Preparation method of polyether type heavy-load worm and gear oil

Abstract

The invention relates to the technical field of industrial lubricating oil, in particular to a preparation method of polyether type heavy-load worm and gear oil, which comprises the following preparation steps: S1, synthesizing an intermediate; s2, synthesizing an ionic liquid; s3, compounding is carried out; and S4, carrying out post-treatment. The ionic liquid containing the trifluoromethylsulfonyl imide group and 4, 4 '-dioctyl diphenylamine generate a synergistic effect, the flash point of the polyether type heavy-load worm and gear oil can be increased by 10-30 DEG C, meanwhile, the three technical problems of flash point, oxidation resistance and low-temperature fluidity are solved, and the polyether type heavy-load worm and gear oil is particularly suitable for heavy-load worm gear transmission systems such as wind power gear boxes and metallurgical machinery.

Description

Technical Field

[0001] The present invention relates to the technical field of industrial lubricating oils, and particularly to a preparation method of a polyether-type heavy-duty worm and worm gear oil. Background Art

[0002] With the development of industrial equipment towards high speed and heavy load, the worm and worm gear drive system has put forward more stringent requirements for the performance of lubricating oils. Traditional mineral oil-based lubricants have shown obvious deficiencies under high temperature, high pressure and extreme friction conditions, which are specifically manifested as follows: 1. Although conventional sulfur / phosphorus extreme pressure additives can improve anti-wear performance, they will corrode copper alloy worm wheels. In addition, solid lubricants such as molybdenum disulfide have poor dispersion stability; 2. Existing technologies usually improve the flash point by adding high-boiling solvents, but this will lead to deterioration of low-temperature fluidity. Summary of the Invention

[0003] The purpose of the present invention is to provide a preparation method of a polyether-type heavy-duty worm and worm gear oil to solve the problems raised in the above background art.

[0004] To achieve the above purpose, the present invention provides the following technical solution: A preparation method of a polyether-type heavy-duty worm and worm gear oil, including the following preparation steps:

[0005] S1. Synthesize an intermediate: Mix polyethylene glycol monomethyl ether and 1-methylimidazole in a molar ratio of 1:(1.1 - 1.2), add them to a reaction kettle under nitrogen protection, heat to 65 ± 2 °C, stir at 1000 rpm for 2 - 3 h, and perform vacuum distillation at 70 °C / 0.08 Pa to obtain the intermediate;

[0006] S2. Synthesize an ionic liquid: Mix the intermediate and lithium bis(trifluoromethanesulfonyl)imide in a molar ratio of 1:(1 - 1.05), heat to 55 ± 2 °C, stir at 600 rpm for 4 - 5 h, cool to room temperature, perform centrifugal filtration, and perform vacuum distillation at 75 °C / 0.1 Pa to obtain the ionic liquid;

[0007] S3. Compound: Add the ionic liquid to a blending kettle, after heating to 80 ± 5 °C, sequentially add 0.8 - 1.2 wt% rust inhibitor, 5 - 8 wt% triethanolamine borate, 0.8 - 1.2 wt% nano tungsten disulfide, and 2.2 - 2.8 wt% 4,4'-dioctyldiphenylamine, stir at 600 rpm for 2 - 3 h, sequentially add 2.5 - 3.5 wt% viscosity modifier and 0.02 - 0.04 wt% defoamer, stir at 2000 rpm for 1 - 2 h, and cool to room temperature to obtain the lubricating oil;

[0008] S4. Post-treatment: Pass the lubricating oil through a 5-μm stainless steel sintered mesh and a 0.1-μm ceramic membrane in sequence to obtain the polyether-type heavy-duty worm and worm gear oil.

[0009] Optionally, the molecular weight of the polyethylene glycol monomethyl ether is 400-600, and the hydroxyl value is 110-130 mg KOH / g.

[0010] Optionally, the chemical general formula of the ionic liquid lubricating oil is A + B － , where A + has a structural formula of , n represents the number of repeating units of the polyethylene glycol chain, and B － has a structural formula of .

[0011] Optionally, the particle size of the nano tungsten disulfide is 50 nm, and the specific surface area is 25 m 2 / g.

[0012] Optionally, the rust inhibitor is one of barium petroleum sulfonate, barium dinonylnaphthalene sulfonate, and calcium lignosulfonate.

[0013] Optionally, the viscosity regulator is one of polyalpha-olefin, polyalkylstyrene, polyisobutene, and polymethacrylate.

[0014] Optionally, the defoamer is polyether-modified silicone oil or fluorinated polyether.

[0015] Compared with the prior art, the present invention has the following beneficial effects:

[0016] 1. By the synergistic effect of the ionic liquid containing trifluoromethylsulfonylimide groups and 4,4'-dioctyldiphenylamine, the present invention can increase the flash point of the polyether-type heavy-duty worm gear oil by 10-30 °C, and at the same time solve the three major technical problems of flash point, antioxidant property, and low-temperature fluidity, and is particularly suitable for heavy-duty worm gear drive systems such as wind power gearboxes and metallurgical machinery;

[0017] 2. The polar groups of the ionic liquid in the present invention can wrap the nano tungsten disulfide particles to prevent agglomeration. Compared with traditional sulfur-containing extreme pressure agents such as sulfurized olefins, the sulfur in the nano tungsten disulfide is stable and there is no risk of copper corrosion. The nano tungsten disulfide particles form a microscopic rolling layer between the friction pairs, converting sliding friction into rolling friction and effectively reducing the friction coefficient. Specific Embodiments

[0018] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Apparently, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.

[0019] Example 1: The present invention provides a preparation method of a polyether-type heavy-duty worm gear oil, including the following preparation steps:

[0020] S1. Synthesis of intermediate: Mix polyethylene glycol monomethyl ether and 1-methylimidazole in a molar ratio of 1:1.1, add them to a reaction kettle under nitrogen protection, heat to 65 °C, stir at 1000 rpm for 2 h, and perform vacuum distillation at 70 °C / 0.08 Pa to obtain the intermediate;

[0021] S2. Synthesis of ionic liquid: Mix the intermediate and lithium bis(trifluoromethanesulfonyl)imide in a molar ratio of 1:1, heat to 55 °C, stir at 600 rpm for 4 h, cool to room temperature, perform centrifugal filtration, and perform vacuum distillation at 75 °C / 0.1 Pa to obtain the ionic liquid;

[0022] S3. Compound: Add the ionic liquid to a blending kettle, after heating to 80 °C, sequentially add 0.8 wt% barium petroleum sulfonate, 5 wt% triethanolamine borate, 0.8 wt% nano tungsten disulfide, and 2.2 wt% 4,4'-dioctyldiphenylamine, stir at 600 rpm for 2 h, sequentially add 2.5 wt% poly-α-olefin and 0.02 wt% polyether-modified silicone oil, stir at 2000 rpm for 1 h, and cool to room temperature to obtain the lubricating oil;

[0023] S4. Post-treatment: Pass the lubricating oil through a 5-μm stainless steel sintered mesh and a 0.1-μm ceramic membrane in sequence to obtain the polyether-type heavy-duty worm gear oil.

[0024] Example 2: The present invention provides a preparation method of a polyether-type heavy-duty worm gear oil, including the following preparation steps:

[0025] S1. Synthesis of intermediate: Mix polyethylene glycol monomethyl ether and 1-methylimidazole in a molar ratio of 1:1.15, add them to a reaction kettle under nitrogen protection, heat to 63 °C, stir at 1000 rpm for 2.5 h, and perform vacuum distillation at 70 °C / 0.08 Pa to obtain the intermediate;

[0026] S2. Synthesis of ionic liquid: Mix the intermediate and lithium bis(trifluoromethanesulfonyl)imide in a molar ratio of 1:1.02, heat to 53 °C, stir at 600 rpm for 4.5 h, cool to room temperature, perform centrifugal filtration, and perform vacuum distillation at 75 °C / 0.1 Pa to obtain the ionic liquid;

[0027] S3. Compound: Add the ionic liquid to a blending kettle, after heating to 75 °C, sequentially add 1.0 wt% barium dinonylnaphthalene sulfonate, 6 wt% triethanolamine borate, 1.0 wt% nano tungsten disulfide, and 2.4 wt% 4,4'-dioctyldiphenylamine, stir at 600 rpm for 2.5 h, sequentially add 3.2 wt% cohesive alkyl styrene and 0.03 wt% polyether-modified silicone oil, stir at 2000 rpm for 1.5 h, and cool to room temperature to obtain the lubricating oil;

[0028] S4. Post-treatment: Pass the lubricating oil through a 5-μm stainless steel sintered mesh and a 0.1-μm ceramic membrane in sequence to obtain the polyether-type heavy-duty worm gear oil.

[0029] Example 3: The present invention provides a preparation method of a polyether-type heavy-duty worm gear oil, comprising the following preparation steps:

[0030] S1. Synthesis of intermediate: Mix polyethylene glycol monomethyl ether and 1-methylimidazole at a molar ratio of 1:1.18, add them to a reaction kettle under nitrogen protection, heat to 66°C, stir at 1000 rpm for 2.5 h, and perform vacuum distillation at 70°C / 0.08 Pa to obtain the intermediate;

[0031] S2. Synthesis of ionic liquid: Mix the intermediate and lithium bis(trifluoromethanesulfonyl)imide at a molar ratio of 1:1.03, heat to 55°C, stir at 600 rpm for 4.5 h, cool to room temperature, perform centrifugal filtration, and perform vacuum distillation at 75°C / 0.1 Pa to obtain the ionic liquid;

[0032] S3. Compound: Add the ionic liquid to a blending kettle, after heating to 83°C, add 1.1 wt% calcium lignosulfonate, 7 wt% triethanolamine borate, 1.1 wt% nano tungsten disulfide, and 2.6 wt% 4,4'-dioctyldiphenylamine in sequence, stir at 600 rpm for 2.5 h, add 3.0 wt% polyisobutene and 0.03 wt% polyether-modified silicone oil in sequence, stir at 2000 rpm for 1.5 h, and cool to room temperature to obtain the lubricating oil;

[0033] S4. Post-treatment: Pass the lubricating oil through a 5-μm stainless steel sintered mesh and a 0.1-μm ceramic membrane in sequence to obtain the polyether-type heavy-duty worm gear oil.

[0034] Example 4: The present invention provides a preparation method of a polyether-type heavy-duty worm gear oil, comprising the following preparation steps:

[0035] S1. Synthesis of intermediate: Mix polyethylene glycol monomethyl ether and 1-methylimidazole at a molar ratio of 1:1.2, add them to a reaction kettle under nitrogen protection, heat to 67°C, stir at 1000 rpm for 3 h, and perform vacuum distillation at 70°C / 0.08 Pa to obtain the intermediate;

[0036] S2. Synthesis of ionic liquid: Mix the intermediate and lithium bis(trifluoromethanesulfonyl)imide at a molar ratio of 1:1.05, heat to 57°C, stir at 600 rpm for 5 h, cool to room temperature, perform centrifugal filtration, and perform vacuum distillation at 75°C / 0.1 Pa to obtain the ionic liquid;

[0037] S3. Compound: Add the ionic liquid into a blending kettle. After heating to 85 °C, successively add 1.2 wt% barium petroleum sulfonate, 8 wt% triethanolamine borate, 1.2 wt% nano tungsten disulfide, and 2.8 wt% 4,4'-dioctyldiphenylamine, stir at 600 rpm for 3 h, successively add 3.5 wt% polymethacrylate and 0.04 wt% fluorinated polyether, stir at 2000 rpm for 2 h, and cool to room temperature to obtain a lubricating oil;

[0038] S4. Post-treatment: Pass the lubricating oil through a 5-μm stainless steel sintered mesh and a 0.1-μm ceramic membrane successively to obtain the polyether-type heavy-duty worm gear oil.

[0039] In Examples 1 to 4, the molecular weight of poly(ethylene glycol) monomethyl ether is 400 - 600, and the hydroxyl value is 110 - 130 mgKOH / g. The chemical general formula of the ionic liquid lubricating oil is A + B － , where the structural formula of A + is , n represents the number of repeating units of the polyethylene glycol chain, and the structural formula of B － is . The particle size of nano tungsten disulfide is 50 nm, and the specific surface area is 25 m 2 / g.

[0040] Comparative Example 1

[0041] It is basically the same as Example 1, and the only difference is that 4,4'-dioctyldiphenylamine is not used.

[0042] Comparative Example 2

[0043] It is basically the same as Example 1, and the only difference is that a high-viscosity mineral base oil is used to replace the ionic liquid to prepare a worm gear mineral oil, where the kinematic viscosity of the high-viscosity mineral base oil at 40 °C is 68 cSt and the specific gravity is 0.873.

[0044] Test Example 1

[0045] Test content: According to the test method disclosed in GB / T 267-1988, respectively test the flash points of the polyether-type heavy-duty worm gear oils prepared in Examples 1 to 4 and Comparative Example 1, and the worm gear mineral oil prepared in Comparative Example 2, and the results are recorded in Table 1.

[0046] Test Example 2

[0047] Test content: According to the test method disclosed in SH / T 0074, the oxidation stability of the polyether heavy-duty worm gear oils prepared in Examples 1-4 and Comparative Example 1 was tested by the rotating oxygen bomb method, and the results were recorded in Table 1. The test temperature was 160 °C, and the test conditions of the oxygen bomb were: pressure 620 Kpa, rotation speed 100 rpm. The oxidation stability was the time required for the oxygen bomb pressure to drop from the highest point to 172 kPa.

[0048] Test Example 3

[0049] Test content: According to the test method disclosed in GB / T 3535-2006, the pour points of the polyether heavy-duty worm gear oils prepared in Examples 1-4 were tested respectively, and the results were recorded in Table 1.

[0050] Table 1

[0051] Flash point (open cup method) / ℃ Oxidation stability / min Pour point / ℃ Example 1 235 321 -43 Example 2 230 334 -43 Example 3 250 328 -43 Example 4 247 325 -43 Comparative Example 1 220 125 - Comparative Example 2 195 - -

[0052] As can be seen from Table 1, 4,4'-dioctyldiphenylamine can increase the flash point of the polyether heavy-duty worm gear oil by 10-30 °C. 4,4'-dioctyldiphenylamine has no significant increase in the flash point of high-viscosity mineral base oil, that is, non-ionic base oil. As can be seen from Table 1, 4,4'-dioctyldiphenylamine can improve the oxidation stability of the polyether heavy-duty worm gear oil.

[0053] Generally, 4,4'-dioctyldiphenylamine, as an amine antioxidant, its main function is to capture free radicals. In the present invention, through the synergistic effect of the ionic liquid containing a trifluoromethylsulfonylimide group and 4,4'-dioctyldiphenylamine, the flash point can be increased by 10-30 °C. The present invention discloses a method for improving the antioxidant property of lubricating oil and effectively increasing its flash point, breaking the traditional concept in the industry.

[0054] As can be seen from Table 1, the pour points of the polyether heavy-duty worm gear oils prepared in Test Examples 1-4 are all -43 °C. Therefore, 4,4'-dioctyldiphenylamine added in the present invention as an amine antioxidant will not cause deterioration of low-temperature fluidity.

[0055] Although the embodiments of the present invention have been shown and described, for those of ordinary skill in the art, it can be understood that various changes, modifications, substitutions and variations can be made to these embodiments without departing from the principles and spirit of the present invention. The scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A preparation method of a polyether-type heavy-duty worm gear oil, characterized in that: It includes the following preparation steps: S1. Synthesis of intermediate: Mix polyethylene glycol monomethyl ether and 1-methylimidazole at a molar ratio of 1:(1.1 - 1.2), add them to a reaction kettle under nitrogen protection, heat to 65±2°C, stir at 1000 rpm for 2 - 3 h, and perform vacuum distillation at 70°C / 0.08 Pa to obtain the intermediate; S2. Synthesis of ionic liquid: Mix the intermediate and lithium bis(trifluoromethanesulfonyl)imide at a molar ratio of 1:(1 - 1.05), heat to 55±2°C, stir at 600 rpm for 4 - 5 h, cool to room temperature, perform centrifugal filtration, and perform vacuum distillation at 75°C / 0.1 Pa to obtain the ionic liquid; S3. Compound: Add the ionic liquid to a blending kettle, after heating to 80±5°C, sequentially add 0.8 - 1.2 wt% rust inhibitor, 5 - 8 wt% triethanolamine borate, 0.8 - 1.2 wt% nano tungsten disulfide, and 2.2 - 2.8 wt% 4,4'-dioctyldiphenylamine, stir at 600 rpm for 2 - 3 h, sequentially add 2.5 - 3.5 wt% viscosity regulator and 0.02 - 0.04 wt% defoamer, stir at 2000 rpm for 1 - 2 h, and cool to room temperature to obtain the lubricating oil; S4. Post-treatment: Pass the lubricating oil through a 5-μm stainless steel sintered mesh and a 0.1-μm ceramic membrane in sequence to obtain the polyether-type heavy-duty worm gear oil.

2. The preparation method of a polyether-based heavy-duty worm gear oil according to claim 1, characterized in that: The molecular weight of the polyethylene glycol monomethyl ether is 400 - 600, and the hydroxyl value is 110 - 130 mgKOH / g.

3. The preparation method of a polyether-based heavy-duty worm and worm gear oil according to claim 1, characterized in that: The chemical general formula of the ionic liquid lubricant is A + B － , where the structural formula of A + is , n represents the number of repeating units of the polyethylene glycol chain, and the structural formula of B － is .

4. The preparation method of a polyether-based heavy-duty worm gear oil according to claim 1, characterized in that: The particle size of the tungsten disulfide nanomaterial is 50 nm, and the specific surface area is 25 m 2 / g.

5. The preparation method of a polyether-based heavy-duty worm gear oil according to claim 1, characterized in that: The rust inhibitor is one of barium petroleum sulfonate, barium dinonylnaphthalene sulfonate, and calcium lignosulfonate.

6. The preparation method of a polyether-based heavy-duty worm gear oil according to claim 1, characterized in that: The viscosity regulator is one of poly-α-olefin, polyalkylstyrene, polyisobutene, and polymethacrylate.

7. The preparation method of a polyether-based heavy-duty worm gear oil according to claim 1, characterized in that: The defoamer is polyether-modified silicone oil or fluorinated polyether.

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