阅读说明：本技术 一种提高高碱值磺酸钙基润滑脂细度的方法 (Method for improving fineness of high-base-number calcium sulfonate-based lubricating grease ) 是由 俞珍权 于 2021-08-31 设计创作，主要内容包括：本发明提供了一种提高高碱值磺酸钙基润滑脂细度的方法,其特征在于,该方法包括以下步骤：1)先将碱值为400～500mgKOH/g的高碱值磺酸钙、润滑脂基础油、转向促进剂、冰醋酸以及水混合后快速搅拌,升温到60-100℃保持反应30-90min,然后进行第一次超声处理；2)向上述反应体系中加入硼酸、氢氧化钙、脂肪酸混合均匀并于在150～200℃下反应1～3h；3)继续升温至250℃进行高温炼制10～20min,得到高碱值磺酸钙基皂油；4)将高碱值磺酸钙皂油降温剪切,加入添加剂和表面活性剂,继续在300r/min下剪切1～2h后进行第二次超声处理,处理完毕后将物料转移到脱气釜内在真空度为0.1～0.2MPa下脱气,即得到高碱值磺酸钙基润滑脂。本发明的方法能够有效提高高碱值磺酸钙润滑脂细度。(The invention provides a method for improving the fineness of high-base-number calcium sulfonate-based lubricating grease, which is characterized by comprising the following steps of: 1) firstly, mixing high-base-number calcium sulfonate with a base number of 400-500 mgKOH/g, lubricating grease base oil, a steering promoter, glacial acetic acid and water, quickly stirring, heating to 60-100 ℃, keeping reacting for 30-90min, and then carrying out first ultrasonic treatment; 2) adding boric acid, calcium hydroxide and fatty acid into the reaction system, uniformly mixing, and reacting for 1-3 h at 150-200 ℃; 3) continuously heating to 250 ℃ for refining at high temperature for 10-20 min to obtain high-base-number calcium sulfonate-based soap oil; 4) and cooling and shearing the high-base-number calcium sulfonate soap oil, adding an additive and a surfactant, continuously shearing for 1-2 hours at 300r/min, carrying out secondary ultrasonic treatment, transferring the material to a degassing kettle after the treatment is finished, and degassing under the vacuum degree of 0.1-0.2 MPa to obtain the high-base-number calcium sulfonate base lubricating grease. The method can effectively improve the fineness of the high-base-number calcium sulfonate lubricating grease.)

1. A method for improving the fineness of high-base-number calcium sulfonate-based lubricating grease is characterized by comprising the following steps of:

1) firstly, mixing high-base-number calcium sulfonate with a base number of 400-500 mgKOH/g, lubricating grease base oil, a steering promoter, glacial acetic acid and water, quickly stirring, heating to 60-100 ℃, keeping reacting for 30-90min, and then carrying out first ultrasonic treatment;

2) adding boric acid, calcium hydroxide and fatty acid into the reaction system, uniformly mixing, and reacting for 1-3 h at 150-200 ℃;

3) continuously heating to 250 ℃ for refining at high temperature for 10-20 min to obtain high-base-number calcium sulfonate-based soap oil;

4) and cooling and shearing the high-base-number calcium sulfonate soap oil, adding an additive and a surfactant, continuously shearing for 1-2 hours at 300r/min, carrying out secondary ultrasonic treatment, transferring the material to a degassing kettle after the treatment is finished, and degassing under the vacuum degree of 0.1-0.2 MPa to obtain the high-base-number calcium sulfonate base lubricating grease.

2. The method for improving the fineness of the high base number calcium sulfonate-based grease in claim 1, wherein the grease base oil in step 1) is one of a naphthenic base-reduced second-wire base oil and a naphthenic base-reduced third-wire base oilAt least one of; the kinematic viscosity of the lubricating grease base oil at 100 ℃ is 5-15 mm²/s。

3. The method for improving the fineness of the high base number calcium sulfonate-based grease of claim 1, wherein the diversion accelerator in step 1) is selected from at least one of calcium carbonate, dodecylbenzene sulfonic acid, carbon dioxide, isopropanol, and ethanol.

4. The method for improving the fineness of the high-base-number calcium sulfonate-based lubricating grease as claimed in claim 1, wherein the mass ratio of the high-base-number calcium sulfonate, the lubricating grease base oil, the steering accelerator, the glacial acetic acid and the water in the step 1) is (20-40): (20-40): (10-15): (1-3): (2-5).

5. The method for improving the fineness of the high base number calcium sulfonate-based grease lubricant according to claim 1, wherein the first ultrasonic treatment condition in step 1) is as follows: the frequency is 80-120 KHz, and the time is 40-60 min.

6. The method for improving the fineness of the high-base-number calcium sulfonate-based lubricating grease according to claim 1, wherein the mass ratio of the boric acid to the calcium hydroxide to the fatty acid in the step 2) is (1-3): (5-10): (6-10).

7. The method for improving the fineness of the high-base-number calcium sulfonate-based lubricating grease according to claim 1, wherein the mass ratio of the additive to the surfactant in the step 3) is (1-3): (1-2).

8. The method for improving the fineness of the high base number calcium sulfonate-based grease of claim 1, wherein the additive in step 3) is an antioxidant, and the antioxidant is one of T551 or T561.

9. The method for improving the fineness of the high base number calcium sulfonate-based grease according to claim 1, wherein the surfactant in step 3) is a phthalate-based Gemini surfactant.

10. The method for improving the fineness of the high base number calcium sulfonate-based grease lubricant according to claim 1, wherein the second ultrasonic treatment condition in the step 3) is as follows: the frequency is 60-80 KHz, and the time is 20-40 min.

Technical Field

The invention belongs to the technical field of lubricants, and particularly relates to a method for improving the fineness of high-base-number calcium sulfonate-based lubricating grease.

Background

Calcium sulfonate is commonly used as a cleaning agent and an antirust agent of lubricating oil, calcium sulfonate-based lubricating grease with high dropping point using calcium sulfonate as a thickening agent appears in the 50 s of the 20 th century, but the oil-soluble Newtonian body calcium sulfonate solution used at the time has small thickening capability and can only be used together with a traditional fatty acid soap thickening agent in a small proportion. In the 60 s, people convert a Newtonian calcium sulfonate solution into non-Newtonian calcium sulfonate with thixotropy, and a high-alkalization technology of calcium sulfonate is introduced in the preparation process of calcium sulfonate-based lubricating grease to prepare high-alkalinity calcium sulfonate-based grease, the dropping point of the high-alkalinity calcium sulfonate-based grease is more than 300 ℃, the stability of a roller is 12 units, the high-alkalinity calcium sulfonate-based grease has good shear stability, but the high-alkalinity calcium sulfonate-based grease is quite viscous, the low-temperature pumping performance is poor, and the further application of the high-alkalinity calcium sulfonate-based grease is prevented. In the middle of the 80 s, the non-Newtonian calcium sulfonate soap and other fatty acid salts are compounded to prepare the composite calcium sulfonate-based lubricating grease, so that the low-temperature pumping performance of the composite calcium sulfonate-based lubricating grease is improved, and the composite calcium sulfonate-based lubricating grease has excellent high-low temperature performance, mechanical stability, colloid stability and oxidation stability and is called as new-generation efficient lubricating grease.

The high-base-number calcium sulfonate-based lubricating grease has excellent extreme pressure, wear resistance, water resistance, salt spray resistance, corrosion resistance, high dropping point, good thermal stability at high temperature and the like, and is widely applied to high-temperature, heavy-load and watery environments such as automobiles, steel, mines, paper making and the like.

Generally, the smaller the fineness of the high base number calcium sulfonate grease, the more excellent the performance. Although the particle size of the amorphous calcium sulfonate is small, the particle size of the amorphous calcium sulfonate is increased after the amorphous calcium sulfonate is converted into calcite-shaped calcium sulfonate through a related process, and the performance of the grease is further reduced.

Based on the above, a method capable of improving the fineness of the high base number calcium sulfonate grease has been desired. The performance of the existing lubricating grease can be effectively improved.

Disclosure of Invention

The invention aims to solve the technical problem of providing a method for improving the fineness of high base number calcium sulfonate lubricating grease aiming at the defects of the prior art. The method can effectively improve the fineness of the high-base-number calcium sulfonate lubricating grease.

The purpose of the invention and the technical problem to be solved are realized by adopting the following technical scheme.

The invention provides a method for improving the fineness of high-base-number calcium sulfonate-based lubricating grease, which comprises the following steps of:

1) firstly, mixing high-base-number calcium sulfonate with a base number of 400-500 mgKOH/g, lubricating grease base oil, a steering promoter, glacial acetic acid and water, quickly stirring, heating to 60-100 ℃, keeping reacting for 30-90min, and then carrying out first ultrasonic treatment;

2) adding boric acid, calcium hydroxide and fatty acid into the reaction system, uniformly mixing, and reacting for 1-3 h at 150-200 ℃;

3) continuously heating to 250 ℃ for refining at high temperature for 10-20 min to obtain high-base-number calcium sulfonate-based soap oil;

4) and cooling and shearing the high-base-number calcium sulfonate soap oil, adding an additive and a surfactant, continuously shearing for 1-2 hours at 300r/min, carrying out secondary ultrasonic treatment, transferring the material to a degassing kettle after the treatment is finished, and degassing under the vacuum degree of 0.1-0.2 MPa to obtain the high-base-number calcium sulfonate base lubricating grease.

Preferably, the grease base oil in step 1) is at least one of a naphthenic minus third-line base oil and a naphthenic minus third-line base oil; the kinematic viscosity of the lubricating grease base oil at 100 ℃ is 5-15 mm²/s。

Preferably, the diversion accelerator in step 1) is selected from at least one of calcium carbonate, dodecylbenzene sulfonic acid, carbon dioxide, isopropanol and ethanol.

Preferably, the mass ratio of the high-base-number calcium sulfonate, the lubricating grease base oil, the steering accelerator, the glacial acetic acid and the water in the step 1) is (20-40): (20-40): (10-15): (1-3): (2-5).

Preferably, the first sonication conditions in step 1) are: the frequency is 80-120 KHz, and the time is 40-60 min.

Preferably, the mass ratio of the boric acid, the calcium hydroxide and the fatty acid in the step 2) is (1-3): (5-10): (6-10).

Preferably, the mass ratio of the additive to the surfactant in the step 3) is (1-3): (1-2).

Preferably, the additive in step 3) is an antioxidant, and the antioxidant is one of T551 or T561.

Preferably, the surfactant in step 3) is a phthalate-based Gemini surfactant.

Preferably, the second ultrasonic treatment conditions in step 3) are: the frequency is 60-80 KHz, and the time is 20-40 min

The invention has the following beneficial effects: on the basis of the existing method for preparing the high-base-number calcium sulfonate-based lubricating grease, the fineness of the lubricating grease can be effectively improved by adding a small amount of surfactant phthalate Gemini surfactant and performing ultrasonic action twice. The addition of the phthalate Gemini surfactant can improve the lubrication degree of the lubricating grease, and through two times of ultrasonic treatment, the reaction can be promoted under the action of ultrasonic waves, so that the fineness of the lubricating grease is improved.

Detailed Description

The technical solutions in the embodiments of the present invention will be described in detail below with reference to the embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. 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 following raw materials are each 100 parts by weight.

1) Firstly, 30 parts of high-base-number calcium sulfonate with a base number of 400-500 mgKOH/g and naphthenic base minus second-thread base oil (the kinematic viscosity at 100 ℃ is 5-15 mm)²/s)30 parts of the raw materials, 14 parts of dodecylbenzene sulfonic acid, 2 parts of glacial acetic acid and 4 parts of water are mixed and then rapidly stirred, the temperature is increased to 80 ℃, the reaction is kept for 60min, and then the first ultrasonic treatment is carried out, wherein the ultrasonic frequency is 100KHz, and the time is 50 min;

2) adding 2 parts of boric acid, 7 parts of calcium hydroxide and 8 parts of fatty acid into the reaction system, uniformly mixing, and reacting at 150 ℃ for 3 hours;

3) continuously heating to 250 ℃ for refining for 15min at high temperature to obtain high-base-number calcium sulfonate-based soap oil;

4) cooling and shearing the high-base-number calcium sulfonate soap oil, adding 5512 parts of antioxidant T and 1 part of phthalate Gemini surfactant, continuously shearing at 300r/min for 1h, then carrying out secondary ultrasonic treatment, wherein the ultrasonic frequency is 70KHz, the ultrasonic time is 30min, transferring the material to a degassing kettle after the treatment, and degassing at the vacuum degree of 0.1-0.2 MPa to obtain the high-base-number calcium sulfonate base lubricating grease. Through measurement, the fineness of the high-base-number calcium sulfonate-based lubricating grease is 350-400 nm.

Example 2

The following raw materials are each 100 parts by weight.

1) Firstly 20 parts of high base number calcium sulfonate with a base number of 400-500 mgKOH/g and naphthenic base triple-reduced base oil (the kinematic viscosity at 100 ℃ is 5-15 mm)²/s)40 parts, 10 parts of isopropanol, 3 parts of glacial acetic acid and 5 parts of water are mixed and then rapidly stirred, the temperature is increased to 80 ℃, the reaction is kept for 60min, and then the first ultrasonic treatment is carried out, wherein the ultrasonic frequency is 100KHz, and the time is 50 min;

2) adding 2 parts of boric acid, 7 parts of calcium hydroxide and 8 parts of fatty acid into the reaction system, uniformly mixing, and reacting at 150 ℃ for 3 hours;

3) continuously heating to 250 ℃ for refining for 15min at high temperature to obtain high-base-number calcium sulfonate-based soap oil;

4) cooling and shearing the high-base-number calcium sulfonate soap oil, adding 5513 parts of antioxidant T and 2 parts of phthalate Gemini surfactant, continuously shearing at 300r/min for 2 hours, then carrying out secondary ultrasonic treatment, wherein the ultrasonic frequency is 70KHz, the ultrasonic time is 30min, transferring the material to a degassing kettle after the treatment, and degassing at the vacuum degree of 0.1-0.2 MPa to obtain the high-base-number calcium sulfonate base lubricating grease. Through measurement, the fineness of the high-base-number calcium sulfonate-based lubricating grease is 300-350 nm.

Example 3

The following raw materials are each 100 parts by weight.

1) Firstly, 40 parts of high base number calcium sulfonate with a base number of 400-500 mgKOH/g and naphthenic base minus second-thread base oil (the kinematic viscosity at 100 ℃ is 5-15 mm)²/s)20 parts of the raw materials, 15 parts of carbon dioxide, 2 parts of glacial acetic acid and 3 parts of water are mixed and then rapidly stirred, the temperature is increased to 80 ℃, the reaction is kept for 60min, and then the first ultrasonic treatment is carried out, wherein the ultrasonic frequency is 100KHz, and the time is 50 min;

2) adding 2 parts of boric acid, 5 parts of calcium hydroxide and 8 parts of fatty acid into the reaction system, uniformly mixing, and reacting at 150 ℃ for 3 hours;

3) continuously heating to 250 ℃ for refining for 15min at high temperature to obtain high-base-number calcium sulfonate-based soap oil;

4) cooling and shearing the high-base-number calcium sulfonate soap oil, adding 5513 parts of antioxidant T and 2 parts of phthalate Gemini surfactant, continuously shearing at 300r/min for 2 hours, then carrying out secondary ultrasonic treatment, wherein the ultrasonic frequency is 70KHz, the ultrasonic time is 30min, transferring the material to a degassing kettle after the treatment, and degassing at the vacuum degree of 0.1-0.2 MPa to obtain the high-base-number calcium sulfonate base lubricating grease. Through measurement, the fineness of the high-base-number calcium sulfonate-based lubricating grease is 250-300 nm.

Example 4

The following raw materials are each 100 parts by weight.

1) Firstly, 30 parts of high base number calcium sulfonate with a base number of 400-500 mgKOH/g and naphthenic base triple-reduction base oil (the kinematic viscosity at 100 ℃ is 5-15 mm)²/s)30 parts of the raw materials, 14 parts of dodecylbenzene sulfonic acid, 2 parts of glacial acetic acid and 4 parts of water are mixed and then rapidly stirred, the temperature is increased to 100 ℃, the reaction is kept for 30min, and then the first ultrasonic treatment is carried out, wherein the ultrasonic frequency is 120KHz, and the time is 40 min;

2) adding 2 parts of boric acid, 7 parts of calcium hydroxide and 8 parts of fatty acid into the reaction system, uniformly mixing, and reacting at 200 ℃ for 1 h;

3) continuously heating to 250 ℃ for refining at high temperature for 10min to obtain high-base-number calcium sulfonate-based soap oil;

4) cooling and shearing the high-base-number calcium sulfonate soap oil, adding an antioxidant T5612 and 1 part of phthalate Gemini surfactant, continuously shearing at 300r/min for 1h, then carrying out secondary ultrasonic treatment, wherein the ultrasonic frequency is 60KHz, the ultrasonic time is 40min, transferring the material to a degassing kettle after the treatment, and degassing at the vacuum degree of 0.1-0.2 MPa to obtain the high-base-number calcium sulfonate base lubricating grease. Through measurement, the fineness of the high-base-number calcium sulfonate-based lubricating grease is 300-400 nm.

Example 5

The following raw materials are each 100 parts by weight.

1) Firstly, the high base number calcium sulfonate with the base number of 400-500 mgKOH/g20 parts of naphthenic base minus two-wire base oil (the kinematic viscosity at 100 ℃ is 5-15 mm)²/s)40 parts, 10 parts of calcium carbonate, 3 parts of glacial acetic acid and 5 parts of water are mixed and then rapidly stirred, the temperature is increased to 60 ℃, the reaction is kept for 90min, and then the first ultrasonic treatment is carried out, wherein the ultrasonic frequency is 80KHz, and the time is 60 min;

2) adding 2 parts of boric acid, 7 parts of calcium hydroxide and 8 parts of fatty acid into the reaction system, uniformly mixing, and reacting at 150 ℃ for 3 hours;

3) continuously heating to 250 ℃ for refining at high temperature for 20min to obtain high-base-number calcium sulfonate-based soap oil;

4) cooling and shearing the high-base-number calcium sulfonate soap oil, adding an antioxidant T5613 and 2 parts of phthalate Gemini surfactant, continuously shearing at 300r/min for 2 hours, then carrying out secondary ultrasonic treatment, wherein the ultrasonic frequency is 80KHz, the ultrasonic time is 30min, transferring the material to a degassing kettle after the treatment, and degassing at the vacuum degree of 0.1-0.2 MPa to obtain the high-base-number calcium sulfonate base lubricating grease. Through measurement, the fineness of the high-base-number calcium sulfonate-based lubricating grease is 200-300 nm.

Example 6

The following raw materials are each 100 parts by weight.

1) Firstly, 40 parts of high base number calcium sulfonate with a base number of 400-500 mgKOH/g and naphthenic base triple-reduction base oil (the kinematic viscosity at 100 ℃ is 5-15 mm)²/s)20 parts, 15 parts of calcium carbonate, 2 parts of glacial acetic acid and 3 parts of water are mixed and then rapidly stirred, the temperature is increased to 80 ℃, the reaction is kept for 70min, and then the first ultrasonic treatment is carried out, wherein the ultrasonic frequency is 100KHz, and the time is 60 min;

2) adding 2 parts of boric acid, 5 parts of calcium hydroxide and 8 parts of fatty acid into the reaction system, uniformly mixing, and reacting at 150 ℃ for 1 h;

3) continuously heating to 250 ℃ for refining for 15min at high temperature to obtain high-base-number calcium sulfonate-based soap oil;

4) cooling and shearing the high-base-number calcium sulfonate soap oil, adding an antioxidant T5613 and 2 parts of phthalate Gemini surfactant, continuously shearing at 300r/min for 2 hours, then carrying out secondary ultrasonic treatment, wherein the ultrasonic frequency is 70KHz, the ultrasonic time is 40min, transferring the material to a degassing kettle after the treatment, and degassing at the vacuum degree of 0.1-0.2 MPa to obtain the high-base-number calcium sulfonate base lubricating grease. Through measurement, the fineness of the high-base-number calcium sulfonate-based lubricating grease is 250-300 nm.

It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.