Composite titanium-lithium mixed soap base lubricating grease and preparation method thereof

Abstract

The invention discloses composite titanium-lithium mixed soap-based lubricating grease and a preparation method thereof. The composite titanium-lithium mixed soap-based lubricating grease is prepared from the following raw materials in percentage by weight: 60-70% of base oil, 10-20% of a lubricating grease additive, 1-5% of a lubricating grease additive and 1-5% of a lubricating grease additive, 20%-30% of a thickening agent; 3%-5% of a friction increasing agent; 2%-3% of a tackifier; 1%-2% of an anti-wear reagent at extreme pressure; and 4%-5% of nano calcium carbonate. The invention also specifically discloses a preparation method of the composite titanium-lithium mixed soap-based lubricating grease. The base oil is vegetable oil and ester oil which have good biodegradability, so that the lubricating grease prepared from the base oil is a green and environment-friendly product, the pollution to the environment can be reduced to the greatest extent, and the environment is protected.

Description

Technical Field

[0001] The invention belongs to the technical field of soap-based lubricating greases, and in particular relates to a composite titanium-lithium mixed soap-based lubricating grease and a preparation method thereof. Background Art

[0002] The development of modern industry has put forward increasingly stringent requirements on the quality of grease, promoted the optimization of the structure of grease varieties in the world, and grease products are developing towards high dropping point, multi-performance and long-life varieties. Composite titanium-lithium-based grease is safe for both producers and users, and the grease prepared with vegetable oil instead of mineral oil has good biodegradability. From the perspective of performance, even without any additives, the composite titanium-lithium-based grease shows equivalent or better performance than the currently widely used composite aluminum-based grease. Adding a small amount of additives can significantly improve the performance. This grease has good compatibility with traditional high-performance greases, and is also the most promising substitute for other currently widely used high-performance greases. However, there are no relevant reports in this regard. Summary of the invention

[0003] In view of the current status quo and usage requirements, the present invention provides a composite titanium-lithium mixed soap-based grease and a preparation method thereof. The composite titanium-lithium mixed soap-based grease prepared by the method not only has excellent extreme pressure and anti-wear properties, high temperature resistance and adhesion, but also has done a lot of research on biodegradability, thereby avoiding secondary pollution to the environment during use as much as possible.

[0004] The present invention adopts the following technical solution to solve the above technical problems: a composite titanium-lithium mixed soap-based grease, characterized in that it is prepared from the following raw materials in weight percentage: Base oil 60%~70%; Thickener 20%~30%; Friction enhancer 3%~5%; Thickener 2%~3%; Extreme pressure anti-wear agent 1%~2%; Nano calcium carbonate 4%~5%.

[0005] Furthermore, the base oil is a mixture of vegetable oil and ester oil in a mass ratio of 1:3; wherein the vegetable oil is one or more of rapeseed oil, castor oil, palm oil, soybean oil or peanut oil; and the ester oil is one or more of dioctyl sebacate, dioctyl adipate or dioctyl phthalate.

[0006] Furthermore, the thickener is one or more of a fatty acid, a dibasic acid, a lithium hydroxide aqueous solution or an alkoxytitanium; wherein the fatty acid is one or more of stearic acid, dodecyl stearic acid or oleic acid; the dibasic acid is C 3~11The low molecular weight acid is specifically boric acid, azelaic acid, sebacic acid or benzoic acid; the mass ratio of lithium hydroxide to water in the lithium hydroxide aqueous solution is 1:3-6.

[0007] Furthermore, the thickener is a mixture of fatty acid, dibasic acid, lithium hydroxide aqueous solution and alkoxy titanium, and the weight percentage of each component in the grease is: Fatty acids 8%~12%; Dibasic acid 3%~5%; Lithium hydroxide aqueous solution 5%~7%; Titanium alkoxide 4%~6%; The fatty acid is one or more of stearic acid, dodecyl stearic acid or oleic acid; the dibasic acid is C 3~11 The low molecular weight acid is specifically boric acid, azelaic acid, sebacic acid or benzoic acid; the mass ratio of lithium hydroxide to water in the lithium hydroxide aqueous solution is 1:3-6.

[0008] Furthermore, the friction enhancer is one or more of 212 phenolic resin, tert-butyl phenolic resin or 871 resin.

[0009] Furthermore, the tackifier is one or more of polyisobutylene, natural rubber or polymethacrylate.

[0010] Furthermore, the extreme pressure anti-wear agent is one or more of sulfided isobutylene, borate or antimony dithiocarbamate.

[0011] The preparation method of the composite titanium-lithium mixed soap-based grease of the present invention is characterized by the following specific steps: (1) Add 1 / 2~2 / 3 of the base oil into the reactor, then add fatty acid and dibasic acid, stir and heat; (2) Raise the temperature to 80°C~95°C, add lithium hydroxide aqueous solution and alkoxy titanium respectively, and stir to mix evenly; (3) Raise the temperature to 95°C~110°C and saponify at constant temperature for 1~2 hours; (4) Raise the temperature to 130°C~150°C, add the friction enhancer, and stir at constant temperature for 15~30 minutes; (5) Raise the temperature to 180°C~210°C, keep the temperature constant for 10~30 minutes, then add the remaining base oil and cool down; (6) Cool down to 60°C~120°C, then add nano calcium carbonate, thickener and extreme pressure anti-wear agent respectively, stir evenly, degas, homogenize and extract the grease to obtain composite titanium-lithium mixed soap-based grease.

[0012] Compared with similar products, the technical solution of the present invention has the following advantages and beneficial effects: 1. The base oils used in the present invention are vegetable oils and ester oils, both of which have good biodegradability. The grease prepared therefrom is a green and environmentally friendly product that can minimize environmental pollution and protect the environment.

[0013] 2. The composite titanium-lithium mixed soap-based grease prepared by the present invention is a multifunctional and multi-effect grease. It is not only environmentally friendly, but also has good compatibility with traditional greases. The combination with lithium-based grease in this solution plays a complementary role, making its performance more excellent.

[0014] 3. The friction enhancer and extreme pressure anti-wear agent in the present invention play a great role in improving the extreme pressure and anti-wear properties of the product, and nano calcium carbonate, as a grease additive, can also play an anti-wear effect by improving the grease structure.

[0015] 4. The tackifier in the present invention has a good effect on improving the adhesion and high temperature resistance of the grease. DETAILED DESCRIPTION

[0016] The specific technical solutions of the present invention are described in detail in conjunction with specific embodiments. Example

[0017] In this embodiment, the base oil is 650 grams of a mixture of rapeseed oil and dioctyl sebacate (mass ratio 1:3), the fatty acid is 90 grams of dodecyl stearic acid, the lithium hydroxide aqueous solution (mass ratio of lithium hydroxide to water is 1:4) is 60 grams, the dibasic acid is 40 grams of boric acid, the alkoxy titanium is 50 grams of tetraisopropoxide titanate, the friction enhancer is 30 grams of 212 phenolic resin, the extreme pressure and anti-wear agent is 15 grams of sulfided isobutylene, the tackifier is 25 grams of polyisobutylene, and the nano calcium carbonate is 40 grams.

[0018] The specific preparation process is: (1) Add 400 g of base oil into a reactor, add 90 g of dodecyl stearic acid and 40 g of boric acid, and stir to raise the temperature.

[0019] (2) Raise the temperature to 90°C, add 60 g of lithium hydroxide aqueous solution and 50 g of tetraisopropyl titanate, and stir evenly.

[0020] (3) Raise the temperature to 105°C and saponify at this temperature for 1.5 hours.

[0021] (4) Raise the temperature to 135°C, add 30 g of 212 phenolic resin, and stir at constant temperature for 15 minutes.

[0022] (5) Raise the temperature to 200°C, keep the temperature constant for 10 minutes, add 250 g of base oil, and cool down.

[0023] (6) Cool down to 80°C, add 15 g of sulfided isobutylene, 25 g of polyisobutylene, and 40 g of nano calcium carbonate in sequence, stir evenly, degas, homogenize, and remove from the kettle to obtain grease. Example

[0024] In this embodiment, the base oil is 650 grams of a mixture of rapeseed oil and dioctyl oxalate (mass ratio 1:3), the fatty acid is 90 grams of dodecyl stearic acid, the lithium hydroxide aqueous solution (mass ratio of lithium hydroxide to water is 1:4) is 60 grams, the dibasic acid is 40 grams of boric acid, the alkoxy titanium is 50 grams of tetraisopropanol titanate, the friction enhancer is 30 grams of 212 phenolic resin, the extreme pressure and anti-wear agent is 15 grams of sulfided isobutylene, the tackifier is 25 grams of polyisobutylene, and the nano calcium carbonate is 40 grams.

[0025] The specific preparation process is: (1) Add 350 g of base oil into a reactor, add 90 g of dodecyl stearic acid and 40 g of sebacic acid, stir and heat.

[0026] (2) Raise the temperature to 90°C, add 60 g of lithium hydroxide aqueous solution and 50 g of tetraisopropyl titanate, and stir evenly.

[0027] (3) Raise the temperature to 105°C and saponify at this temperature for 1.5 hours.

[0028] (4) Raise the temperature to 145°C, add 30 g of 212 phenolic resin, and stir at constant temperature for 15 minutes.

[0029] (5) Raise the temperature to 200°C, keep the temperature constant for 10 minutes, add 300 g of base oil, and cool down.

[0030] (6) Cool down to 80°C, add 15 g of sulfided isobutylene, 25 g of polyisobutylene, and 40 g of nano calcium carbonate in sequence, stir evenly, degas, homogenize, and remove from the kettle to obtain grease. Example

[0031] In this embodiment, the base oil is 650 grams of a mixture of soybean oil and dioctyl sebacate (1:3), the fatty acid is 90 grams of dodecyl stearic acid, the lithium hydroxide aqueous solution (the mass ratio of lithium hydroxide to water is 1:4) is 60 grams, the dibasic acid is 40 grams of boric acid, the alkoxy titanium is 50 grams of tetraisopropoxide titanate, the friction enhancer is 30 grams of 212 phenolic resin, the extreme pressure and anti-wear agent is 15 grams of sulfided isobutylene, the tackifier is 25 grams of polyisobutylene, and the nano calcium carbonate is 40 grams.

[0032] The specific preparation process is: (1) Pour 400 g of base oil into a reactor, add 90 g of dodecyl stearic acid and 40 g of boric acid, and stir to raise the temperature.

[0033] (2) Raise the temperature to 90°C, add 60 g of lithium hydroxide aqueous solution and 50 g of tetraisopropyl titanate, and stir evenly.

[0034] (3) Raise the temperature to 105°C and saponify at this temperature for 1 hour.

[0035] (4) Raise the temperature to 130°C, add 30 g of 212 phenolic resin, and stir at constant temperature for 15 minutes.

[0036] (5) Raise the temperature to 200°C, keep the temperature constant for 10 minutes, add 250 g of base oil, and cool down.

[0037] (6) Cool down to 80°C, add 15 g of sulfided isobutylene, 25 g of polyisobutylene and 40 g of nano calcium carbonate in sequence, stir evenly, degas, homogenize and remove from the kettle to obtain grease. Example

[0038] In this embodiment, the base oil is 650 grams of a mixture of castor oil and dioctyl sebacate (mass ratio 1:3), the fatty acid is 90 grams of stearic acid, the lithium hydroxide aqueous solution (mass ratio of lithium hydroxide to water is 1:4) is 60 grams, the dibasic acid is 40 grams of benzoic acid, the alkoxy titanium is 50 grams of tetraisopropoxide titanate, the friction enhancer is 30 grams of 212 phenolic resin, the extreme pressure and anti-wear agent is 15 grams of sulfided isobutylene, the tackifier is 25 grams of polyisobutylene, and the nano calcium carbonate is 40 grams.

[0039] The specific preparation process is: (1) Pour 380 g of base oil into a reactor, add 90 g of stearic acid and 40 g of benzoic acid, stir and heat.

[0040] (2) Raise the temperature to 90°C, add 60 g of lithium hydroxide aqueous solution and 50 g of tetraisopropyl titanate, and stir evenly.

[0041] (3) Raise the temperature to 105°C and saponify at this temperature for 1 hour.

[0042] (4) Raise the temperature to 135°C, add 30 g of 212 phenolic resin, and stir at constant temperature for 15 minutes.

[0043] (5) Raise the temperature to 200°C, keep the temperature constant for 10 minutes, add 270 g of base oil, and cool down.

[0044] (6) Cool down to 85°C, add 15 g of sulfided isobutylene, 25 g of polyisobutylene and 40 g of nano calcium carbonate in sequence, stir evenly, degas, homogenize and remove from the kettle to obtain grease.

[0045] After testing, the indicators of the grease obtained in Examples 1 to 4 are shown in the following table: Dropping point / ℃ PB value / N Wear scar diameter / mm Adhesion rate / % Embodiment 1 271 686 0.33 26.3 Embodiment 2 269 686 0.31 25.7 Embodiment 3 274 686 0.36 24.8 Embodiment 4 270 686 0.34 25.9 The basic principles, main features and advantages of the present invention are shown and described above. Without departing from the spirit and scope of the present invention, the present invention may also be subject to various changes and improvements, which all fall within the scope of the present invention to be protected.

Claims

1. A composite titanium-lithium mixed soap-based grease, characterized in that It is prepared from the following raw materials in percentage by weight: Base oil 60%~70%; Thickener 20%~30%; Friction enhancer 3%~5%; Thickener 2%~3%; Extreme pressure anti-wear agent 1%~2%; Nano calcium carbonate 4%~5%.

2. The composite titanium-lithium mixed soap-based grease according to claim 1, characterized in that: The base oil is a mixture of vegetable oil and ester oil in a mass ratio of 1:3; the vegetable oil is one or more of rapeseed oil, castor oil, palm oil, soybean oil or peanut oil; the ester oil is one or more of dioctyl sebacate, dioctyl adipate or dioctyl phthalate.

3. The composite titanium-lithium mixed soap-based grease according to claim 1, characterized in that: The thickener is one or more of fatty acid, dibasic acid, lithium hydroxide aqueous solution or alkoxy titanium; wherein the fatty acid is one or more of stearic acid, dodecyl stearic acid or oleic acid; the dibasic acid is C 3~11 The low molecular weight acid is specifically boric acid, azelaic acid, sebacic acid or benzoic acid; the mass ratio of lithium hydroxide to water in the lithium hydroxide aqueous solution is 1:3-6.

4. The composite titanium-lithium mixed soap-based grease according to claim 1, characterized in that: The thickener is a mixture of fatty acid, dibasic acid, lithium hydroxide aqueous solution and alkoxy titanium, and the weight percentage of each component in the grease is: Fatty acids 8%~12%; Dibasic acid 3%~5%; Lithium hydroxide aqueous solution 5%~7%; Titanium alkoxide 4%~6%; The fatty acid is one or more of stearic acid, dodecyl stearic acid or oleic acid; the dibasic acid is C 3~11 The low molecular weight acid is specifically boric acid, azelaic acid, sebacic acid or benzoic acid; the mass ratio of lithium hydroxide to water in the lithium hydroxide aqueous solution is 1:3-6.

5. The composite titanium-lithium mixed soap-based grease according to claim 1, characterized in that: The friction enhancer is one or more of 212 phenolic resin, tert-butyl phenolic resin or 871 resin.

6. The composite titanium-lithium mixed soap-based grease according to claim 1, characterized in that: The tackifier is one or more of polyisobutylene, natural rubber or polymethacrylate.

7. The composite titanium-lithium mixed soap-based grease according to claim 1, characterized in that: The extreme pressure anti-wear agent is one or more of sulfided isobutylene, borate or antimony dithiocarbamate.

8. A method for preparing the composite titanium-lithium mixed soap-based grease according to claim 1, characterized in that The specific steps are: (1) Add 1 / 2~2 / 3 of the base oil into the reactor, then add fatty acid and dibasic acid, stir and heat; (2) Raise the temperature to 80°C~95°C, add lithium hydroxide aqueous solution and alkoxy titanium respectively, and stir to mix evenly; (3) Raise the temperature to 95°C~110°C and saponify at constant temperature for 1~2 hours; (4) Raise the temperature to 130°C~150°C, add the friction enhancer, and stir at constant temperature for 15~30 minutes; (5) Raise the temperature to 180°C~210°C, keep the temperature constant for 10~30 minutes, then add the remaining base oil and cool down; (6) Cool down to 60°C~120°C, then add nano calcium carbonate, thickener and extreme pressure anti-wear agent respectively, stir evenly, degas, homogenize and extract the grease to obtain composite titanium-lithium mixed soap-based grease.