阅读说明：本技术 一种宽范围多皂基自修复润滑脂及其制备方法 (Wide-range multi-soap-base self-repairing lubricating grease and preparation method thereof ) 是由 文永鹏 张振忠 张青青 黎雁英 文永飞 林俊宇 粟保金 于 2019-09-20 设计创作，主要内容包括：本发明公开了一种宽范围多皂基自修复润滑脂及其制备方法。所述的润滑脂按质量百分比计,由下述组成制成：金属粉0.2～2％、蛇纹石粉0.2～2％、分散剂0.1～2％、余量为基础脂。本发明所述润滑脂不仅具有优良的抗磨性能和减摩效果,还对摩擦副表面具有较好的自修复功能,适用于各种摩擦副部件的润滑,有利于提高其使用寿命；而且制备方法简单。(The invention discloses a wide-range multi-soap-base self-repairing lubricating grease and a preparation method thereof. The lubricating grease is prepared from the following components in percentage by mass: 0.2-2% of metal powder, 0.2-2% of serpentine powder, 0.1-2% of dispersing agent and the balance of basic grease. The lubricating grease disclosed by the invention has excellent wear resistance and antifriction effect, also has a good self-repairing function on the surface of a friction pair, is suitable for lubricating various friction pair components, and is beneficial to prolonging the service life of the friction pair components; and the preparation method is simple.)

1. a wide-range multi-soap-base self-repairing lubricating grease is characterized in that: the composite material is prepared from the following components in percentage by mass:

0.2-2% of metal powder, 0.2-2% of serpentine powder, 0.1-2% of dispersant and the balance of basic grease, wherein:

the metal powder is one or the combination of more than two of nano copper powder, nickel powder, tin powder and bismuth powder;

the dispersant is a combination of more than two of oleic acid, dimethyl silicone oil, dodecahydroxy stearic acid and polyvinyl alcohol;

the basic grease is a lubricating grease product which meets the physical and chemical performance indexes of international standard, national standard or industrial standard.

2. The wide range multi-soap-based self-healing grease of claim 1, wherein: the weight percentage of each component is as follows:

0.4-1% of metal powder, 0.4-1% of serpentine powder, 0.2-2% of dispersing agent and the balance of basic grease.

3. The wide range multi-soap based self-healing grease of claim 1 or 2, wherein: the particle size of the metal powder is 10-500 nm.

4. The wide range multi-soap based self-healing grease of claim 1 or 2, wherein: the particle size of the serpentine powder is 10-500 nm.

5. The method of making the broad range multi-soap based self-healing grease of claim 1 comprising the steps of:

1) weighing the components according to the formula for later use;

2) dispersing agent and absolute ethyl alcohol are mixed according to the proportion of 1: mixing the materials in a mass ratio of 20-30, and performing ultrasonic dispersion to obtain a dispersion solution; adding metal powder into the solution, and performing ultrasonic dispersion to obtain a metal powder solution subjected to coating dispersion treatment;

3) adding serpentine powder into the metal powder solution subjected to coating and dispersion treatment, and performing ultrasonic dispersion and shearing dispersion to obtain a nano metal/ore composite solution;

4) removing the dispersion medium from the obtained nano metal/ore composite solution to obtain nano metal/ore composite powder;

5) mixing the obtained nano metal/ore composite powder with basic grease, homogenizing, and performing three-roller grinding for multiple times to obtain the final product.

6. The method of claim 5, wherein: in the step 2), in the steps 2) and 3), ultrasonic dispersion is carried out at the temperature of 30-50 ℃.

7. The method of claim 5, wherein: in the step 3), the shearing and dispersing are carried out at the rotating speed of 800-3000 rpm for 30-60 min.

8. The method of claim 5, wherein: in the step 5), homogenizing is carried out at a rotating speed of 50-500 rpm for 10-20 min.

Technical Field

The invention relates to lubricating grease, in particular to wide-range multi-soap-base self-repairing lubricating grease and a preparation method thereof.

Background

At present, the research range of nano lubricating additives, particularly self-repairing additives, at home and abroad is wide, but as most of the nano lubricating additives are metal friction pairs in actual mechanical equipment, a firm and non-falling self-repairing layer needs to be formed, the expansion coefficient of the repairing layer is required to be basically consistent with the expansion coefficient of the friction pairs, and the nano lubricating additives and the self-repairing additives can be effectively realized only by forming firm combination with the friction pairs. At present, the expansion coefficient of the lubricating additive containing nano soft metal powder and natural serpentine ore powder is only close to that of a metal friction pair, and a self-repairing compensation layer which is integrated with the friction pair and cannot fall off is formed under the action of friction energy, so that the lubricating additive is mainly concentrated on the two series at home and abroad and research. In contrast, when the nano soft metal powder lubricating additive generates a self-repairing effect, the required friction energy is low, the self-repairing speed is high, the wear-resistant and anti-friction performance is good, but the preparation cost is high. The nano serpentine mineral powder lubricating additive has good wear resistance and extreme pressure performance, but the required repairing energy is very high, and the friction reducing performance is relatively low. Therefore, the development trend is to prepare a composite lubricating friction self-repairing product combining the advantages of the two.

In the prior art, most of the preparation processes of the lubricating grease added with the nano particles are complex, the influence of compatibility of various additives needs to be considered in the esterification and saponification processes of the lubricating grease, and if the selection is not reasonable, the comprehensive performance of the obtained product is reduced.

Disclosure of Invention

The technical problem to be solved by the invention is to provide the wide-range multi-soap-base self-repairing lubricating grease which has very good intermiscibility and compatibility with lubricating grease of various thickening agents and the preparation method thereof.

In order to solve the technical problems, the invention adopts the following technical scheme:

a wide-range multi-soap-base self-repairing lubricating grease is prepared from the following components in percentage by mass:

0.2-2% of metal powder, 0.2-2% of serpentine powder, 0.1-2% of dispersant and the balance of basic grease, wherein:

the metal powder is one or the combination of more than two of nano copper powder, nickel powder, tin powder and bismuth powder;

the dispersant is a combination of more than two of oleic acid, dimethyl silicone oil, dodecahydroxy stearic acid and polyvinyl alcohol;

the basic grease is a lubricating grease product which meets the physical and chemical performance indexes of international standard, national standard or industrial standard.

In the technical scheme, the particle size of the metal powder is preferably 10-500 nm, and more preferably D50 is less than or equal to 100 nm.

In the above technical solution, the serpentine powder preferably contains more than 43% of MgO and SiO₂: the preferred particle size of the serpentine powder with the content of more than 43 percent is 10-500 nm, and the more preferred D50 is less than or equal to 100 nm.

In the above technical scheme, the mass percentages of the components are preferably as follows: 0.4-1% of metal powder, 0.4-1% of serpentine powder, 0.2-2% of dispersing agent and the balance of basic grease.

In the technical scheme of the invention, the related base grease can be various lubricating grease products meeting the physical and chemical performance indexes of international standard, national standard or industrial standard, such as calcium-based lubricating grease, lithium-based lubricating grease, composite aluminum-based lubricating grease, calcium sulfonate-based lubricating grease or polyurea-based lubricating grease and the like.

The invention also provides a preparation method of the wide-range multi-soap-base self-repairing lubricating grease, which comprises the following steps:

1) weighing the components according to the formula for later use;

2) dispersing agent and absolute ethyl alcohol are mixed according to the proportion of 1: mixing the materials in a mass ratio of 20-30, and performing ultrasonic dispersion to obtain a dispersion solution; adding metal powder into the dispersion solution, and performing ultrasonic dispersion to obtain a metal powder solution subjected to coating dispersion treatment;

3) adding serpentine powder into the metal powder solution subjected to coating and dispersion treatment, and performing ultrasonic dispersion and shearing dispersion to obtain a nano metal/ore composite solution;

4) removing the dispersion medium from the obtained nano metal/ore composite solution to obtain nano metal/ore composite powder;

5) mixing the obtained nano metal/ore composite powder with basic grease, homogenizing, and performing three-roller grinding for multiple times to obtain the final product.

The metal powder, serpentine powder, dispersant, base grease and the like involved in the above preparation method are selected as described above.

In the steps 2) and 3) of the preparation method, the ultrasonic dispersion is preferably carried out at 30-50 ℃, and the ultrasonic time is preferably 10-30 min.

In the step 3) of the preparation method, the shearing dispersion is preferably carried out at a rotating speed of 800-3000 rpm, and the time is preferably 30-60 min.

In the step 5) of the preparation method, the homogenization is preferably carried out at a rotating speed of 50-500 rpm, and the homogenization time is preferably 10-20 min; the rolling is usually carried out in a three-roller grinding machine, and the rolling times are usually 3-5 times.

Compared with the prior art, the invention is characterized in that:

1. on the premise of fully considering the self-performance of each additive component, the additives are reasonably selected and proportioned to effectively play the synergistic effect between the additives, so that the obtained product has excellent wear resistance and friction reduction effect, has a good self-repairing function on the surface of a friction pair, is suitable for lubricating various friction pair components and is beneficial to prolonging the service life of the friction pair components.

2. In the process, the dispersed and surface-modified nano metal/ore composite powder is directly added into the base grease, and the mixture is homogenized, ground and dispersed uniformly, so that the production process is greatly simplified, and the use cost is low; and the nano metal/ore composite powder and lubricating grease of various thickener types have very good intermiscibility, compatibility and coordination enhancement effect.

Detailed Description

The present invention will be better understood from the following detailed description of specific examples, which should not be construed as limiting the scope of the present invention.

Example 1

1) Weighing the following components in percentage by mass:

0.8% of metal powder (composed of tin powder and bismuth powder according to a mass ratio of 1: 4, wherein the particle diameters of the tin powder and the bismuth powder are D50 and 80nm), and 0.8% of serpentine powder (the content of MgO in the serpentine powder is more than 43%, and SiO in the serpentine powder is₂: the content is more than 43 percent, the particle size of the serpentine powder is D50 is 100nm), 0.4 percent, dispersant (prepared by mixing oleic acid, dimethyl silicon oil and dodecahydroxy stearic acid according to the weight ratio of 10: 1: 3) 0.4%, 98.4% of a base grease (lithium complex grease);

2) mixing a dispersing agent and absolute ethyl alcohol according to the proportion of 1: 20, ultrasonically dispersing and stirring at 30-50 ℃ for 5min, then adding metal powder, ultrasonically dispersing at 30-50 ℃ and stirring for 20min to obtain a metal powder solution coated and dispersed;

3) adding serpentine powder into the metal powder solution subjected to coating and dispersion treatment, performing ultrasonic dispersion for 20min at the temperature of 30-50 ℃, and then performing high-speed shearing dispersion for 60min at the rotating speed of 1000rpm to obtain a nano metal/ore composite solution;

4) removing absolute ethyl alcohol from the obtained nano metal/ore composite solution through vacuum filtration to obtain dry metal/ore composite powder;

5) and mixing the obtained metal/ore composite powder with basic grease, homogenizing for 10min at the rotating speed of 100rpm, and then placing the mixture into a three-roll grinder to grind for 3 times to obtain the self-repairing lubricating grease disclosed by the invention.

Example 2

1) Weighing the following components in percentage by mass:

metal powder (composed of copper powder, nickel powder and tin powder according to the mass ratio of 4: 3: 3, wherein the particle diameters of the copper powder, the nickel powder and the tin powder are D50 being 50nm) 1%, and serpentine powder (the MgO content in the serpentine powder is more than 43%, and SiO is in the serpentine powder)₂: the content is more than 43 percent, the particle diameter of the serpentine powder is D50 is 80nm) is 0.5 percent, and the dispersant (composed of dodecahydroxy stearic acid and polyvinyl alcohol according to the proportion of 1: 1) 0.5%, 98% of a base grease (polyurea grease);

2) mixing a dispersing agent and absolute ethyl alcohol according to the proportion of 1: 30, ultrasonically dispersing and stirring for 5min at the temperature of 30-40 ℃, then adding metal powder, ultrasonically dispersing and stirring for 30min at the temperature of 30-40 ℃ to obtain a metal powder solution coated and dispersed;

3) adding serpentine powder into the metal powder solution subjected to coating and dispersion treatment, performing ultrasonic dispersion for 30min at the temperature of 30-40 ℃, and then performing high-speed shearing dispersion for 60min at the rotating speed of 1000rpm to obtain a nano metal/ore composite solution;

4) removing absolute ethyl alcohol from the obtained nano metal/ore composite solution through vacuum filtration to obtain dry metal/ore composite powder;

5) and mixing the obtained metal/ore composite powder with basic grease, homogenizing for 15min at the rotating speed of 200rpm, and then placing the mixture into a three-roll grinder to grind for 5 times to obtain the self-repairing lubricating grease disclosed by the invention.

Example 3

1) Weighing the following components in percentage by mass:

0.6% of metal powder (comprising copper powder, tin powder and bismuth powder according to the mass ratio of 2: 2: 6, wherein the particle sizes of the copper powder, the tin powder and the bismuth powder are all D50 being 50nm), and 0.6% of serpentine powder (the content of MgO in the serpentine powder is more than 43%, and the content of SiO in the serpentine powder is more than 43%)₂: the content is more than 43 percent, the particle size of the serpentine powder is D50 is 100nm), 0.9 percent, dispersant (prepared by mixing oleic acid and dimethyl silicone oil according to the proportion of 1: 3) 0.5%, 98% of a base grease (polyurea grease);

2) mixing a dispersing agent and absolute ethyl alcohol according to the proportion of 1: 25, performing ultrasonic dispersion and stirring for 5min at 40 ℃, then adding metal powder, performing ultrasonic dispersion and stirring for 30min at 30 ℃ to obtain a metal powder solution coated and dispersed;

3) adding serpentine powder into the metal powder solution coated and dispersed, performing ultrasonic dispersion for 30min at 50 ℃, and then performing high-speed shearing dispersion for 60min at the rotating speed of 1000rpm to obtain a nano metal/ore composite solution;

4) removing absolute ethyl alcohol from the obtained nano metal/ore composite solution through vacuum filtration to obtain dry metal/ore composite powder;

5) and mixing the obtained metal/ore composite powder with basic grease, homogenizing for 15min at the rotating speed of 200rpm, and then placing the mixture into a three-roll grinder to grind for 5 times to obtain the self-repairing lubricating grease disclosed by the invention.

Example 4

Example 3 was repeated except that: the step 1) is carried out according to the following operations:

1) metal powder (copper powder and nickel powder in a ratio of 1: 1, the particle diameters of the copper powder and the nickel powder are respectively D50 being 30nm, 1.2 percent, and serpentine powder (the content of MgO in the serpentine powder is more than 43 percent and SiO is₂: the content is more than 43 percent, the particle size of the serpentine powder is D50 is 50nm) is 0.6 percent, and the dispersant (prepared by mixing oleic acid, dimethyl silicone oil and dodecahydroxy stearic acid according to the weight ratio of 10: 1: 3) 1% and a base grease (calcium grease) 97.2%.

Example 5

Example 3 was repeated except that: the step 1) is carried out according to the following operations:

1) 2% of metal powder (copper powder, the particle size of the copper powder is D50 is 50nm), and 2% of serpentine powder (the content of MgO in the serpentine powder is more than 43% and SiO is contained in the serpentine powder)₂: the content is more than 43 percent, the particle size of the serpentine powder is D50 is 100nm) is 1.5 percent, and the dispersant (prepared by mixing oleic acid and dodecahydroxystearic acid according to the weight ratio of 1: 5) 2% and base ester (aluminum-based composite grease) 94.5%.

The greases obtained in examples 1 to 3 of the present invention and the base greases used in examples 1 and 2 were tested for their properties, and the results are shown in table 1 below.

TABLE 1

The applicant sent the grease obtained as described in example 1 to a certain steel company in Liuzhou for testing, and the total amount of the grease was 5.53 tons (6 batches) to the steel company 4 months and 10 days before 2018, and the grease was put into production line for testing within 30 days after shipment.

The feedback report from the above iron and steel companies to the applicant after use shows:

after the self-lubricating grease (the product of the invention) is on line, the related technicians of the steel company keep track, and open the bearing cover to check the bearing in each maintenance, so that the service condition of the lubricating grease is good.

By 2 and 25 months in 2019, the use period of each batch exceeds seven and a half months, and the use effect is good. Compared with the prior lubricating grease (extreme pressure composite lithium base grease), the lubricating grease has no abnormal condition under the condition that the consumption of the lubricating grease is not increased, the service cycle exceeds seven and half months, the expected effect and the protocol requirement on trial use are achieved, the specific comparison data is shown in the following table 2, and the comprehensive judgment result is that the trial use is qualified.

Table 2: