Compound titanium urea-based grease and its preparation method

Abstract

The present invention discloses a composite titanium urea-based grease and a preparation method thereof, and relates to the technical field of grease. The preparation method of the present invention comprises the following steps: S1: adding tetraisopropyl titanate after mixing a stearic acid compound, a low molecular weight acid compound, an isocyanate compound and a base oil component 1, and continuing the reaction; S2: heating to 90-115°C, adding deionized water, and keeping the temperature for reaction; S3: continuing to heat and keep the temperature; S4: high-temperature refining, adding a structure improver, reacting for a period of time, adding the base oil component 2, cooling and adding additives to obtain a composite titanium polyurea grease. The present application prepares a thickener added to a titanium urea-based grease by a one-step process, which has the characteristics of good thermal stability and strong antioxidant properties, simple process, and excellent product performance.

Description

Technical Field

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

[0002] In the past two years, with the rapid development of the new energy industry, the demand for lithium resources in the battery and energy storage industries has increased significantly. The price of lithium hydroxide monohydrate has skyrocketed, leading to a sharp increase in the cost of lithium-based greases for grease manufacturers. General-purpose lithium and lithium-complex products, which account for a large market share, are facing an unaffordable situation. Current trends indicate that lithium resource prices are unlikely to fall in the near term and may even rise further. Finding suitable alternatives has become the top priority for grease manufacturers. Considering both cost and performance, polyurea grease has become the preferred choice. With excellent oxidation stability and high-temperature resistance, it represents an upgrade to traditional lithium-based products and has been widely used in industries such as metallurgy and home appliances. However, the structural strength of the polyurea thickener gel particles is relatively low. Compared with lithium-based greases, it exhibits poor adhesion and lacks skeletal strength, making it prone to loss in areas without a good seal. Furthermore, the shear stability of conventional polyureas is inferior to that of lithium-based greases. Therefore, improving the relevant properties of polyurea greases has become a hot research topic for grease manufacturers.

[0003] Extensive research has been conducted abroad on composite polyurea thickeners, and commercial products such as polyurea metal sodium salts, polyurea metal lithium salts, polyurea-calcium acetate composites, and polyurea-calcium acetate / calcium carbonate composites have also been widely used. This patent utilizes composite titanium, which exhibits excellent gelling properties, superior shear resistance, and good extreme pressure and anti-wear properties, to compound the polyurea thickener. This composite titanium urea-based grease exhibits excellent overall performance, making it a perfect alternative and upgrade to lithium-based greases. Summary of the Invention

[0004] The purpose of the present invention is to provide a composite titanium urea-based grease and a preparation method thereof to solve the following technical problems:

[0005] Existing polyurea thickener gel particles have the disadvantage of low structural strength. Compared with lithium-based grease, they also have insufficient adhesion and no skeleton strength. They are easy to lose in some application areas without good sealing and have poor shear stability compared to lithium-based grease.

[0006] The purpose of the present invention can be achieved through the following technical solutions:

[0007] The preparation method of composite titanium urea-based grease comprises the following steps:

[0008] S1: Mix the stearic acid compound, the low molecular weight acid compound, the isocyanate compound and the base oil component, heat to 60-80°C, add the amine compound, keep warm for 0.1-0.5h, add tetraisopropyl titanate, and keep warm for 0.5-1h;

[0009] S2: Continue heating to 90-115°C, add deionized water, and keep warm for 20-40 minutes;

[0010] S3: Continue heating to 130-140°C and keep warm for 20-40 minutes;

[0011] S4: Continue high-temperature refining, add a structure improver, keep warm for 10-30 minutes, add the base oil component 2, cool to 70-90°C, add additives, and obtain a composite titanium polyurea grease.

[0012] As a further solution of the present invention: the base oil component 1 and the base oil component 2 are in the same distribution ratio, and are obtained by mixing one or two of cycloalkyl oil and paraffin-based mineral oil in any ratio.

[0013] As a further embodiment of the present invention, the base oil component 1 and the base oil component 2 both have a kinematic viscosity of 150-220 mm at 40°C. 2 / s.

[0014] As a further embodiment of the present invention, the structure improving agent is one or more of trimethylolpropane ester, pentaerythritol oleate, polymethacrylate, glycerol, and polyisobutylene mixed in any ratio.

[0015] As a further solution of the present invention: the additive is one or more of di-tert-butyl-p-cresol, diphenylamine, and zinc dialkylthiophosphate mixed in any ratio.

[0016] As a further embodiment of the present invention, the amine compound is any one of octadecylamine, aniline, and cyclohexylamine; the low molecular weight acid compound is any one of benzoic acid and adipic acid; the stearic acid compound is any one of dodecyl stearic acid and pentaerythritol stearate; and the isocyanate compound is diphenylmethane-4,4'-diisocyanate.

[0017] As a further embodiment of the present invention, the mass ratio of stearic acid compounds, low molecular weight acid compounds, isocyanate compounds, amine compounds, tetraisopropyl titanate, deionized water, structure improver, additives, base oil component one, and base oil component two is 2-8:1-1.2:1-2:0.6-2:2-5:5-10:1-10:0.5-5:35-45:35-45.

[0018] As a further solution of the present invention: the high temperature refining in S4 is specifically: heating to 160-190° C. to carry out high temperature refining reaction for 0.5-1 hour.

[0019] Composite titanium urea-based grease, prepared by any of the above preparation methods.

[0020] Beneficial effects of the present invention:

[0021] The present application uses stearic acid compounds, low molecular weight acid compounds, isocyanate compounds, amine compounds, and tetraisopropyl titanate as raw materials to prepare an organic compound as a thickener for titanium urea-based grease, which has the characteristics of good thermal stability and strong antioxidant properties. The present application adds additives to the components to improve the load-bearing capacity of the titanium urea-based grease and reduce wear. The present application adds a structural improver to the components to improve the shear resistance. The composite titanium polyurea thickener and composite titanium urea-based grease prepared in the present application are prepared by a one-step process, which is simple and has excellent product performance. DETAILED DESCRIPTION

[0022] The following is a clear and complete description of the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative efforts are within the scope of protection of the present invention.

[0023] Example 1

[0024] The preparation method of composite titanium urea-based grease comprises the following steps:

[0025] S1: Use cycloalkyl oil as base oil component 1 and base oil component 2. The kinematic viscosity of cycloalkyl oil at 40°C is 220 mm 2 / s;

[0026] S2: Mix 2 g of dodecyl hydroxystearic acid, 1 g of benzoic acid, 1 g of diphenylmethane-4,4'-diisocyanate and 35 g of cycloalkyl oil, heat to 60°C, add 0.6 g of cyclohexylamine, keep warm for 0.1 h, add 2 g of tetraisopropyl titanate, and keep warm for 0.5 h;

[0027] S3: Continue heating to 90°C, add 5g of deionized water, and keep warm for 20min;

[0028] S4: Continue heating to 130°C and keep warm for 20 minutes;

[0029] S5: Raise the temperature to 160°C for high-temperature refining reaction, react for 0.5h, add 1g of pentaerythritol oleate, keep warm for 10min, add 35g of cycloalkyl oil, cool to 70°C, add 0.5g of diphenylamine, and obtain composite titanium polyurea grease.

[0030] Example 2

[0031] The preparation method of composite titanium urea-based grease comprises the following steps:

[0032] S1: Use cycloalkyl oil as base oil component 1 and base oil component 2. The kinematic viscosity of cycloalkyl oil at 40°C is 220 mm 2 / s;

[0033] S2: Mix 4 g of dodecyl hydroxystearic acid, 1.1 g of benzoic acid, 1.2 g of diphenylmethane-4,4'-diisocyanate and 37 g of cycloalkyl oil, heat to 65°C, add 1 g of cyclohexylamine, keep warm for 0.2 h, add 3 g of tetraisopropyl titanate, and keep warm for 0.6 h;

[0034] S3: Continue heating to 95°C, add 6g of deionized water, and keep warm for 25min;

[0035] S4: Continue heating to 135°C and keep warm for 25 minutes;

[0036] S5: Raise the temperature to 170°C for high-temperature refining reaction, react for 0.6h, add 3g of pentaerythritol oleate, keep warm for 15min, add 38g of cycloalkyl oil, cool to 75°C, add 1g of diphenylamine, and obtain composite titanium polyurea grease.

[0037] Example 3

[0038] The preparation method of composite titanium urea-based grease comprises the following steps:

[0039] S1: Use cycloalkyl oil as base oil component 1 and base oil component 2. The kinematic viscosity of cycloalkyl oil at 40°C is 220 mm 2 / s;

[0040] S2: Mix 5 g of dodecyl hydroxystearic acid, 1.1 g of benzoic acid, 1.4 g of diphenylmethane-4,4'-diisocyanate, and 39 g of cycloalkyl oil, heat to 70°C, add 1.2 g of cyclohexylamine, and keep warm for 0.3 h. Add 4 g of tetraisopropyl titanate and keep warm for 0.7 h.

[0041] S3: Continue heating to 100°C, add 7g of deionized water, and keep warm for 30min;

[0042] S4: Continue heating to 135°C and keep warm for 30 minutes;

[0043] S5: Raise the temperature to 180°C for high-temperature refining reaction, react for 0.7h, add 6g of pentaerythritol oleate, keep warm for 20min, add 40g of cycloalkyl oil, cool to 80°C, add 2g of diphenylamine, and obtain composite titanium polyurea grease.

[0044] Example 4

[0045] The preparation method of composite titanium urea-based grease comprises the following steps:

[0046] S1: Use cycloalkyl oil as base oil component 1 and base oil component 2. The kinematic viscosity of cycloalkyl oil at 40°C is 220 mm 2 / s;

[0047] S2: Mix 6 g of dodecyl hydroxystearic acid, 1.2 g of benzoic acid, 1.8 g of diphenylmethane-4,4'-diisocyanate and 45 g of cycloalkyl oil, heat to 80°C, add 1.5 g of cyclohexylamine, keep warm for 0.4 h, add 4 g of tetraisopropyl titanate, and keep warm for 0.7 h;

[0048] S3: Continue heating to 110°C, add 10g of deionized water, and keep warm for 35min;

[0049] S4: Continue heating to 135°C and keep warm for 35 minutes;

[0050] S5: Raise the temperature to 180°C for high-temperature refining reaction, react for 1 hour, add 9g of pentaerythritol oleate, keep warm for 30 minutes, add 45g of cycloalkyl oil, cool to 90°C, add 4g of diphenylamine, and obtain composite titanium polyurea grease.

[0051] Example 5

[0052] The preparation method of composite titanium urea-based grease comprises the following steps:

[0053] S1: Use cycloalkyl oil as base oil component 1 and base oil component 2. The kinematic viscosity of cycloalkyl oil at 40°C is 220 mm 2 / s;

[0054] S2: 8 g of dodecyl hydroxystearic acid, 1.2 g of benzoic acid, 2 g of diphenylmethane-4,4'-diisocyanate and 45 g of cycloalkyl oil were mixed, the temperature was raised to 80°C, 2 g of cyclohexylamine was added, and the reaction was kept warm for 0.5 h. 5 g of tetraisopropyl titanate was added and the temperature was kept warm for 1 h.

[0055] S3: Continue heating to 115°C, add 10g of deionized water, and keep warm for 40min;

[0056] S4: Continue heating to 140°C and keep warm for 40 minutes;

[0057] S5: Raise the temperature to 190°C for high-temperature refining reaction, react for 1 hour, add 10g of pentaerythritol oleate, keep warm for 30 minutes, add 45g of cycloalkyl oil, cool to 90°C, add 5g of diphenylamine, and obtain composite titanium polyurea grease.

[0058] Performance testing

[0059] (1) Thermal stability: Tested according to GB / T269. The test results are shown in Table 1.

[0060] (2) Antioxidant properties: tested according to SH / T 0325. The test results are shown in Table 1.

[0061] Table 1: Statistics of performance test data of Examples 1-5

[0062]

[0063] As can be seen from Table 1, the grease prepared in this application has the characteristics of good thermal stability and excellent antioxidant performance.

[0064] The above is a detailed description of an embodiment of the present invention. However, the content described is only a preferred embodiment of the present invention and should not be considered to limit the scope of the present invention. All equivalent changes and improvements made within the scope of the present invention should still fall within the scope of the patent coverage of the present invention.

Claims

1. A method for preparing a composite titanium urea-based grease, characterized in that: The steps include: S1: Mix the stearic acid compound, the low molecular weight acid compound, the isocyanate compound and the base oil component, heat to 60-80°C, add the amine compound, keep warm for 0.1-0.5h, add tetraisopropyl titanate, and keep warm for 0.5-1h; S2: Continue heating to 90-115°C, add deionized water, and keep warm for 20-40 minutes; S3: Continue heating to 130-140°C and keep warm for 20-40 minutes; S4: Continue high-temperature refining, add a structure improver, keep warm for 10-30 minutes, add the base oil component 2, cool to 70-90°C, add additives, and obtain a composite titanium polyurea grease; The structure improving agent is one or more of trimethylolpropane ester, pentaerythritol oleate, polymethacrylate, glycerol and polyisobutylene mixed in any ratio.

2. The method for preparing the composite titanium urea-based grease according to claim 1, characterized in that: The base oil component 1 and the base oil component 2 have the same distribution ratio, and are obtained by mixing one or two of cycloalkyl oil and paraffin-based mineral oil in any ratio.

3. The method for preparing the composite titanium urea-based grease according to claim 2, characterized in that: The base oil component 1 and the base oil component 2 both have a kinematic viscosity of 150-220 mm² / s at 40°C.

4. The method for preparing the composite titanium urea-based grease according to claim 1, characterized in that: The additive is one or more of di-tert-butyl-p-cresol, diphenylamine and zinc dialkylthiophosphate mixed in any ratio.

5. The method for preparing the composite titanium urea-based grease according to claim 1, characterized in that: The amine compound is any one of octadecylamine, aniline, and cyclohexylamine; the low molecular weight acid compound is any one of benzoic acid and adipic acid; the stearic acid compound is any one of dodecyl stearic acid and pentaerythritol stearate; and the isocyanate compound is diphenylmethane-4,4'-diisocyanate.

6. The method for preparing the composite titanium urea-based grease according to claim 1, characterized in that: The mass ratio of stearic acid compounds, low molecular weight acid compounds, isocyanate compounds, amine compounds, tetraisopropyl titanate, deionized water, structure improver, additives, base oil component one, and base oil component two is 2-8:1-1.2:1-2:0.6-2:2-5:5-10:1-10:0.5-5:35-45:35-45.

7. The method for preparing the composite titanium urea-based grease according to claim 1, characterized in that: The specific steps of the medium-high temperature refining in S4 are as follows: heating the temperature to 160-190° C. for high temperature refining reaction, and the reaction time is 0.5-1 hour.

8. Composite titanium urea-based grease, characterized in that: Prepared by the preparation method according to any one of claims 1 to 7.

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