阅读说明：本技术 一种高抗磨减摩含钼润滑油添加剂的制备和应用 (Preparation and application of high-wear-resistance antifriction molybdenum-containing lubricating oil additive ) 是由 张晨曦 田国华 于 2019-08-23 设计创作，主要内容包括：本发明涉及润滑油添加剂技术领域,是一种高抗磨减摩润滑油添加剂制备及其应用,所述添加剂使不饱和脂肪酸、二乙醇胺以及含钼化合物反应,最终所得产品中含有钼元素,且不含硫、磷等元素。有机钼是具有优良抗磨减摩效果,在润滑油和润滑脂中有效降低滑动表面的摩擦和磨损,提高载荷能力。延长机器使用寿命,提高了经济效益。本发明列举了几种高抗磨减摩润滑油添加剂的制备,方法简单易行,所用物质环保易降解且价格低廉,适合大规模的产业化生产。(The invention relates to the technical field of lubricating oil additives, in particular to preparation and application of a high-wear-resistance antifriction lubricating oil additive. The organic molybdenum has excellent wear-resistant and antifriction effects, and can effectively reduce friction and wear of sliding surfaces in lubricating oil and lubricating grease and improve load capacity. The service life of the machine is prolonged, and the economic benefit is improved. The invention discloses preparation of a plurality of high-wear-resistance antifriction lubricating oil additives, the method is simple and easy to implement, the used substances are environment-friendly, easy to degrade and low in price, and the preparation method is suitable for large-scale industrial production.)

1. A high wear-resistant antifriction molybdenum-containing lubricating oil additive is characterized in that: the raw materials of the additive comprise fatty acid diethanolamide and sodium molybdate; the fatty acid diethanolamide is diethanolamide containing long carbon chains; the sodium molybdate is sodium molybdate aqueous solution acidified by acetic acid. Fatty acid diethanolamide reacts with sodium molybdate to prepare fatty acid diethanolamide molybdate under the action of an accelerator. The mass percentage of molybdenum in the additive is 1-10%.

2. The fatty acid diethanolamide molybdate according to claim 1 characterized in that: the raw materials for synthesizing the fatty acid diethanolamide comprise monobasic fatty acid, thionyl chloride and diethanolamine, wherein the monobasic fatty acid comprises but not limited to myristoleic acid, palmitoleic acid, oleic acid, ricinoleic acid, erucic acid, linoleic acid, linolenic acid and arachidonic acid and also comprises derivatives of corresponding main components.

3. The fatty acid diethanolamide molybdate according to claim 1 characterized in that: the sodium molybdate is an acetic acid acidified sodium molybdate water solution, and the mass percentage of the sodium molybdate is 50-90%.

4. A method for producing a fatty acid diethanolamide molybdate according to any one of claims 1 to 3, characterized by comprising the following steps:

preparation of fatty acid diethanolamide: adding long-chain fatty acid and thionyl chloride with equal molar weight into a reaction vessel in sequence, reacting for 4 hours, distilling under reduced pressure to remove excessive raw materials to obtain fatty acyl chloride, then adding diethanolamine and dichloromethane with equal molar weight in sequence, and reacting for 6 hours to obtain a target product;

preparation of fatty acid diethanolamide molybdate: weighing a certain mass of long-chain fatty acid or a derivative thereof, adding equimolar amounts of fatty acid diethanolamide and sodium molybdate and a certain amount of accelerator, and reacting at 80-150 ℃ for 15 hours to obtain a target product.

5. The lubricant additive according to claim 1, wherein the accelerator used in the reaction of the product of the amide condensation with the molybdenum-containing compound includes, but is not limited to, alcohols and amides, and the amount of the accelerator added is 1 to 5%.

6. The lubricant additive according to claim 1, wherein the additive is added to the lubricant in an amount of 1 to 10%, preferably 1 to 3%.

Technical Field

The invention relates to the technical field of mechanical friction lubrication, in particular to a high-abrasion-resistance lubricating oil additive.

Background

Friction is unavoidable in the mechanical operation engineering of modern industry, the service life of a machine is shortened or even the machine is scrapped due to excessive wear in the working process of a plurality of mechanical parts, and meanwhile, if energy consumed in the process of acting the friction surface is overcome, other acting forms are inevitably generated, so fuel consumed by wear accounts for a large proportion of the total fuel consumption, the market of lubricating oil is more and more emphasized by various countries, the performance of the lubricating oil is improved to achieve the effects of wear resistance and friction reduction, and the significance of the lubricating oil to national economy is not ignored. The research on lubricating oil additives is also increasingly important in order to improve the tribological properties of base oils or general lubricating oils.

The molybdenum series additive is one of extreme pressure antiwear lubricant additives and is also an accepted environment-friendly lubricant additive. The global molybdenum ore reserves are about 1500 million tons, and are mainly distributed in countries such as the United states, China, Chile, Russia, Canada and the like, and China is one of the countries with the most abundant molybdenum resources in the world. The molybdenum element has excellent tribological performance, is suitable for preparing various high-grade lubricating oil (grease), and is widely used as a lubricating agent for various mechanical equipment, such as gear oil, turbine oil, engine oil and the like. The addition of the lubricating oil additive obviously improves the friction phenomenon of the machine during operation, improves the working efficiency and reduces the oil consumption.

The earliest studies on molybdenum-containing lubricating oil additives began with molybdenum disulfide. Although excellent lubricity can be achieved, due to the characteristics of the layered structure, the additive cannot be dispersed in oil, is insoluble and insoluble in an organic system, and greatly limits the use, so that some oil-soluble molybdenum-containing additives are applied to lubricating oil. Lubricating oil additives are indispensable and increasingly demanded in modern industries in China, and China also faces a plurality of key technical problems in the research of molybdenum series lubricating oil additives, such as synthesis technology, stability in the use of additives and the like. And domestic similar products have the problems of low molybdenum content, deep color, still unsatisfactory oil solubility and the like, so that the development of a novel molybdenum-containing lubricating oil additive with excellent performance is necessary.

Disclosure of Invention

In view of the above background problems, the present invention aims to provide a method for preparing a lubricating oil additive with excellent wear resistance and friction reduction performance by reacting an unsaturated fatty acid with a molybdenum-containing compound, so as to improve the friction resistance and lubricity of the lubricating oil.

In one aspect of the present invention, the present invention provides a method for preparing a lubricating oil additive by reacting an unsaturated fatty acid with a molybdenum-containing compound.

Wherein, the raw material in the synthesis of the molybdenum-containing lubricating oil additive comprises unsaturated fatty monobasic acid and unsaturated fatty polybasic acid. The oil containing unsaturated fatty monobasic acid and unsaturated fatty polybasic acid includes but is not limited to myristoleic acid, palmitoleic acid, oleic acid, ricinoleic acid, erucic acid, linoleic acid, linolenic acid and arachidonic acid, and also includes derivatives of corresponding main components, preferably oleic acid and derivatives thereof.

The fat and the corresponding derivatives of the unsaturated fatty monoacid and the unsaturated fatty polyacid can be food grade and also can be industrial grade.

Wherein, the molybdenum element in the molybdenum-containing lubricating oil additive accounts for about 1 to 10 percent of the additive content.

As another aspect of the invention, the invention provides a preparation method for preparing an anti-wear and anti-friction lubricating oil additive by using a molybdenum-containing compound, which comprises the following steps:

weighing a certain mass of oleic acid or derivatives thereof, adding alcohol amine and sodium molybdate with different mass percentages and promoters with different mass percentages, and reacting for 15 hours at 80-150 ℃ to obtain a target product.

Wherein, the accelerant includes but not limited to alcohols and amides. The addition amount of the organic silicon compound can be 1-5%, and the preferable amount is 3%.

As another aspect of the invention, the invention also provides a preparation method of the wear-resistant and antifriction lubricating oil containing the molybdenum element, which comprises the following steps:

the molybdenum-containing anti-wear and anti-friction lubricating oil additive prepared by the preparation method is directly added into lubricating oil and uniformly mixed to obtain a target product;

wherein the mass percentage of the anti-wear and anti-friction lubricating oil additive prepared by reacting the prepared unsaturated fatty acid with a molybdenum-containing compound in the lubricating oil is 1-10%, and preferably 1-3%.

The synthesis method adopted by the invention is simple, convenient and safe to operate, can be degraded, meets the requirements of low toxicity and environmental friendliness, and is practical and economical. The composite material can be used for mechanical equipment, obviously improves the friction resistance, effectively protects the machine and reduces the loss of non-renewable energy. .

Drawings

Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. Also, like reference numerals are used to refer to like parts throughout the drawings. In the drawings:

FIG. 1 is a flow chart of the process for preparing the molybdenum-containing lubricating oil additive of the present invention

FIG. 2 shows P in base oils for different amounts of molybdenum-containing lubricant additives_BValue of

FIG. 3 is a graph of the coefficient of friction of various amounts of molybdenum-containing lubricating oil additives in base oils

Detailed Description

Exemplary embodiments of the present disclosure will be described in more detail below with reference to the accompanying drawings. While exemplary embodiments of the present disclosure are shown in the drawings, it should be understood that the present disclosure may be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art.

The molybdenum-containing high-antiwear antifriction lubricating oil additive is made up by using oleic acid or its derivative including myristoleic acid, palmitoleic acid, oleic acid, ricinoleic acid, erucic acid, linoleic acid, linolenic acid and arachidonic acid, and acidified aqueous solution of sodium molybdate, and the described accelerating agent includes but not limited to alcohols, polyethanol and amides.

As shown in figure 1, the invention discloses a preparation method for preparing a molybdenum-containing high-antiwear lubricating oil additive. Comprises the following steps:

weighing a certain mass of oleic acid or derivatives thereof, adding alcohol amine and sodium molybdate with different mass percentages and promoters with different mass percentages, and reacting for 15 hours at 80-150 ℃ to obtain a target product. The mass percentage of the prepared high-wear-resistance antifriction molybdenum-containing lubricating oil additive in the lubricating oil is 1-10%, and preferably 1-3%.

The above description is only exemplary of the present invention and should not be taken as limiting the invention, as any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

The present invention is described in more detail below with reference to specific examples.

Example 1

Adding diethanolamine into oleic acid, uniformly mixing, heating to 150 ℃, reacting for 3-5 hours, cooling to 60-70 ℃, continuously adding diethanolamine and a small amount of alkali liquor, and reacting for 5-6 hours to obtain an intermediate product. And under the protection of nitrogen, heating, adding an acidified sodium molybdate aqueous solution (the material ratio of sodium molybdate to oleic acid diethanolamide is 0.1: 1), reacting for 3-5 hours, and naturally cooling at room temperature to obtain the target product.

Example 2

Adding diethanolamine into myristic acid, uniformly mixing, heating to 140 ℃, reacting for 3-5 hours, cooling to 60-70 ℃, continuously adding diethanolamine and a small amount of alkali liquor, and reacting for 5-6 hours to obtain an intermediate product. And under the protection of nitrogen, heating, adding an acidified sodium molybdate aqueous solution (the molar ratio of sodium molybdate to the intermediate product is 0.3: 1), reacting for 3-5 hours, and naturally cooling at room temperature to obtain the target product.

Example 3

Adding diethanolamine into palmitoleic acid, uniformly mixing, heating to 145 ℃, reacting for 3-5 hours, cooling to 60-70 ℃, continuously adding diethanolamine and a small amount of alkali liquor, and reacting for 5-6 hours to obtain an intermediate product. And under the protection of nitrogen, heating, adding an acidified sodium molybdate aqueous solution (the molar ratio of sodium molybdate to the intermediate product is 0.5: 1), reacting for 3-5 hours, and naturally cooling at room temperature to obtain the target product.

Example 4

Adding diethanolamine into ricinoleic acid, uniformly mixing, heating to 155 ℃, reacting for 3-5 hours, cooling to 60-70 ℃, continuously adding diethanolamine and a small amount of alkali liquor, and reacting for 5-6 hours to obtain an intermediate product. And under the protection of nitrogen, heating, adding an acidified sodium molybdate aqueous solution (the molar ratio of sodium molybdate to the intermediate product is 0.1: 1), reacting for 3-5 hours, and naturally cooling at room temperature to obtain the target product.

Example 5

Adding diethanolamine into erucic acid, uniformly mixing, heating to 160 ℃, reacting for 3-5 hours, cooling to 60-70 ℃, continuously adding diethanolamine and a small amount of alkali liquor, and reacting for 5-6 hours to obtain an intermediate product. And under the protection of nitrogen, heating, adding an acidified sodium molybdate aqueous solution (the molar ratio of sodium molybdate to the intermediate product is 0.3: 1), reacting for 3-5 hours, and naturally cooling at room temperature to obtain the target product.

Example 6

Adding diethanolamine into linoleic acid, uniformly mixing, heating to 155 ℃, reacting for 3-5 hours, cooling to 60-70 ℃, continuously adding diethanolamine and a small amount of alkali liquor, and reacting for 5-6 hours to obtain an intermediate product. And under the protection of nitrogen, heating, adding an acidified sodium molybdate aqueous solution (the molar ratio of sodium molybdate to oleic acid diethanolamide is 0.5: 1), reacting for 3-5 hours, and naturally cooling at room temperature to obtain the target product.

Example 7

Adding diethanolamine into arachidonic acid, mixing uniformly, heating to 145 ℃, reacting for 3-5 hours, cooling to 60-70 ℃, continuously adding diethanolamine and a small amount of alkali liquor, and reacting for 5-6 hours to obtain an intermediate product. And under the protection of nitrogen, heating, adding an acidified sodium molybdate aqueous solution (the molar ratio of sodium molybdate to the intermediate product is 0.7: 1), reacting for 3-5 hours, and naturally cooling at room temperature to obtain the target product.

Wherein, the base oil can be used as the commercial lubricating oil additive.

Testing of storage stability:

the prepared target product is kept stand for 15 days and 30 days, and the condition of the target product is observed.

Through experiments, after 15 days, the high-wear-resistance antifriction molybdenum-containing lubricating oil additive has no precipitation and delamination. Even after 30 days, the lubricant additive still has no precipitation stratification, which indicates that the lubricant additive is very stable.

Testing of hydrolytic stability

And (3) standing the prepared target product for 5 days, 10 days, 15 days, 20 days, 25 days and 30 days in an open manner, and observing the condition of the target product. Through experiments, the high anti-wear lubricating oil additive has no turbidity after 10 days, and even after 30 days, the high anti-wear lubricating oil additive also has no turbidity, which indicates that the lubricating oil additive has high hydrolysis stability. The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.

TABLE 1P in base oils with different amounts of additives_BValue of

Adding amount of	0％	1.0％	1.5％	2.0％
					PBValue of	570N	1021N	1093N	1031N

TABLE 2 hydrolytic stability of lubricating oil additives

Days of rest	5 days	10 days	15 days
				Phenomenon(s)	Without obvious change	Without obvious change	Without obvious change

Days of rest	20 days	25 days	30 days
				Phenomenon(s)	Without obvious change	Without obvious change	Without obvious change