CN113999709A - Application of hydrotalcite or modified hydrotalcite as anti-ultraviolet antioxidant in lubricating oil/grease - Google Patents

Application of hydrotalcite or modified hydrotalcite as anti-ultraviolet antioxidant in lubricating oil/grease Download PDF

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Publication number
CN113999709A
CN113999709A CN202111419445.XA CN202111419445A CN113999709A CN 113999709 A CN113999709 A CN 113999709A CN 202111419445 A CN202111419445 A CN 202111419445A CN 113999709 A CN113999709 A CN 113999709A
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hydrotalcite
lubricating oil
grease
antioxidant
modified
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韩景宾
刘自茹
李勇
靳祖超
段雪
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Beijing University of Chemical Technology
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Beijing University of Chemical Technology
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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
    • C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
    • C10M125/10—Metal oxides, hydroxides, carbonates or bicarbonates
    • 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
    • C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
    • C10M125/18—Compounds containing halogen
    • 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
    • C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
    • C10M125/20—Compounds containing nitrogen
    • 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
    • C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
    • C10M125/24—Compounds containing phosphorus, arsenic or antimony
    • 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
    • C10M2201/06—Metal compounds
    • C10M2201/062—Oxides; Hydroxides; Carbonates or bicarbonates
    • 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
    • C10M2201/08—Inorganic acids or salts thereof
    • C10M2201/081—Inorganic acids or salts thereof containing halogen
    • 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
    • C10M2201/08—Inorganic acids or salts thereof
    • C10M2201/082—Inorganic acids or salts thereof containing nitrogen
    • 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
    • C10M2201/085—Phosphorus oxides, acids or salts
    • 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
    • C10N2030/10—Inhibition of oxidation, e.g. anti-oxidants
    • 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

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Lubricants (AREA)

Abstract

The invention provides an application of hydrotalcite or modified hydrotalcite as an anti-ultraviolet antioxidant in lubricating oil/grease, belonging to the technical field of lubricating grease, comprising the following steps: mixing hydrotalcite or modified hydrotalcite with lubricating oil/grease. The invention takes hydrotalcite or modified hydrotalcite as the uvioresistant antioxidant of the lubricating oil/grease, the hydrotalcite has a main laminated plate structure, the surface of the laminated plate contains a large number of hydroxyl groups, the hydrotalcite quenches a large number of free radicals generated in the photo-thermal oxidation process of the lubricating oil/grease by removing H from the hydroxyl groups of the laminated plate, and can shield ultraviolet rays by the actions of chemical absorption, physical reflection or scattering and the like, and the hydrotalcite as an additive is added into the lubricating oil/grease to effectively slow down the oxidation of the lubricating oil/grease. The results of the examples show that after hydrotalcite or modified hydrotalcite is added into lubricating oil, the sample is irradiated by ultraviolet rays for 60 hours, the light transmittance of the sample is 30%, the oxidation induction time of the lubricating oil is 1173min, and the bearing life is 188 hours.

Description

Application of hydrotalcite or modified hydrotalcite as anti-ultraviolet antioxidant in lubricating oil/grease
Technical Field
The invention relates to the technical field of lubricating grease, in particular to application of hydrotalcite or modified hydrotalcite as an anti-ultraviolet antioxidant in lubricating oil/grease.
Background
With the rapid development of society, industry and economy, the mechanization level is continuously improved, and the lubricating oil/grease is more and more valued. Lubricating oil/grease is a liquid lubricant widely applied to mechanical equipment, and the lubricating grease can reduce friction and abrasion on a metal surface, can continuously absorb heat from the friction surface, reduces the temperature of the friction surface, and plays a role in cooling, so that the normal operation of the mechanical equipment is maintained, the faults and damages of the machine are reduced, and the service life of the mechanical equipment is prolonged.
The lubricating oil/grease is discolored under the irradiation of sunlight and ultraviolet rays, so that the thermal oxidation of the lubricating oil/grease is intensified, and the performance of the lubricating oil/grease is further reduced. At present, in order to slow down the oxidation speed of lubricating oil/grease, an antioxidant such as diphenylamine or phenol antioxidant T501 is generally added into the lubricating oil/grease, but the existing antioxidant has outstanding defects and does not have ultraviolet resistance, and the lubricating oil/grease added with the existing antioxidant has large color change after being irradiated by sunlight and ultraviolet light, so that the performance is greatly reduced.
Therefore, how to improve the oxidation resistance and ultraviolet resistance of the lubricating oil/grease becomes a difficult problem in the prior art.
Disclosure of Invention
The invention aims to provide application of hydrotalcite or modified hydrotalcite as an anti-ultraviolet antioxidant in lubricating oil/grease. The invention adopts the hydrotalcite or the modified hydrotalcite as the uvioresistant antioxidant, and can improve the oxidation resistance and the uvioresistant performance of the lubricating oil/grease.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides an application of hydrotalcite or modified hydrotalcite as an anti-ultraviolet antioxidant in lubricating oil/grease, which comprises the following steps: mixing hydrotalcite or modified hydrotalcite with lubricating oil/grease.
Preferably, the mass ratio of the hydrotalcite or the modified hydrotalcite to the lubricating oil/grease is (0.2-5): 100.
preferably, the mass ratio of the hydrotalcite or the modified hydrotalcite to the lubricating oil/grease is (1-5): 100.
preferably, the mass ratio of the hydrotalcite or the modified hydrotalcite to the lubricating oil/grease is (2-5): 100.
preferably, the structural formula of the hydrotalcite is shown as formula I: [ M ] A1 2-+xN3 x+(OH)2]x+(An-)x/n·mH2O is shown as formula I.
Preferably, M in formula I comprises one of Mg, Ca and Zn.
Preferably, N in formula I comprises Al.
Preferably, the molar ratio of M to N in the formula I is (2-4): 1.
preferably, A in the formula In-Including NO3-, CO3 2-、Cl-And PO4 3-One kind of (1).
Preferably, x in formula I is 1: (5-3).
The invention provides an application of hydrotalcite or modified hydrotalcite as an anti-ultraviolet antioxidant in lubricating oil/grease, which comprises the following steps: mixing hydrotalcite or modified hydrotalcite with lubricating oil/grease. The invention takes hydrotalcite or modified hydrotalcite as the anti-ultraviolet antioxidant of lubricating oil/grease, the hydrotalcite has a main laminated plate structure, the surface of the laminated plate contains a large amount of hydroxyl, and the hydrotalcite quenches a large amount of free radicals (such as R & free radical, RO & free radical and ROO & free radical) generated in the photo-thermal oxidation process of the lubricating oil/grease by removing H from the hydroxyl of the laminated plate, and simultaneously can shield ultraviolet rays through the actions of chemical absorption, physical reflection or scattering and the like. The hydrotalcite is used as an additive and added into the lubricating oil/grease, so that ultraviolet rays can be effectively shielded, the oxidative aging of the lubricating oil/grease can be slowed down, and the antioxidant stability can be improved; the hydrotalcite can be used as an antioxidant, more importantly, as an ultraviolet absorbent, and has the function of 'one dose of functionalization'. The results of the examples show that after hydrotalcite or modified hydrotalcite is added into lubricating oil, the sample is irradiated by ultraviolet rays for 60 hours, the light transmittance of the sample is 30%, the oxidation induction time of the lubricating oil is 1173min, and the bearing life is 188 hours.
Drawings
FIG. 1 is an XRD pattern of hydrotalcite prepared according to example 1 of the present invention;
FIG. 2 is an SEM photograph of hydrotalcite prepared in example 1 of the present invention;
FIG. 3 is an XRD pattern of hydrotalcite prepared according to example 2 of the present invention;
FIG. 4 is an SEM image of hydrotalcite prepared in example 2 of the present invention;
FIG. 5 is a color chart of lubricants of examples 1 and 3 and comparative examples 1 to 5 of the present invention after being subjected to ultraviolet irradiation for 60 hours;
FIG. 6 is a color chart of greases of example 4 and comparative examples 6 to 8 of the present invention after ultraviolet irradiation for 60 hours.
Detailed Description
The invention provides an application of hydrotalcite or modified hydrotalcite as an anti-ultraviolet antioxidant in lubricating oil/grease, which comprises the following steps: mixing hydrotalcite or modified hydrotalcite with lubricating oil/grease.
The source of the lubricating oil/grease is not particularly limited in the present invention, and commercially available products known to those skilled in the art may be used.
In the present invention, the mass ratio of the hydrotalcite or modified hydrotalcite to the lubricating oil/grease is preferably (0.2 to 5): 100, more preferably (1-5): 100, more preferably (2-5): 100, most preferably (3-5): 100. in the present invention, the hydrotalcite has a bulk laminate structure, the laminate surface contains a large number of hydroxyl groups, and the hydrotalcite quenches a large number of radicals (such as R, RO, and ROO radicals) generated during photo-thermal oxidation of the lubricating oil/grease by dehydriding the laminate hydroxyl groups, while it can shield ultraviolet rays by the action of chemical absorption, physical reflection, scattering, or the like. The hydrotalcite is used as an additive and added into the lubricating oil/grease, so that ultraviolet rays can be effectively shielded, the oxidative aging of the lubricating oil/grease can be slowed down, and the antioxidant stability can be improved; the hydrotalcite can be used as an antioxidant, more importantly, as an ultraviolet absorbent, and has the function of 'one dose of functionalization'; the hydrotalcite is modified, so that the antioxidant and ultraviolet resistant effects of the hydrotalcite are further improved. The invention limits the mass ratio of the hydrotalcite or the modified hydrotalcite to the lubricating oil/grease within the range, and can further improve the oxidation resistance and the ultraviolet resistance of the lubricating oil/grease.
The operation of mixing the hydrotalcite or the modified hydrotalcite with the lubricating oil/grease is not particularly limited, and the technical scheme of mixing materials, which is well known to those skilled in the art, can be adopted.
In the present invention, the general structural formula of the hydrotalcite is preferably as shown in formula I:
[M1 2-x+N3 x +(OH)2]x+(An-)x/n·mH2o is shown as formula I.
In the present invention, M in formula I preferably includes one of Mg, Ca and Zn, more preferably Mg; n in the formula I preferably comprises Al; the molar ratio of M to N in the formula I is preferably (2-4): 1; in the formula I, An-Preferably comprising NO3-, CO3 2-、Cl-And PO4 3-More preferably CO3 2-(ii) a In the formula I, x is preferably 1: (5-3). The invention limits the general structural formula of the hydrotalcite in the range, can adjust the structure and interlayer spacing of the hydrotalcite, enhances the capability of shielding ultraviolet rays through chemical absorption, physical reflection or scattering, and further improves the oxidation resistance and ultraviolet resistance of the lubricating oil/grease.
In the present invention, the method for preparing the hydrotalcite is preferably: hydrothermal crystallization or nucleation/crystallization isolation.
In the present invention, the hydrothermal crystallization method preferably includes: mixing the M source, the N source, urea and water, and carrying out hydrothermal crystallization to obtain the hydrotalcite.
In the present invention, the M source preferably comprises a nitrate, chloride, sulfate or carbonate salt of M, more preferably a nitrate salt.
In the present invention, the N source preferably comprises a nitrate or chloride salt of N.
In the present invention, the ratio of the amounts of the M source and the N source is preferably (2 to 4): 1, more preferably (2 to 3.5): 1, most preferably (2-3): 1. The invention limits the quantity ratio of M source and N source in the above range, can adjust the structure, composition and particle size of hydrotalcite, avoid producing impurity phase, and further improve the uvioresistant and antioxidant performance of lubricating oil/grease.
In the present invention, the ratio of the amount of the urea substance to the total amount of the M source and the N source is preferably (2 to 8): 1, more preferably (3-7): 1, most preferably (4-6): 1. in the present invention, the urea is used to provide hydroxide ions, carbonate ions. In the present invention, the ratio of the amount of urea to the total amount of the M source and the N source is limited to the above range, and M and N can be more sufficiently reacted with urea to obtain a hydrotalcite material.
In the invention, the total concentration of the N source and the M source is preferably (0.01-0.8) mol/L, more preferably (0.3-0.6) mol/L, and most preferably (0.4-0.5) mol/L. The total concentration of the N source and the M source is limited in the range, so that the components can be dissolved more fully.
The operation of mixing the M source, the N source, the urea and the water is not particularly limited in the invention, and the technical scheme of mixing materials, which is well known to those skilled in the art, can be adopted.
In the invention, the temperature of the hydrothermal crystallization is preferably 90-140 ℃, more preferably 100-130 ℃, and most preferably 110-120 ℃; the time for the hydrothermal crystallization is preferably 12-48 h, and more preferably 24-36 h. The invention limits the temperature and time of hydrothermal crystallization in the above range, can fully carry out hydrothermal crystallization reaction, improves the crystallinity of hydrotalcite, adjusts the particle size of the product, and further improves the uvioresistant and antioxidant properties of the lubricating oil/grease.
After the hydrothermal crystallization is finished, the product of the hydrothermal crystallization is preferably sequentially cooled, centrifuged, washed and dried to obtain the hydrotalcite.
In the present invention, the cooling is preferably natural cooling; the end point of the cooling is preferably room temperature.
In the invention, the rotation speed of the centrifugation is preferably 3000-6000 rpm, more preferably 4000-5000 rpm; the time for centrifugation is preferably 3-5 min, and more preferably 4 min.
In the present invention, the washing preferably includes water washing and ethanol washing which are performed in this order; the number of times of the water washing and the ethanol washing is preferably 3-5 times, and more preferably 4 times.
In the invention, the drying temperature is preferably 40-70 ℃, and more preferably 50-60 ℃; the drying time is preferably 10-24 hours, and more preferably 12-18 hours.
In the present invention, the nucleation/crystallization isolation method preferably includes:
(1) mixing an N source, an M source and water to obtain a mixed solution 1;
(2) a is to ben-Mixing a source and an alkali to obtain a mixed solution 2;
(3) mixing the mixed solution 1 obtained in the step (1) with the mixed solution 2 obtained in the step (2) and carrying out colloid milling to obtain a gel solution;
(4) carrying out hydrothermal crystallization on the gel solution obtained in the step (3) to obtain hydrotalcite;
the steps (1) and (2) are not in sequence.
The invention mixes N source, M source and water to obtain mixed solution 1.
In the present invention, the M source preferably comprises a nitrate, chloride, sulfate or carbonate salt of M, more preferably a nitrate salt.
In the present invention, the N source preferably comprises a nitrate or chloride salt of N.
In the present invention, the ratio of the amounts of the M source and the N source is preferably (2 to 4): 1, more preferably (2 to 3.5): 1, most preferably (2-3): 1. The invention limits the quantity ratio of M source and N source in the above range, can obtain complete hydrotalcite structure, avoid the generation of impurity phase, and further improve the uvioresistant and antioxidant performance of the lubricating oil/grease.
In the present invention, the concentration of the N source in the mixed solution 1 is preferably (0.01-1) mol/L, more preferably (0.02-0.08) mol/L, and most preferably (0.03-0.05) mol/L. In the present invention, the concentration of the N source in the mixed solution 1 is limited to the above range, and the respective components can be dissolved more sufficiently.
The operation of mixing the N source, the M source and the water is not particularly limited in the invention, and the technical scheme of material mixing which is well known to the skilled person can be adopted.
The invention will An-The source and base are mixed to give a mixed solution 2.
In the present invention, said An-The source preferably comprises An-Potassium salt or sodium salt of (a).
In the present invention, the base is preferably sodium hydroxide, potassium hydroxide or calcium hydroxide. In the present invention, the base is used to provide hydroxide ions.
In the present invention, the ratio of the amount of the substance of the base to the total amount of the M source and the N source is preferably (1.5 to 2.5): 1, more preferably (1.5 to 2): 1. in the present invention, the ratio of the amount of the base to the total amount of the M source and the N source is limited to the above range, and M and N can be reacted with the base more sufficiently.
The invention is directed to said An-The operation of mixing the source and the base is not particularly limited, and a technical scheme of mixing materials well known to those skilled in the art may be adopted.
After the mixed solution 1 and the mixed solution 2 are obtained, the mixed solution 1 and the mixed solution 2 are mixed and subjected to colloid milling to obtain a gel solution.
In the present invention, A in the mixed solution 2n-The ratio of the amount of the N source in the mixed solution 1 to the source is preferably (2 to 4): 1, more preferably (2-3): 1. the invention mixes A in the solution 2n-The ratio of the amount of the substance of the source to the N source in the mixed solution 1 is defined within the above range,can adjust the content of interlayer anions to obtain hydrotalcite with complete structure.
In the invention, the speed of the colloid mill is preferably 3500-4500 rpm, more preferably 4000 rpm; the time of the colloid mill is preferably 3-6 min, and more preferably 4-5 min. The present invention limits the rate and time of the colloid mill to the above ranges, enabling more thorough mixing of the components.
After obtaining the gel solution, the invention carries out hydrothermal crystallization on the gel solution to obtain the hydrotalcite.
In the invention, the temperature of the hydrothermal crystallization is preferably 90-140 ℃, more preferably 100-130 ℃, and most preferably 110-120 ℃; the time for the hydrothermal crystallization is preferably 12-48 h, and more preferably 24-36 h. The invention limits the temperature and time of hydrothermal crystallization in the above range, can fully perform the hydrothermal crystallization reaction, improve the crystallinity of the hydrotalcite, adjust the particle size of the hydrotalcite, and further improve the uvioresistant and antioxidant properties of the lubricating oil/grease.
After the hydrothermal crystallization is finished, the product of the hydrothermal crystallization is preferably sequentially cooled, centrifuged, washed and dried to obtain the hydrotalcite.
In the present invention, the cooling is preferably natural cooling; the end point of the cooling is preferably room temperature.
In the invention, the rotation speed of the centrifugation is preferably 3000-6000 rpm, more preferably 4000-5000 rpm; the time for centrifugation is preferably 3-5 min, and more preferably 4 min.
In the present invention, the washing preferably includes water washing and ethanol washing which are performed in this order; the number of times of the water washing and the ethanol washing is preferably 3-5 times, and more preferably 4 times.
In the invention, the drying temperature is preferably 40-70 ℃, and more preferably 50-60 ℃; the drying time is preferably 10-24 hours, and more preferably 12-18 hours.
The invention controls the process parameters such as the dosage of each component, the reaction temperature, the reaction time and the like in the preparation process of the hydrotalcite, improves the crystallinity and the structural integrity of the hydrotalcite, and further improves the performance of the hydrotalcite material.
After obtaining the hydrotalcite, the invention preferably modifies the hydrotalcite to obtain the modified hydrotalcite.
The modification method of the present invention is not particularly limited, and the hydrotalcite may be modified by a modification method known to those skilled in the art.
The hydrotalcite is modified, so that the ultraviolet resistance and oxidation resistance of the hydrotalcite can be further improved.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The application of hydrotalcite as an uvioresistant antioxidant in lubricating oil (alkyl naphthalene base oil) is prepared by adding hydrotalcite into the lubricating oil and performing ultrasonic treatment to uniformly disperse the hydrotalcite;
the mass ratio of the hydrotalcite to the lubricating oil is 0.5: 100;
the structural formula of the hydrotalcite is [ Mg ]2+ 2/3Al3+ 1/3(OH)2]1/3+(CO3 2-)1/6；
The preparation method of the hydrotalcite comprises the following steps: mixing Mg (NO)3)2·6H2O、Al(NO3)3·9H2Mixing O, urea and deionized water (the concentration of magnesium nitrate is 0.02mol/L, the concentration of aluminum nitrate is 0.01mol/L, and the concentration of urea is 0.18mol/L) (the ratio of the amount of magnesium to aluminum is 2:1, the total concentration of magnesium and aluminum is 0.03mol/L, and the ratio of the amount of urea to the total amount of magnesium and aluminum is 6:1), transferring the obtained mixed metal ion solution into a polytetrafluoroethylene high-pressure reaction kettle, carrying out hydrothermal crystallization reaction at 110 ℃ for 24h, cooling to room temperature, centrifuging at 4000rpm for 5min, washing the obtained solid component with water for 3 times, washing with ethanol for 3 times, and then washing with 60 rpm for 3 timesDrying at the temperature of 12 hours to obtain the LDHs hydrotalcite.
Example 2
The application of hydrotalcite as an uvioresistant antioxidant in lubricating oil (alkyl naphthalene base oil) is prepared by adding hydrotalcite into the lubricating oil and performing ultrasonic treatment to uniformly disperse the hydrotalcite;
the mass ratio of the hydrotalcite to the lubricating oil is 0.5: 100;
the structural formula of the hydrotalcite is [ Mg ]2+ 2/3Al3+ 1/3(OH)2]1/3+(CO3 2-)1/6；
The preparation method of the hydrotalcite comprises the following steps: mixing Mg (NO)3)2·6H2O、Al(NO3)3·9H2Mixing O and deionized water (the concentration of magnesium nitrate is 0.02mol/L, the concentration of aluminum nitrate is 0.01mol/L) (the mass ratio of magnesium to aluminum is 2:1, and the total concentration of magnesium and aluminum is 0.03mol/L) to obtain a mixed solution 1; mixing NaOH and Na2CO3Mixing with deionized water (concentration of NaOH is 0.048mol/L, Na)2CO3The concentration of the sodium hydroxide is 0.02mol/L) to obtain a mixed solution 2, mixing the mixed solution 1 and the mixed solution 2 (the ratio of the amount of NaOH to the total amount of magnesium and aluminum is 1.6:1, and the ratio of the amount of sodium carbonate to the amount of aluminum nitrate is 2:1) at 4000rpm, carrying out colloid mill for 5min, carrying out hydrothermal crystallization reaction at 110 ℃ for 8h, cooling to room temperature, centrifuging at 4000rpm for 5min, washing the obtained solid component for 3 times with water, washing with ethanol for 3 times, and then drying at 60 ℃ for 12h to obtain the LDHs hydrotalcite.
Example 3
An application of modified hydrotalcite as uvioresistant antioxidant in lubricating oil is prepared by adding modified hydrotalcite (401 APE003I, product of Shandong Wanxinwei materials science and technology Co., Ltd.) into lubricating oil (alkyl naphthalene base oil), and ultrasonically dispersing the modified hydrotalcite uniformly;
the mass ratio of the modified hydrotalcite to the lubricating oil is 0.5: 100.
Example 4
An application of hydrotalcite as an anti-ultraviolet antioxidant in lubricating grease is that the hydrotalcite is added into the lubricating grease (lithium-based grease) and is uniformly mixed by a three-roller machine;
the mass ratio of the hydrotalcite to the lubricating grease is 0.5: 100;
the structure and preparation method of the hydrotalcite are the same as example 1.
Example 5
The application of modified hydrotalcite as an uvioresistant antioxidant in lubricating grease is characterized in that the modified hydrotalcite (401 APE003I, product of Shandong Wanxinwei materials science and technology Co., Ltd.) is added into the lubricating grease (lithium grease) and is uniformly mixed by a three-roller machine;
the mass ratio of the modified hydrotalcite to the lubricating grease is 0.5: 100.
Example 6
The mass ratio of the hydrotalcite to the lubricating oil in example 1 was replaced by 5:100, and the other parameters were the same as in example 1.
Example 7
The mass ratio of hydrotalcite to grease in example 4 was replaced with 5:100, and the other parameters were the same as in example 4.
Comparative example 1
The hydrotalcite from example 1 was replaced with the antioxidant diphenylamine, with the other parameters being the same as in example 1.
Comparative example 2
The hydrotalcite of example 1 was replaced with antioxidant T501, and the other parameters were the same as in example 1.
Comparative example 3
The hydrotalcite of example 1 was replaced with antioxidant T531 and the other parameters were the same as in example 1.
Comparative example 4
The hydrotalcite in example 1 was replaced with antioxidant L101, and the other parameters were the same as in example 1.
Comparative example 5
The hydrotalcite of example 1 was replaced with antioxidant V81, and the other parameters were the same as in example 1.
Comparative example 6
The hydrotalcite from example 4 was replaced with the antioxidant diphenylamine, with the other parameters being the same as in example 4.
Comparative example 7
The hydrotalcite of example 4 was replaced with antioxidant V81, and the other parameters were the same as in example 4.
Comparative example 8
The hydrotalcite of example 4 was replaced with antioxidant T531 and the other parameters were the same as in example 4.
The XRD patterns of the hydrotalcites prepared in example 1 were measured, and the results are shown in fig. 1. As can be seen from FIG. 1, the material prepared by the present invention has hydrotalcite characteristic peaks (003), (006), (009), etc., which indicates that the present invention successfully prepares hydrotalcite and the crystallinity of the sample is high.
The hydrotalcite prepared in example 1 was tested for SEM image and the results are shown in fig. 2. As can be seen from FIG. 2, the hydrotalcite prepared by the present invention has a typical hexagonal sheet structure, further proving that the particle size of the hydrotalcite is about 2 μm when the hydrotalcite is successfully prepared.
The XRD pattern of the hydrotalcite prepared in example 2 was tested, and the result is shown in fig. 3. The hydrotalcite prepared in example 2 was tested for SEM image and the results are shown in fig. 4. As can be seen from fig. 3 and 4, the hydrotalcite material was successfully prepared by the present invention, and the prepared hydrotalcite material was nano-sized.
Transferring the lubricating oil obtained in the embodiments 1, 3 and 1-5 into a watch glass, placing the watch glass into an ultraviolet aging test chamber, carrying out an aging test for 60 hours under the conditions of irradiation of a 340nm ultraviolet lamp and 70 ℃, observing and recording the color change of the lubricating oil, wherein the blank sample does not contain hydrotalcite or antioxidant, and the hydrotalcite, the modified hydrotalcite and diphenylamine are added in the uppermost row from left to right in sequence; the middle row is sequentially added with T501, T531 and L101 from left to right; the bottom row is sequentially added with V81 and blank from left to right.
As can be seen from FIG. 5, after 60h of ultraviolet irradiation, the color of the lubricating oil gradually deepens from colorless, a blank sample changes from colorless to orange yellow, and a sample added with antioxidant diphenylamine and T531 changes from colorless to dark brown, which indicates that the lubricating oil has poor ultraviolet resistance effect and does not have an ultraviolet blocking function; the color change degree of the sample added with the antioxidant V81 is larger, and the performance is poorer; the color change degree of the sample added with the antioxidant T501 and L101 is larger than that of the sample added with the hydrotalcite, which indicates that the performance of the sample is inferior to that of the hydrotalcite material; as can be seen from the figure, the lubricating oil added with hydrotalcite has the minimum color change degree, and the color change degree is smaller than that of a blank sample, which indicates that the hydrotalcite material has obvious anti-ultraviolet effect; the color change degree of the sample added with the modified hydrotalcite is smaller than that of a blank sample, and the hydrotalcite or the modified hydrotalcite is further proved to have excellent ultraviolet resistance effect.
The sample subjected to the aging test was sampled for quantitative analysis, and its light transmittance at 501nm was measured with an ultraviolet spectrophotometer, and the results are shown in Table 1.
TABLE 1 light transmittance of samples before and after UV irradiation
Antioxidant agent Light transmittance before ultraviolet irradiation% Light transmittance after ultraviolet irradiation%
Example 1 Hydrotalcite 98.8 30
Example 3 Modified hydrotalcite 94.8 37.1
Comparison ofExample 1 Diphenylamine 92.8 0.1
Comparative example 2 T501 86.4 17
Comparative example 3 T531 90.2 0
Comparative example 4 L101 95.1 23
Comparative example 5 V81 96.8 1.8
Blank group 99.2 41.4
As can be seen from Table 1, the transmittance of the blank sample is reduced from 99.2% to 41.4% after 60h of ultraviolet irradiation; the light transmittance of the sample added with antioxidant diphenylamine and T531 is almost zero after ultraviolet irradiation; the light transmittance of the sample added with the antioxidant V81 is reduced from 96.8 percent to 1.8 percent; the light transmittance of a sample added with the antioxidant T501 is reduced from 86.4 percent to 17 percent; the light transmittance of the sample added with the hydrotalcite is reduced from 98.8% to 30% after ultraviolet irradiation, and the light transmittance of the sample added with the modified hydrotalcite is reduced to 37.1% after ultraviolet irradiation, which shows that the lubricating oil provided by the invention has excellent ultraviolet resistance.
The greases of example 4 and comparative examples 6-8 were tested for uv resistance using the same method, and the results are shown in fig. 6, where hydrotalcite, T531, blank, V81 and diphenylamine were added in the order from left to right. As can be seen from FIG. 6, after 60h of ultraviolet irradiation, the color of the grease gradually deepens from white, and the color of the sample added with the antioxidant T531 is directly changed from white to black brown, which indicates that the anti-ultraviolet effect is poor; the color of the sample added with the antioxidant V81 and diphenylamine is changed from white to brown, which indicates that the ultraviolet resistance effect is poor; the color change of the sample added with the hydrotalcite is the lightest and is lighter than that of a blank sample, which indicates that the sample has excellent ultraviolet resistance.
The sample of example 6 was subjected to the PDSC oxidative induction period test, test method: using a high-pressure differential scanning calorimeter, adding the simulated lubricating grease to be tested into a PDSC test pool, heating to 180 ℃, keeping the temperature, introducing 3.5MPa pure oxygen after the lubricating grease reaches balance, starting to record a DSC curve at the moment, wherein the curve stably indicates that no oxidation occurs, and recording the time required by the process when an inflection point appears on the curve, wherein the results are shown in Table 2.
TABLE 2 Oxidation Induction time of neat lubricating oils and lubricating oils of example 6
Sample (I) Oxidative induction time/min
Lubricating oil 295
Example 6 1173
As can be seen from Table 2, the oxidation induction time of the lubricating oil is 295min when no hydrotalcite is added, and the oxidation induction time of the lubricating oil reaches 1173min after hydrotalcite is added, which is improved by 4 times compared with a blank sample, so that the oxidation induction time of the lubricating oil is greatly prolonged, and the oxidation stability of hydrotalcite is very good.
The grease bearing life of example 7 was tested according to ASTM D3336 and the results are shown in table 3.
TABLE 3 bearing life of pure greases and greases of example 7
Sample (I) Bearing life/h
Lubricating grease 40h
Example 7 188h
As can be seen from Table 3, the bearing life of the grease was 40 hours without hydrotalcite, and after hydrotalcite was added, the bearing life of the grease was 188 hours, which is 2.5 times that of the blank sample, and the bearing life of the grease was greatly improved.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (10)

1. The application of hydrotalcite or modified hydrotalcite as uvioresistant antioxidant in lubricating oil/grease includes: mixing hydrotalcite or modified hydrotalcite with lubricating oil/grease.
2. The use according to claim 1, wherein the mass ratio of the hydrotalcite or modified hydrotalcite to the lubricating oil/grease is (0.2-5): 100.
3. the use according to claim 2, wherein the mass ratio of the hydrotalcite or modified hydrotalcite to the lubricating oil/grease is (1-5): 100.
4. the use according to claim 3, wherein the mass ratio of the hydrotalcite or modified hydrotalcite to the lubricating oil/grease is (2-5): 100.
5. the use according to claim 1, wherein the hydrotalcite has a general structural formula as shown in formula I:
Figure FDA0003376701960000011
6. use according to claim 5, wherein M in formula I comprises one of Mg, Ca and Zn.
7. The use according to claim 5, wherein N in formula I comprises Al.
8. The use according to claim 5, wherein the molar ratio of M to N in formula I is (2-4): 1.
9. the use according to claim 5, wherein A in formula In-Comprising NO3 -、CO3 2-、Cl-And PO4 3-One kind of (1).
10. The use according to claim 5, wherein x is 1 in formula I: (5-3).
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CN114806674A (en) * 2022-04-24 2022-07-29 北京化工大学 Thickening agent intercalated hydrotalcite, preparation method and application of thickening agent intercalated hydrotalcite as lubricating grease thickening agent
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