grease composition provided by the embodiment is prepared from the following components in percentage by mass:
18 percent of high-base-number synthetic calcium alkyl benzene sulfonate (the base oil accounts for 50 percent of the high-base-number calcium alkyl benzene sulfonate, and the calcium alkyl benzene sulfonate consists of calcium benzene sulfonate and calcium dodecyl benzene sulfonate with the weight ratio of 1;
1% of n-amyl alcohol;
0.1 percent of calcium hydroxide;
0.9 percent of salicylic acid;
60% of deeply refined mineral base oil;
10% of ester oil;
8% of olefin synthetic oil;
2 percent of antioxidant.
The preparation method of the lubricating grease composition comprises the following steps:
(1) Adding high-base-number synthetic calcium alkyl benzene sulfonate with a total base number of 420mgKOH/g, 150BS and water accounting for 10 percent of the total weight of the high-base-number synthetic calcium alkyl benzene sulfonate into a laboratory pilot-scale atmospheric kettle, mixing, stirring and heating to 90 ℃.
(2) Adding n-amyl alcohol into the reaction kettle, stirring, controlling the temperature to be constant temperature of 85 ℃, converting for 1 hour, and after the constant temperature is finished, taking a sample and carrying out an infrared spectrometer test to achieve the infrared detection qualification; namely 862-865cm of characteristic absorption peak of amorphous calcium carbonate in infrared spectrum detection in a sample -1 The peak position disappeared at 881cm -1 And if a strong sharp absorption peak appears at the peak position, the calcium carbonate is completely converted into a calcite crystal form from an amorphous crystal form, and the infrared detection is qualified.
(3) And controlling the temperature to 90 ℃ after the product is qualified, adding calcium hydroxide, stirring for 30 minutes, adding salicylic acid for saponification, diluting the calcium hydroxide by 3 times of water in advance, counting the weight of the water from the total weight, and controlling the temperature and saponifying for 60 minutes.
(4) Heating to 150 ℃, controlling the heating time for 4 hours, keeping the temperature at the highest temperature for 10min, and adding PAO8 for quenching to facilitate the formation of a soap fiber structure.
(5) When the temperature is reduced to 120 ℃, diphenylamine is added, trimellitate is finally added, and the mixture is adjusted to the cone penetration of a specified mark by three-roll mill rolling oil and then filled into a finished product.
Example 2
The low-noise complex calcium sulfonate-based lubricating grease composition provided by the embodiment is prepared from the following components in percentage by mass:
35% of high-base-number synthetic calcium alkylbenzene sulfonate (the base oil accounts for 50% of the high-base-number calcium alkylbenzene sulfonate consists of calcium benzenesulfonate and calcium dodecylbenzenesulfonate, wherein the weight ratio of the calcium benzenesulfonate to the calcium dodecylbenzenesulfonate is 1;
1% of octanediol;
0.2 percent of calcium hydroxide;
1.8 percent of salicylic acid;
41.5% of deeply refined mineral base oil;
5% of ester oil;
15% of olefin synthetic oil;
0.5 percent of antioxidant.
The preparation method of the lubricating oil composition comprises the following steps:
(1) Adding the high-base-number synthetic calcium alkyl benzene sulfonate with the total base number of 420mgKOH/g, 150BS and water accounting for 12 percent of the total weight of the high-base-number synthetic calcium alkyl benzene sulfonate into a laboratory small-test normal-pressure kettle, mixing, stirring and heating to 85 ℃, wherein the weight of the water does not account for the total weight.
(2) Adding octanediol into the reaction kettle, stirring, controlling the temperature at 90 ℃ for constant temperature conversion for 2 hours, and after the constant temperature is finished, taking a sample and carrying out infrared spectrometer test to achieve qualified infrared detection; namely 862-865cm of characteristic absorption peak of amorphous calcium carbonate in infrared spectrum detection in a sample -1 The peak position disappeared at 882cm -1 And if a strong sharp absorption peak appears at the peak position, the calcium carbonate is completely converted into a calcite crystal form from an amorphous crystal form, and the infrared detection is qualified.
(3) And controlling the temperature to 85-95 ℃ after the product is qualified, adding calcium hydroxide, stirring for 30 minutes, adding salicylic acid for saponification, diluting the calcium hydroxide by 3 times of water in advance, counting the weight of the water by the total weight, and controlling the temperature and saponifying for 60 minutes.
(4) Heating to 160 ℃, controlling the heating time for 4 hours, keeping the temperature at the highest temperature for 10min, and adding PAO8 for quenching to facilitate the formation of a soap fiber structure.
(5) When the temperature is reduced to 120 ℃, diphenylamine is added, trimellitate is finally added, and the mixture is adjusted to the cone penetration of a specified mark by three-roll mill rolling oil and then filled into a finished product.
Example 3
The low-noise complex calcium sulfonate-based lubricating grease composition provided by the embodiment is prepared from the following components in percentage by mass:
35% of high-base-number synthetic calcium alkylbenzene sulfonate (the base oil accounts for 50% of the high-base-number calcium alkylbenzene sulfonate consists of calcium benzenesulfonate and calcium dodecylbenzenesulfonate, wherein the weight ratio of the calcium alkylbenzene sulfonate to the calcium dodecylbenzenesulfonate is 1;
1% of octanediol;
0.8 percent of calcium hydroxide;
1.2% of boric acid;
30% of deeply refined mineral base oil;
10% of ester oil;
20% of olefin synthetic oil;
2 percent of antioxidant.
The preparation method of the lubricating oil composition comprises the following steps:
(1) Adding the high-base-number synthetic calcium alkyl benzene sulfonate with the total base number of 420mgKOH/g, 150BS and water accounting for 12 percent of the total weight of the high-base-number synthetic calcium alkyl benzene sulfonate into a laboratory small-test normal-pressure kettle, mixing, stirring and heating to 95 ℃.
(2) Adding octanediol into the reaction kettle, stirring, controlling the temperature at 95 ℃ for constant temperature conversion for 2 hours, and after the constant temperature is finished, taking a sample and carrying out infrared spectrometer test to achieve qualified infrared detection; namely 862-865cm of characteristic absorption peak of amorphous calcium carbonate in infrared spectrum detection in a sample -1 The peak position disappeared at 882cm -1 The carbon is indicated by the strong sharp absorption peak at the peak positionAnd (4) completely converting the calcium carbonate from an amorphous crystal form into a calcite crystal form, and then, passing the infrared detection.
(3) And controlling the temperature to 85 ℃ after the product is qualified by an infrared spectrogram, adding calcium hydroxide, stirring for 60 minutes, adding boric acid for saponification, diluting the calcium hydroxide by 1-3 times of water in advance, counting the weight of the water, and controlling the temperature and saponifying for 30-60 minutes.
(4) And (3) heating to 155 ℃, controlling the heating time for 3 hours, keeping the temperature at the highest temperature for 15 minutes, and adding PAO8 for quenching to facilitate the formation of a soap fiber structure.
(5) When the temperature is reduced to 120 ℃, diphenylamine is added, trimellitate is finally added, and the mixture is adjusted to the cone penetration of a specified mark by three-roll mill rolling oil and then filled into a finished product.
Example 4
The low-noise complex calcium sulfonate-based lubricating grease composition provided by the embodiment is prepared from the following components in percentage by mass:
20% of high-base-number synthetic calcium alkylbenzene sulfonate (the base oil accounts for 50% of the high-base-number calcium alkylbenzene sulfonate, and the calcium alkylbenzene sulfonate consists of calcium benzene sulfonate and calcium dodecyl benzene sulfonate, wherein the carbon atoms of alkyl side chains of the calcium alkylbenzene sulfonate account for 20-24% in a weight ratio of 1;
5% of octanediol;
0.1 percent of calcium hydroxide;
2.9 percent of boric acid;
55% of deeply refined mineral base oil;
10% of ester oil;
5% of olefin synthetic oil;
2 percent of antioxidant.
The preparation method of the lubricating oil composition comprises the following steps:
(1) Adding the high-base-number synthetic calcium alkyl benzene sulfonate with the total base number of 400mgKOH/g, 150BS and water accounting for 20 percent of the total weight of the high-base-number synthetic calcium alkyl benzene sulfonate into a laboratory pilot-scale atmospheric kettle, mixing, stirring and heating to 90 ℃.
(2) Adding octanediol into the reaction kettle, stirring, controlling the temperature at 85 deg.C, converting for 2 hr, and taking out sample after constant temperatureTesting by a spectrometer to ensure that the infrared detection is qualified; namely 862-865cm of characteristic absorption peak of amorphous calcium carbonate in infrared spectrum detection in a sample -1 The peak position disappeared at 883cm -1 And if a strong sharp absorption peak appears at the peak position, the calcium carbonate is completely converted into a calcite crystal form from an amorphous crystal form, and the infrared detection is qualified.
(3) And controlling the temperature to 95 ℃ after the product is qualified by an infrared spectrogram, adding calcium hydroxide, stirring for 60 minutes, adding boric acid for saponification, diluting the calcium hydroxide by 3 times of water in advance, counting the weight of the water from the total weight, and controlling the temperature and saponifying for 30 minutes.
(4) And (3) heating to 152 ℃, controlling the heating time for 4 hours, keeping the temperature at the highest temperature for 15min, and adding PAO8 for quenching to facilitate the formation of a soap fiber structure.
(5) When the temperature is reduced to 120 ℃, diphenylamine is added, trimellitate is finally added, and the mixture is rolled by a three-roll mill to adjust the cone penetration of a specified mark and then a finished product is filled.
Example 5
The low-noise complex calcium sulfonate-based lubricating grease composition provided by the embodiment is prepared from the following components in percentage by mass:
24% of high-base-number synthetic calcium alkylbenzene sulfonate (the base oil accounts for 50% of the high-base-number calcium alkylbenzene sulfonate, and the calcium alkylbenzene sulfonate consists of calcium benzenesulfonate and calcium dodecylbenzenesulfonate, wherein the carbon atoms of alkyl side chains are 20-24, and the weight ratio of the calcium benzenesulfonate to the calcium dodecylbenzenesulfonate is 1;
2% of octanediol;
3 percent of calcium hydroxide;
4% of boric acid;
48% of deeply refined mineral base oil;
8% of ester oil;
10% of olefin synthetic oil;
1% of antioxidant.
The preparation method of the lubricating oil composition comprises the following steps:
(1) Adding high-base-number synthetic calcium alkyl benzene sulfonate with a total base number of 400mgKOH/g, 150BS and water accounting for 15 percent of the total weight of the high-base-number synthetic calcium alkyl benzene sulfonate into a laboratory pilot-scale atmospheric kettle, mixing, stirring and heating to 90 ℃.
(2) Adding octanediol into the reaction kettle, stirring, controlling the temperature at 90 ℃ for constant temperature conversion for 1 hour, and after the constant temperature is finished, taking a sample and carrying out infrared spectrometer test to achieve qualified infrared detection; namely 862-865cm of characteristic absorption peak of amorphous calcium carbonate in infrared spectrum detection in a sample -1 The peak position disappeared at 8801m -1 And if a strong sharp absorption peak appears at the peak position, the calcium carbonate is completely converted into a calcite crystal form from an amorphous crystal form, and the infrared detection is qualified.
(3) And (3) controlling the temperature to 85-95 ℃ after the product is qualified by an infrared spectrogram, adding calcium hydroxide, stirring for 30 minutes, adding boric acid for saponification, diluting the calcium hydroxide by 1 time of water in advance, not counting the weight of the water into the total weight, and controlling the temperature and saponifying for 60 minutes.
(4) And (3) heating to 152 ℃, controlling the heating time for 4 hours, keeping the temperature at the highest temperature for 15min, and adding PAO8 for quenching to facilitate the formation of a soap fiber structure.
(5) When the temperature is reduced to 120 ℃, diphenylamine is added, trimellitate is finally added, and the mixture is rolled by a three-roll mill to adjust the cone penetration of a specified mark and then a finished product is filled.
Example 6
The low-noise complex calcium sulfonate-based lubricating grease composition provided by the embodiment is prepared from the following components in percentage by mass:
28% of high-base-number synthetic calcium alkylbenzene sulfonate (the high-base-number calcium alkylbenzene sulfonate comprises 50% of base oil and calcium benzene sulfonate and calcium dodecyl benzene sulfonate which have the carbon atom number of an alkyl side chain of 20-24 and the weight ratio of 1;
1.5% of octanediol;
0.1 percent of calcium hydroxide
0.1% of boric acid;
42.3 percent of deeply refined mineral base oil;
7% of ester oil;
20% of olefin synthetic oil;
1 percent of antioxidant.
The preparation method of the lubricating oil composition comprises the following steps:
(1) Adding high-base-number synthetic calcium alkyl benzene sulfonate with a total base number of 400mgKOH/g, 150BS and water accounting for 15 percent of the total weight of the high-base-number synthetic calcium alkyl benzene sulfonate into a laboratory pilot-scale atmospheric kettle, mixing, stirring and heating to 85-95 ℃.
(2) Adding octanediol into the reaction kettle, stirring, controlling the temperature to be 85-95 ℃ for constant-temperature conversion for 2 hours, and after the constant temperature is finished, taking a sample and carrying out infrared spectrometer test to achieve qualified infrared detection; namely 862-865cm of characteristic absorption peak of amorphous calcium carbonate in infrared spectrum detection in a sample -1 The peak position disappeared at 884cm -1 And if a strong sharp absorption peak appears at the peak position, the calcium carbonate is completely converted into a calcite crystal form from an amorphous crystal form, and the infrared detection is qualified.
(3) And controlling the temperature to 85 ℃ after the product is qualified by an infrared spectrogram, adding calcium hydroxide, stirring for 30 minutes, adding boric acid for saponification, diluting the calcium hydroxide by 3 times of water in advance, counting the weight of the water from the total weight, and controlling the temperature and saponifying for 60 minutes.
(4) And (3) heating to 152 ℃, controlling the heating time for 4 hours, keeping the temperature at the highest temperature for 10-15min, and adding PAO8 for quenching to facilitate the formation of a soap fiber structure.
(5) When the temperature is reduced to 120 ℃, diphenylamine is added, trimellitate is finally added, and the mixture is adjusted to the cone penetration of a specified mark by three-roll mill rolling oil and then filled into a finished product.
Comparative example 1
The grease composition of this comparative example differs from example 1 in that the calcium dodecylbenzenesulfonate is replaced with an equal amount of high boiling alkylbenzene sulfonic acid.
Comparative example 2
The grease composition of this comparative example differs from that of example 1 in that the calcium dodecylbenzenesulfonate is replaced with an equal amount of calcium long-chain linear alkylbenzene sulfonate.
Comparative example 3
Is a commercial lithium-based low-noise bearing grease.
Comparative example 4
Is a commercial low noise polyurea grease.
The performance data for examples 1-6 and comparative examples 1-4 are shown in tables 1 and 2.
TABLE 1
Figure BDA0003179947740000121
Figure BDA0003179947740000131
TABLE 2
Figure BDA0003179947740000132
Figure BDA0003179947740000141
Remarking: the samples for testing 1,3,6,12 months in the examples and the comparative examples are stored in a sample library according to the GB/T269 storage requirement and tested according to the GB/T requirement.
From the above data the following conclusions can be drawn:
1) The composite calcium sulfonate-based lubricating grease prepared by the method reduces the content of high-base-number synthetic calcium alkylbenzene sulfonate in the lubricating grease, meanwhile, the high-base-number synthetic calcium alkylbenzene sulfonate fibers are finer, and the size of calcium carbonate in the high-base-number synthetic calcium alkylbenzene sulfonate is more uniform.
2) The test data of the composite calcium sulfonate-based lubricating grease prepared by the method in the BVT-8 bearing axial load-loaded vibration test is good, which shows that the product has excellent silencing performance in loaded 2216 bearing.
3) After the composite calcium sulfonate-based lubricating grease prepared by the method is stored for one year, the oil separation amount of a sample steel mesh is stable, the phenomenon of large amount of oil separation of the lubricating grease is not generated, and the composite calcium sulfonate-based lubricating grease is superior to the comparative lithium-based and polyurea-based low-noise lubricating grease, so that the product disclosed by the invention has good colloid stability after long-term storage.
4) The composite calcium sulfonate-based lubricating grease prepared by the method has good extreme pressure anti-wear performance, can effectively reduce the running resistance of equipment, reduces the abrasion of mechanical equipment during running, and has excellent performance in a mute test under the condition that a medium-sized bearing is added with a certain load.
5) The composite calcium sulfonate grease prepared by the method of the invention passes the corrosion resistance test under the condition of 5% saline water, and is superior to comparative examples 3 and 4, which shows that the composite calcium sulfonate grease has excellent antirust performance and can play a long-acting protection role on lubricating equipment.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (11)

1. The low-noise composite calcium sulfonate-based lubricating grease composition is characterized by being prepared from the following components in percentage by mass:
high-base number synthetic calcium alkyl benzene sulfonate 18-35%;
1-5% of transforming agent;
0.1 to 3 percent of calcium hydroxide;
0.1 to 4 percent of composite acid;
30-60% of deeply refined mineral base oil;
5-10% of ester oil;
5-20% of olefin synthetic oil;
the calcium alkyl benzene sulfonate in the high-base number synthetic calcium alkyl benzene sulfonate comprises the following components in a weight ratio of 1: (0.05-0.3) long-chain linear calcium alkylbenzene sulfonate and calcium dodecylbenzene sulfonate;
the long-chain linear calcium alkylbenzene sulfonate is calcium benzene sulfonate with alkyl side chain carbon atom number of 20-24.
2. The low-noise complex calcium sulfonate-based grease composition according to claim 1, wherein the total base number of the high-base number synthetic calcium alkylbenzene sulfonate is 360 to 425 mgKOH/g; the high-alkalinity synthetic calcium alkyl benzene sulfonate needs to be diluted by base oil, and the base oil accounts for 40-60% of the total weight.
3. The low-noise complex calcium sulfonate-based grease composition according to claim 1 or 2, wherein the converting agent is a C4-C8 alcohol compound or a C2-C4 acid compound;
the composite acid is one or two selected from salicylic acid, sebacic acid, stearic acid and boric acid.
4. The low noise complex calcium sulfonate grease composition according to claim 3, wherein the C4-C8 alcohol compound is at least one of n-hexanol, n-pentanol, hexanediol, 1,2-hexanediol, octanediol, 2,3-butanediol.
5. The low-noise complex calcium sulfonate grease composition according to claim 3, wherein the C2-C4 acid-based compound is at least one selected from acetic acid and propionic acid.
6. The low-noise complex calcium sulfonate-based grease composition according to claim 1 or 2, wherein the deeply refined mineral base oil is a type of mineral base oil having a kinematic viscosity at 40 ℃ of 200 to 480mm 2 /s。
7. The low noise complex calcium sulfonate-based grease composition according to claim 1, wherein the ester oil is selected from any one of trimellitate, pentaerythritol ester, and dioctyl sebacate.
8. The low-noise complex calcium sulfonate grease composition according to claim 1 or 2, wherein the olefin synthetic oil is formed by polymerizing C8, C10 and C12 olefins and has a kinematic viscosity of 8-20mm at 100 ℃ 2 /s。
9. The low noise calcium complex sulfonate grease composition according to claim 1 or 2, wherein the grease composition further comprises 0.2-2.0% by mass of an antioxidant, and the antioxidant is diphenylamine.
10. The method for preparing the low-noise complex calcium sulfonate-based grease composition according to claim 1 or 2, wherein the high-base number synthetic calcium alkyl benzene sulfonate is subjected to crystal transformation by a transforming agent in the deep refined mineral base oil and is compounded, then, under the condition of 150-160 ℃, the olefin synthetic oil is added for quenching, and finally, the antioxidant and the ester oil are added and mixed uniformly.
11. The method for preparing a low-noise complex calcium sulfonate-based grease composition according to claim 10, comprising the steps of:
(1) Adding high-base-number synthetic calcium alkyl benzene sulfonate, deep refined mineral base oil and water accounting for 10-20% of the total weight of the high-base-number synthetic calcium alkyl benzene sulfonate into a normal-pressure reaction kettle according to a specified weight ratio, mixing, stirring and heating to 85-95 ℃;
(2) Adding a transforming agent, stirring, controlling the temperature to be 85-95 ℃ and transforming for 1-2 hours, so that the calcium carbonate is completely transformed into a calcite crystal form from an amorphous crystal form;
(3) Controlling the temperature to 85-95 ℃, adding calcium hydroxide, stirring for 30-60 minutes, adding composite acid for saponification, diluting the calcium hydroxide by 1-3 times of water in advance, counting the weight of the water, controlling the temperature, and keeping for 30-60 minutes;
(4) Heating to 150-160 deg.C, controlling heating time for 2-4 hr, keeping the temperature at the highest temperature for 10-15min, adding olefin synthetic oil, and quenching to form soap fiber structure;
(5) And (3) when the temperature is reduced to below 150 ℃, adding an antioxidant, finally adding ester oil, adjusting to the cone penetration of a specified mark by three-roll oil rolling, and filling to obtain a finished product.
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