Preparation method of polymerized grease

Abstract

The invention relates to a preparation method of polymerized grease, which is characterized in that methane sulfonic acid and / or perchloric acid are / is used as a catalyst, vegetable oil is used as a raw material, the vegetable oil and the catalyst are stirred and mixed, the temperature is controlled at 100-160 DEG C, and the reaction is performed for 120-300 minutes; adding water for washing to remove the catalyst, cooling to 50 DEG C, and pouring out the reaction product to obtain the reaction product, namely the polymerized grease, which can be used for the bio-based lubricating grease.

Description

Technical Field

[0001] The invention belongs to the field of fine chemicals and relates to a method for preparing polymerized grease, and the international patent classification belongs to C10M. Background Art

[0002] Vegetable oil is a renewable energy source, especially soybean oil, which is a cheap and common agricultural renewable resource. In particular, genetically modified soybeans have a high oil content. Their molecular structure contains three ester groups, multiple double bonds and long alkyl chains. This unique molecular structure with a high degree of unsaturation can be fully utilized.

[0003] In the research of polymerized oils, continuous innovation is needed to find methods for synthesizing biodegradable polymerized oils with different degrees of polymerization.

[0004] The present invention provides a method for preparing polymerized oils, that is, a method for synthesizing plant oil-based polymerized oils. The use and synthesis method of such oil esters have not been reported yet. Summary of the invention

[0005] 1. A method for preparing polymerized oil, characterized in that vegetable oil is used as raw material to carry out polymerization reaction to obtain polymerized oils of different molecular weights, and the preparation method comprises the following steps:

[0006] (1) Add vegetable oil to a reactor equipped with a stirrer, add a catalyst while stirring, and inject the catalyst below the liquid level;

[0007] (2) Setting the heating temperature to 90°C, and then heating at a heating rate of 5°C;

[0008] (3) stirring and heating to 100-160° C., and maintaining the reaction for 120-300 min;

[0009] (4) Lower the temperature to 50°C;

[0010] (5) Add hot water to the polymerized oil and stir for 10-30 minutes, then stop stirring and allow to settle to separate the water, and repeat this process three times;

[0011] (6) The washed oil is vacuum dried at 100°C to remove residual water to obtain polymerized oil.

[0012] 2. The method according to 1, characterized in that the catalyst is methanesulfonic acid.

[0013] 3. The method according to 1, characterized in that the catalyst is perchloric acid.

[0014] 4. The method according to 1 and 2, characterized in that the amount of catalyst used is 5%-10% of the total amount (weight) of the raw materials.

[0015] 5. The method according to 1 and 3, characterized in that the amount of catalyst used is 0.5%-2% of the total amount (weight) of the raw materials.

[0016] In the method, the catalyst used is methanesulfonic acid or perchloric acid. When methanesulfonic acid is used, the catalyst amount is 5-10% of the total weight of soybean oil, and when perchloric acid is used, the catalyst amount is 0.5-2% of the total weight of soybean oil.

[0017] The reaction temperature of the process is 100-160°C. When using methanesulfonic acid as a catalyst, the reaction temperature is 130-160°C, optimally 150-160°C, and the maximum reaction temperature does not exceed 160°C and is not lower than 130°C. When using perchloric acid as a catalyst, the reaction temperature is 100-150°C, optimally 120-130°C, and the maximum reaction temperature does not exceed 150°C.

[0018] Effects of the Invention

[0019] Polymerized grease has a wide range of uses. We can control the molecular weight of polymerized grease according to different reaction temperatures, reaction times, and catalyst dosages to obtain the desired product. Polymerized grease has a high kinematic viscosity and viscosity index and has a wide range of application value. It can be used in lubricating oils and greases.

[0020] The preparation of polymerized oils and fats according to the above method has a yield of more than 95%, and can be produced intermittently or continuously. DETAILED DESCRIPTION

[0021] The following is a detailed description of the embodiments of the present invention: This embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation method and process are given, but the protection scope of the present invention is not limited to the following embodiments. The experimental methods in the following embodiments without specifying specific conditions are usually carried out under conventional conditions.

[0022] All ranges disclosed herein are inclusive and independently combinable. The endpoints of ranges and any values ​​disclosed herein are not limited to the exact range or value, and these ranges or values ​​should be understood to include values ​​approximating these ranges or values.

[0023] Example 1

[0024] In a 500mL three-necked flask, add 500g soybean oil and 25g catalyst methanesulfonic acid, set the heating temperature to 90°C, and then heat at a heating rate of 5°C; stir and heat to 130°C, keep the reaction for 120min; then reduce the temperature to 50°C; add hot water to the polymerized oil, stir for 10-30 minutes, then stop stirring and settle to separate water, wash 3 times in this way; vacuum dry the washed oil at 100°C to remove residual water to obtain polymerized oil, and measure its 100°C kinematic viscosity: 38.82mm 2 / s, the kinematic viscosity of ordinary soybean oil at 100℃ is 7.37mm 2 / s.

[0025] Example 2

[0026] In a 500mL three-necked flask, add 500g soybean oil and 25g catalyst methanesulfonic acid, set the heating temperature to 90℃, and then heat at a heating rate of 5℃; stir and heat to 140℃, keep the reaction for 120min; then reduce the temperature to 50℃; add hot water to the polymerized oil, stir for 10-30 minutes, then stop stirring and settle to separate water, wash 3 times in this way; vacuum dry the washed oil at 100℃ to remove residual water to obtain polymerized oil, and measure its 100℃ kinematic viscosity: 75.67mm 2 / s, the kinematic viscosity of ordinary soybean oil at 100℃ is 7.37mm 2 / s.

[0027] Example 3

[0028] In a 500mL three-necked flask, add 500g soybean oil and 25g catalyst methanesulfonic acid, set the heating temperature to 90°C, and then heat at a heating rate of 5°C; stir and heat to 150°C, keep the reaction for 120min; then reduce the temperature to 50°C; add hot water to the polymerized oil, stir for 10-30 minutes, then stop stirring and settle to separate water, wash 3 times in this way; vacuum dry the washed oil at 100°C to remove residual water to obtain polymerized oil, and measure its 100°C kinematic viscosity: 137.45mm 2 / s, the kinematic viscosity of ordinary soybean oil at 100℃ is 7.37mm 2 / s.

[0029] Example 4

[0030] In a 500mL three-necked flask, add 500g soybean oil and 30g catalyst methanesulfonic acid, set the heating temperature to 90℃, and then heat at a heating rate of 5℃; stir and heat to 150℃, keep the reaction for 150min; then reduce the temperature to 50℃; add hot water to the polymerized oil, stir for 10-30 minutes, then stop stirring and settle to separate water, wash 3 times in this way; vacuum dry the washed oil at 100℃ to remove residual water to obtain polymerized oil, and measure its 100℃ kinematic viscosity: 1607.96mm 2 / s, the kinematic viscosity of ordinary soybean oil at 100℃ is 7.37mm 2 / s.

[0031] Example 5

[0032] In a 500mL three-necked flask, add 500g soybean oil and 30g catalyst methanesulfonic acid, set the heating temperature to 90℃, and then heat at a heating rate of 5℃; stir and heat to 160℃, keep the reaction for 120min; then reduce the temperature to 50℃; add hot water to the polymerized oil, stir for 10-30 minutes, then stop stirring and settle to separate water, wash 3 times in this way; vacuum dry the washed oil at 100℃ to remove residual water to obtain polymerized oil, and measure its 100℃ kinematic viscosity: 216.14mm 2 / s, the kinematic viscosity of ordinary soybean oil at 100℃ is 7.37mm 2 / s.

[0033] Example 6

[0034] In a 500mL three-necked flask, add 500g soybean oil and 5g catalyst perchloric acid, set the heating temperature to 90°C, and then heat at a heating rate of 5°C; stir and heat to 100°C, keep the reaction for 120min; then reduce the temperature to 50°C; add hot water to the polymerized oil, stir for 10-30 minutes, then stop stirring and settle to separate water, wash 3 times in this way; vacuum dry the washed oil at 100°C to remove residual water to obtain polymerized oil, and measure its 100°C kinematic viscosity: 151.39mm 2 / s, the kinematic viscosity of ordinary soybean oil at 100℃ is 7.37mm 2 / s.

[0035] Example 7

[0036] In a 500mL three-necked flask, add 500g soybean oil and 5g perchloric acid catalyst, set the heating temperature to 90°C, and then heat at a heating rate of 5°C; stir and heat to 120°C, and keep the reaction for 120 minutes; then reduce the temperature to 50°C; add hot water to the polymerized oil, stir for 10-30 minutes, then stop stirring and settle to separate water, and wash 3 times in this way; vacuum dry the washed oil at 100°C to remove residual water to obtain polymerized oil, and measure its 100°C kinematic viscosity: 193.86mm 2 / s, the kinematic viscosity of ordinary soybean oil at 100℃ is 7.37mm 2 / s.

[0037] Example 8

[0038] In a 500mL three-necked flask, add 500g soybean oil and 2.5g perchloric acid catalyst, set the heating temperature to 90°C, and then heat at a heating rate of 5°C; stir and heat to 120°C, and keep the reaction for 120 minutes; then reduce the temperature to 50°C; add hot water to the polymerized oil, stir for 10-30 minutes, then stop stirring and settle to separate water, and wash 3 times in this way; vacuum dry the washed oil at 100°C to remove residual water to obtain polymerized oil, and measure its 100°C kinematic viscosity: 31.94mm 2 / s, the kinematic viscosity of ordinary soybean oil at 100℃ is 7.37mm 2 / s.

[0039] Example 9

[0040] In a 500mL three-necked flask, add 500g soybean oil and 7.5g perchloric acid catalyst, set the heating temperature to 90°C, and then heat at a heating rate of 5°C; stir and heat to 120°C, and keep the reaction for 120 minutes; then reduce the temperature to 50°C; add hot water to the polymerized oil, stir for 10-30 minutes, then stop stirring and settle to separate water, and wash 3 times in this way; vacuum dry the washed oil at 100°C to remove residual water to obtain polymerized oil, and measure its 100°C kinematic viscosity: 152.12mm 2 / s, the kinematic viscosity of ordinary soybean oil at 100℃ is 7.37mm 2 / s.

[0041] Example 10

[0042] In a 500mL three-necked flask, add 500g soybean oil and 10g perchloric acid catalyst, set the heating temperature to 90°C, and then heat at a heating rate of 5°C; stir and heat to 120°C, and keep the reaction for 120 minutes; then reduce the temperature to 50°C; add hot water to the polymerized oil, stir for 10-30 minutes, then stop stirring and settle to separate water, and wash 3 times in this way; vacuum dry the washed oil at 100°C to remove residual water to obtain polymerized oil, and measure its 100°C kinematic viscosity: 72.11mm 2 / s, the kinematic viscosity of ordinary soybean oil at 100℃ is 7.37mm 2 / s.

[0043] Of course, the present invention may have many other embodiments. Without departing from the spirit and essence of the present invention, technicians familiar with the field may make various corresponding changes and deformations based on the present invention, but these corresponding changes and deformations should all fall within the scope of protection of the present invention.

Claims

1. A method for preparing a polymerized grease, characterized in that Vegetable oil is used as raw material to carry out polymerization reaction to obtain polymerized oils with different molecular weights. The synthesized products can have different uses. The preparation method includes the following steps: (1) Add vegetable oil to a reactor equipped with a stirrer, add a catalyst while stirring, and inject the catalyst below the liquid level; (2) Setting the heating temperature to 90°C, and then heating at a heating rate of 5°C; (3) stirring and heating to 100-160° C., and maintaining the reaction for 120-300 min; (4) Lower the temperature to 50°C; (5) Add hot water to the polymerized oil and stir for 10-30 minutes, then stop stirring and allow to settle to separate the water, and repeat this process three times; (6) The washed oil is vacuum dried at 100°C to remove residual water to obtain polymerized oil.

2. The method according to claim 1, characterized in that The catalyst is methanesulfonic acid.

3. The method according to claim 1, characterized in that The catalyst is perchloric acid.

4. The method according to claim 1 and 2, characterized in that The amount of catalyst used is 5-10% of the total amount (weight) of raw materials.

5. According to claims 1 and 3, characterized in that The amount of catalyst used is 0.5-2% of the total amount (weight) of raw materials.