CN108410540B - Nano zinc oxide composite antioxidant material and preparation method and application thereof - Google Patents
Nano zinc oxide composite antioxidant material and preparation method and application thereof Download PDFInfo
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- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
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- 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
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- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
- C10M2215/04—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms
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- C10N2020/00—Specified physical or chemical properties or characteristics, i.e. function, of component of lubricating compositions
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- 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
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
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Abstract
The invention belongs to the technical field of lubricating oil, and relates to a nano zinc oxide composite antioxidant material which is mainly prepared from the following raw materials in parts by weight: 0.3-2 parts of zinc chloride, 10-25 parts of distilled water, 0.1-0.8 part of sodium hydroxide, 1-5 parts of organic antioxidant, 0.5-5 parts of amine compound and 50-80 parts of ethanol. The invention also provides a preparation method of the nano zinc oxide composite antioxidant material, and the nano zinc oxide composite antioxidant material is used as an antioxidant to be added into lubricating oil, so that the antioxidant capacity of the lubricating oil can be obviously improved, the increase of the acid value and the viscosity of an oil product is effectively inhibited, the oil change period is prolonged, the economic benefit is improved, and the nano zinc oxide composite antioxidant material has a good application prospect.
Description
Technical Field
The invention belongs to the technical field of lubricating oil additives, and particularly relates to a nano zinc oxide composite antioxidant material, a preparation method thereof and application of the nano zinc oxide composite antioxidant material as a lubricating oil antioxidant.
Background
The oxidation stability of lubricating oil is one of the important indexes for evaluating the performance of lubricating oil. In the using process of the lubricating oil, the lubricating oil is easily oxidized and deteriorated under the influence of factors such as ambient oxygen, temperature, metal ion catalysis and the like, so that the lubricating performance of the lubricating oil is rapidly reduced. Therefore, an antioxidant is required to be added to improve the oxidation stability of the oil product, prevent the oil product from being oxidized, prolong the oil change period and protect equipment.
With the increasing quality grades of lubricating oils, stringent requirements are placed on viscosity increase control, deposit reduction, and wear reduction, as well as higher requirements on antioxidant performance and thermal stability. In lubricating oils, researchers have developed several classes of effective antioxidants, the major classes of which include masked phenolic compounds and amines, both organic and less thermally stable. In the case of local high temperature of the friction pair, the organic antioxidant may volatilize and even decompose, so it is a necessary trend to study the high temperature antioxidant. Inorganic materials such as zinc oxide, cerium oxide and the like have better thermal stability and chemical inertness, also have the capability of removing free radicals, and can be used as an antioxidant to be applied in the fields of macromolecules and biology; however, when the antioxidant is used in lubricating oil as an antioxidant, the antioxidant capacity is poor, and the requirement of industrial application cannot be met.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a nano zinc oxide composite antioxidant material, which solves the problems of the prior antioxidant in the using process, is added into lubricating oil as the antioxidant, has good dispersion stability, can obviously improve the oxidation stability of the lubricating oil at high temperature and prolong the service life of the lubricating oil, and has wide application prospect.
The invention also provides a preparation method of the nano zinc oxide composite antioxidant material and application of the nano zinc oxide composite antioxidant material as a lubricating oil antioxidant.
In order to achieve the purpose, the invention adopts the following technical scheme:
a nano-zinc oxide composite antioxidant material is characterized in that an organic antioxidant is used as a modifier and is connected to the surface of nano-zinc oxide; the composite antioxidant material is mainly prepared from the following raw materials in parts by weight:
0.3 to 2 parts of zinc chloride,
10-25 parts of distilled water,
0.1 to 0.8 part of sodium hydroxide,
1-5 parts of an organic antioxidant,
0.5 to 5 parts of amine compound,
50-80 parts of ethanol.
The preparation method of the nano-zinc oxide composite antioxidant material specifically comprises the following steps:
1) taking the raw materials in proportion, dissolving zinc chloride in a proper amount of distilled water to form a solution A, dissolving sodium hydroxide in the balance of distilled water to form a solution B, mixing and stirring the solution A and the solution B, and performing suction filtration and washing to obtain a white solid product a;
2) uniformly dispersing the solid product a obtained in the step 1) by using a proper amount of ethanol, then adding an organic antioxidant, and stirring for reaction to obtain a light yellow solid product b;
3) uniformly mixing the solid product b obtained in the step 2) with the balance of ethanol (generally stirring at room temperature for 20-40 min), adding an amine compound, and reacting at 40-60 ℃ for 4-15 h; and after the reaction is finished, performing centrifugal separation, taking the solid, and washing and drying the solid to obtain a sand-yellow solid product.
Specifically, in the step 1), mixing and stirring are carried out at room temperature, and the mixing and stirring time is 5-30 min.
Specifically, in the step 2), stirring reaction is carried out at room temperature, and the stirring reaction time is 0.5-5 h.
The invention also provides the application of the nano zinc oxide composite antioxidant material as a lubricating oil antioxidant. In the invention, the organic antioxidant and the amine compound can be conventional compounds in the field. Specifically, the organic antioxidant may be a hindered phenol type antioxidant containing a reactive functional group, such as methyl 3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate, etc.; the amine compound can be organic amine compound, such as tetraethylammonium hydroxide, tetrabutylammonium hydroxide, tetrapropylammonium hydroxide, etc.
The invention takes an organic antioxidant as a modifier, and prepares a nano zinc oxide composite material with a surface modified with organic antioxidant molecules by an in-situ modification method; the antioxidant is added into the lubricating oil as an antioxidant, has good dispersion stability, can obviously improve the oxidation stability of the lubricating oil at high temperature, prolongs the service life of the lubricating oil, and has wide application prospect. Compared with the prior art, the invention has the following advantages:
1) according to the invention, the organic antioxidant and the inorganic nano zinc oxide are compounded together, so that the thermal stability of the composite material is improved, and the novel nano antioxidant is prepared;
2) the organic antioxidant is connected to the surface of the nano zinc oxide as a modifier, and the dispersion stability of the nano zinc oxide in the lubricating oil can be improved due to the existence of the organic antioxidant modifier;
3) the invention provides a preparation method of an organic antioxidant and nano zinc oxide composite material, and the organic antioxidant and nano zinc oxide composite material is used as an antioxidant to be added into lubricating oil, so that the oxidation stability of the lubricating oil can be obviously improved, the oil change period is prolonged, the economic benefit is improved, and the organic antioxidant and nano zinc oxide composite material has a good application prospect;
4) the preparation process has the advantages of simple equipment, cheap and easily-obtained raw materials, low cost and high yield, and is suitable for large-scale industrial production.
Drawings
FIG. 1 is an optical photograph of the nano-zinc oxide composite antioxidant material prepared in example 1 of the present invention;
FIG. 2 is a TEM photograph of the nano-zinc oxide composite antioxidant material prepared in example 1 of the present invention;
FIG. 3 is an optical photograph of the nano-zinc oxide composite antioxidant material prepared in example 1 of the present invention dispersed in DIOS;
FIG. 4 shows the oxidation induction time of the nano zinc oxide composite antioxidant material prepared in example 1 of the present invention obtained by the rotating oxygen bomb test under different contents.
Detailed Description
The present invention will now be described in detail with reference to specific examples, which are intended to be illustrative only and should not be construed as limiting the scope of the invention. The insubstantial modifications and adaptations of the present invention as described above will now occur to those skilled in the art and are considered to be within the scope of the present invention.
In the following examples, the raw materials were used in parts by weight.
Example 1
A nano zinc oxide composite antioxidant material is prepared from the following raw materials in parts by weight: 0.3 part of zinc chloride, 15 parts of distilled water, 0.5 part of sodium hydroxide, 3 parts of hindered phenol organic antioxidant 3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid, 5 parts of organic amine compound tetraethylammonium hydroxide and 70 parts of ethanol.
The preparation method of the organic antioxidant modified nano-zinc oxide composite antioxidant material specifically comprises the following steps:
1) dissolving 0.3 part of zinc chloride in 10 parts of distilled water to form a solution A, dissolving 0.5 part of sodium hydroxide in 5 parts of distilled water to form a solution B, mixing and stirring the solution A and the solution B for 10min, and performing suction filtration and washing to obtain a white solid product a;
2) uniformly dispersing the solid product a obtained in the step 1) in 10 parts of ethanol, then adding 3 parts of hindered phenol organic antioxidant 3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid, and stirring for reaction for 3 hours to obtain a light yellow solid product b;
3) adding the solid product b obtained in the step 2) into 60 parts of ethanol, uniformly mixing, adding 5 parts of organic amine compound tetraethylammonium hydroxide, and reacting at 50 ℃ for 4 hours; and after the reaction is finished, performing centrifugal separation, taking the solid, washing and drying to obtain the sand-yellow solid product nano zinc oxide composite antioxidant material.
FIG. 1 is an optical photograph of the nano-zinc oxide composite antioxidant material prepared in example 1, and FIG. 2 is a transmission electron microscope photograph of the nano-zinc oxide composite antioxidant material prepared in example 1. As can be seen from the figure: the obtained nano zinc oxide composite antioxidant material has small grain diameter, very uniform dispersion and average grain diameter of about 5 nm.
Example 2
A nano zinc oxide composite antioxidant material is prepared from the following raw materials in parts by weight: 1 part of zinc chloride, 20 parts of distilled water, 0.2 part of sodium hydroxide, 2 parts of hindered phenol organic antioxidant methyl 3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate, 3 parts of organic amine compound tetrabutylammonium hydroxide and 80 parts of ethanol.
The preparation method of the organic antioxidant modified nano-zinc oxide composite antioxidant material specifically comprises the following steps:
1) dissolving 1 part of zinc chloride in 15 parts of distilled water to form a solution A, dissolving 0.2 part of sodium hydroxide in 5 parts of distilled water to form a solution B, mixing and stirring the solution A and the solution B for 15min, and performing suction filtration and washing to obtain a white solid product a;
2) uniformly dispersing the solid product a obtained in the step 1) in 10 parts of ethanol, then adding 2 parts of hindered phenol organic antioxidant 3- (3, 5-di-tert-butyl-4-hydroxyphenyl) methyl propionate, and stirring for reacting for 1h to obtain a light yellow solid product b;
3) adding the solid product b obtained in the step 2) into 70 parts of ethanol, uniformly mixing, adding 3 parts of organic amine compound tetrabutyl ammonium hydroxide, and reacting at 55 ℃ for 8 hours; and after the reaction is finished, performing centrifugal separation, taking the solid, washing and drying to obtain the sand-yellow solid product nano zinc oxide composite antioxidant material.
Example 3
A nano zinc oxide composite antioxidant material is prepared from the following raw materials in parts by weight: 0.8 part of zinc chloride, 25 parts of distilled water, 0.8 part of sodium hydroxide, 5 parts of hindered phenol organic antioxidant 3- (3, 5-di-tert-butyl-4-hydroxyphenyl) methyl propionate, 5 parts of organic amine compound tetrapropyl ammonium hydroxide and 70 parts of ethanol.
The preparation method of the organic antioxidant modified nano-zinc oxide composite antioxidant material specifically comprises the following steps:
1) dissolving 0.8 part of zinc chloride in 15 parts of distilled water to form a solution A, dissolving 0.8 part of sodium hydroxide in 10 parts of distilled water to form a solution B, mixing and stirring the solution A and the solution B for 20min, and performing suction filtration and washing to obtain a white solid product a;
2) uniformly dispersing the solid product a obtained in the step 1) in 10 parts of ethanol, then adding 5 parts of phenol-resistant organic antioxidant 3- (3, 5-di-tert-butyl-4-hydroxyphenyl) methyl propionate, and stirring for reacting for 4 hours to obtain a light yellow solid product b;
3) adding the solid product b obtained in the step 2) into 60 parts of ethanol, uniformly mixing, adding 5 parts of organic amine compound tetrapropylammonium hydroxide, and reacting at 60 ℃ for 10 hours; and after the reaction is finished, performing centrifugal separation, taking the solid, washing and drying to obtain the sand-yellow solid product nano zinc oxide composite antioxidant material.
Example 4
A nano zinc oxide composite antioxidant material is prepared from the following raw materials in parts by weight: 0.5 part of zinc chloride, 10 parts of distilled water, 0.1 part of sodium hydroxide, 1 part of hindered phenol organic antioxidant 3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid, 2 parts of organic amine compound tetrabutyl ammonium hydroxide and 70 parts of ethanol.
The preparation method of the organic antioxidant modified nano zinc oxide composite material specifically comprises the following steps:
1) dissolving 0.5 part of zinc chloride in 5 parts of distilled water to form a solution A, dissolving 0.1 part of sodium hydroxide in 5 parts of distilled water to form a solution B, mixing and stirring the solution A and the solution B for 15min, and performing suction filtration and washing to obtain a white solid product a;
2) uniformly dispersing the solid product a obtained in the step 1) in 20 parts of ethanol, then adding 1 part of hindered phenol organic antioxidant 3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid, and stirring for reaction for 3 hours to obtain a light yellow solid product b;
3) adding the solid product b obtained in the step 2) into 50 parts of ethanol, uniformly mixing, adding 2 parts of tetrabutylammonium hydroxide serving as an organic amine compound, and reacting at 50 ℃ for 6 hours; and after the reaction is finished, performing centrifugal separation, taking the solid, washing and drying to obtain the sand-yellow solid product nano zinc oxide composite antioxidant material.
Example 5
A nano zinc oxide composite antioxidant material is prepared from the following raw materials in parts by weight: 2 parts of zinc chloride, 20 parts of distilled water, 0.5 part of sodium hydroxide, 3 parts of hindered phenol organic antioxidant 3- (3, 5-di-tert-butyl-4-hydroxyphenyl) methyl propionate, 3 parts of organic amine compound tetrapropyl ammonium hydroxide and 58 parts of ethanol.
A preparation method of an organic antioxidant modified nano zinc oxide composite material specifically comprises the following steps:
1) dissolving 2 parts of zinc chloride in 15 parts of distilled water to form a solution A, dissolving 0.5 part of sodium hydroxide in 5 parts of distilled water to form a solution B, mixing and stirring the solution A and the solution B for 30min, and performing suction filtration and washing to obtain a white solid product a;
2) uniformly dispersing the solid product a obtained in the step 1) in 8 parts of ethanol, then adding 3 parts of hindered phenol organic antioxidant 3- (3, 5-di-tert-butyl-4-hydroxyphenyl) methyl propionate, and stirring for reacting for 2 hours to obtain a light yellow solid product b;
3) adding the solid product b obtained in the step 2) into 50 parts of ethanol, uniformly mixing, adding 3 parts of organic amine compound tetrapropylammonium hydroxide, and reacting at 60 ℃ for 12 h; and after the reaction is finished, performing centrifugal separation, taking the solid, washing and drying to obtain the sand-yellow solid product nano zinc oxide composite antioxidant material.
Application test:
FIG. 3 is a photograph showing the dispersion of the nano-zinc oxide composite antioxidant prepared in example 1 of the present invention dissolved in diisooctyl sebacate (DIOS for short), and it can be seen from the figure that: the obtained sample has good solubility.
FIG. 4 shows the results of the rotating oxygen bomb test of the nano-zinc oxide composite antioxidant material prepared in example 1 of the present invention in DIOS. As can be seen in fig. 4: the oxidation induction time of the unadditized DIOS base oil was 44 min; after 0.25wt% of the nano zinc oxide composite antioxidant material prepared in the example 1 is added, the antioxidant time is increased to 119 min; after 0.5wt% of the nano zinc oxide composite antioxidant material prepared in the example 1 is added, the antioxidant time is increased to 139 min; after 0.75wt% of the nano zinc oxide composite antioxidant material prepared in the example 1 is added, the antioxidant time is increased to 150 min; after 1wt% of the nano zinc oxide composite antioxidant material prepared in example 1 was added, the antioxidant time was increased to 149 min. The comparison shows that the antioxidant effect of the nano composite antioxidant prepared by the invention is obviously improved.
The nano zinc oxide composite antioxidant material prepared in the example 1 is added into base oil polyalphaolefin (PAO for short), and the oxidation induction time is measured by utilizing a pressure differential scanning calorimetry. Under the conditions of high pressure and pure oxygen at 180 ℃ and 3.5MPa, the oxidation induction time of the PAO base oil which is not added is 6 min; the nano zinc oxide composite antioxidant material prepared by separately adding 0.5wt% of the PAO can prolong the oxidation induction time to 19 min. Under the conditions of 170 ℃ and 3.5MPa of high-pressure pure oxygen, the oxidation induction time of the PAO not added is 13.8 min; the nano zinc oxide composite antioxidant material prepared by separately adding 0.5wt% of the PAO can prolong the oxidation induction time to 40.1 min.
The nano zinc oxide composite antioxidant material prepared in the example 1 is added into DIOS base oil, and the oxidation induction time is measured by using a pressure differential scanning calorimetry method. Under the conditions of 190 ℃ and 3.5MPa of high-pressure pure oxygen, the oxidation induction time of the unadditized DIOS base oil is 4.1 min; the nano zinc oxide composite antioxidant material prepared by separately adding 0.5wt% in DIOS can prolong the oxidation induction time to 8.6 min. Under the conditions of high pressure pure oxygen of 180 ℃ and 3.5MPa, the oxidation induction time of the unadditized DIOS is 5.8 min; the nano zinc oxide composite antioxidant material prepared by separately adding 0.5wt% in DIOS can prolong the oxidation induction time to 17.6 min.
The nano zinc oxide composite antioxidant material prepared in the example 1 is added into liquid paraffin, and the oxidation induction time is measured by utilizing a pressure differential scanning calorimetry method. Under the conditions of 170 ℃ and 3.5MPa of high-pressure pure oxygen, the oxidation induction time of the liquid paraffin which is not added is 4.7 min; the nano zinc oxide composite antioxidant material prepared by separately adding 0.5wt% of the nano zinc oxide composite antioxidant material into the liquid paraffin can prolong the oxidation induction time to 7.3 min. Under the conditions of 160 ℃ and 3.5MPa of high-pressure pure oxygen, the oxidation induction time of the liquid paraffin which is not added is 8.4 min; the nano zinc oxide composite antioxidant material prepared by separately adding 0.5wt% of the nano zinc oxide composite antioxidant material into the liquid paraffin can prolong the oxidation induction time to 11.9 min.
The antioxidant properties of the nanocomposite antioxidants prepared in examples 2 to 5 were also determined by a rotary oxygen bomb test and a pressure differential scanning calorimetry test. The test result shows that: the performance of the products prepared in the embodiments 2 to 5 is equivalent to the antioxidant performance of the nano zinc oxide composite antioxidant material prepared in the embodiment 1, namely the oxidation induction time is obviously prolonged, the service life of the lubricating oil can be prolonged, and the application prospect is good.
In summary, it can be seen that: the organic antioxidant modified nano zinc oxide composite antioxidant material is used as an antioxidant and added into lubricating oil, can obviously improve the antioxidant capacity of the lubricating oil, effectively inhibit the increase of the acid value and the viscosity of an oil product, prolong the oil change period, improve the economic benefit and have good application prospect.
Claims (5)
1. The nano zinc oxide composite antioxidant material is characterized by being mainly prepared from the following raw materials in parts by weight:
0.3 to 2 parts of zinc chloride,
10-25 parts of distilled water,
0.1 to 0.8 part of sodium hydroxide,
1-5 parts of an organic antioxidant,
0.5 to 5 parts of amine compound,
50-80 parts of ethanol;
the organic antioxidant is 3- (3, 5-di-tert-butyl-4-hydroxyphenyl) methyl propionate or 3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid; the amine compound is tetraethyl ammonium hydroxide, tetrabutyl ammonium hydroxide or tetrapropyl ammonium hydroxide.
2. The preparation method of the nano zinc oxide composite antioxidant material as claimed in claim 1, is characterized by comprising the following steps:
1) taking the raw materials in proportion, dissolving zinc chloride in a proper amount of distilled water to form a solution A, dissolving sodium hydroxide in the balance of distilled water to form a solution B, mixing and stirring the solution A and the solution B, and performing suction filtration and washing to obtain a solid product a;
2) uniformly dispersing the solid product a obtained in the step 1) by using a proper amount of ethanol, then adding an organic antioxidant, and stirring for reaction to obtain a solid product b;
3) uniformly mixing the solid product b obtained in the step 2) with the balance of ethanol, adding an amine compound, and reacting at 40-60 ℃ for 4-15 h; after the reaction is finished, centrifugal separation is carried out, and the solid is taken out, washed and dried to obtain the catalyst.
3. The preparation method of the nano zinc oxide composite antioxidant material as claimed in claim 2, wherein in the step 1), the mixing and stirring are carried out at room temperature for 5-30 min.
4. The preparation method of the nano zinc oxide composite antioxidant material as claimed in claim 2, wherein in the step 2), the stirring reaction is carried out at room temperature for 0.5-5 h.
5. The use of the nano zinc oxide composite antioxidant material of claim 1 as an antioxidant for lubricating oil.
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