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A kind of lithium-composite calcium base lubricating grease and preparation method thereof

A technology of complex calcium-based lubricating grease and base oil, which is applied in lubricating compositions, thickeners, and the petroleum industry, and can solve problems such as poor comprehensive performance, unstable performance of lubricating grease products, and serious volatilization of small molecular acids. Achieve the effect of avoiding difficult operation and shortening the reaction time at high temperature

Active Publication Date: 2020-01-10
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The problems of this preparation process are that small molecular acid volatilization phenomenon is serious, saponification reaction cannot be completely carried out, and the properties of the obtained lubricating grease products are unstable and the comprehensive performance is poor.

Method used

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  • A kind of lithium-composite calcium base lubricating grease and preparation method thereof
  • A kind of lithium-composite calcium base lubricating grease and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Prepare 20kg of lubricating grease, the thickener amount is 12%, the mass ratio of complex calcium soap to lithium soap is 1:9, and the mass ratio of calcium hydroxide to lithium hydroxide monohydrate is 1:4.8.

[0030] Raw material components: 12-hydroxystearic acid (1.27kg); acetic acid (0.11kg, content ≥ 99%); lithium hydroxide monohydrate (0.41kg); calcium hydroxide (0.09kg); base oil Daqing 400 (17.6 kg, 100℃ kinematic viscosity 9.7mm 2 / s).

[0031] Add 11kg of mineral base oil Daqing 400 and 0.06kg of calcium hydroxide aqueous solution dissolved in 3 times the amount of water into the saponification reaction kettle, mix and stir evenly, heat up to 38°C, add 0.11kg of acetic acid, react for 30min, then heat up to 87°C, Add 1.27kg of 12-hydroxystearic acid, until the 12-hydroxystearic acid is completely dissolved, add 0.03kg of calcium hydroxide and 0.41kg of lithium hydroxide monohydrate mixed lye dissolved in 8 times the amount of water, and react at 90°C 60min...

Embodiment 2

[0033] Prepare 20kg of lubricating grease, the thickener amount is 20%, the mass ratio of complex calcium soap to lithium soap is 3:7, and the mass ratio of calcium hydroxide to lithium hydroxide monohydrate is 1:1.08.

[0034] Raw material components: 12-hydroxystearic acid (2.67kg); terephthalic acid (0.54kg); lithium hydroxide monohydrate (0.39kg); calcium hydroxide (0.36kg); Daqing 400 (16kg, 100 ° C exercise Viscosity 9.7mm 2 / s).

[0035] Lithium complex calcium-based grease was prepared according to the method of Example 1, except that a raw material used in the preparation was changed, the acetic acid used was changed to terephthalic acid, and the thickener content was changed from 12% to 20%. The mass ratio of complex calcium soap and lithium soap in the thickener was changed from 1:9 to 3:7; and the preparation process conditions were changed, and the reaction time between calcium hydroxide and small molecule acid was changed from 30 minutes to 60 minutes. The prod...

Embodiment 3

[0037] Prepare 20kg of lubricating grease, the thickener amount is 30%, the mass ratio of complex calcium soap to lithium soap is 5:5, and the mass ratio of calcium hydroxide to lithium hydroxide monohydrate is 1:0.46.

[0038] Raw material components: stearic acid (4.16kg); boric acid (1.34kg, content ≥ 99%); lithium hydroxide monohydrate (0.44kg); calcium hydroxide (0.95kg); Daqing 400 (14kg, 100 ℃ kinematic viscosity 9.7mm 2 / s).

[0039] Lithium complex calcium-based grease was prepared according to the method of Example 1, the difference being that the two raw materials used in the preparation were changed, the 12-hydroxystearic acid used was changed to stearic acid, the acetic acid used was changed to boric acid, thickened The thickener content was changed from 12% to 30%, and the mass ratio of complex calcium soap and lithium soap in the thickener was changed from 1:9 to 5:5.

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Abstract

The invention provides a preparation method of lithium-complex calcium lubricating grease. The preparation method comprises the following steps: (1) adding a part of calcium hydroxide aqueous solution in a part of base oil, and uniformly stirring; (2) heating, and adding small molecule acid to carry out reaction while rising the temperature to 20-60 DEG C; (3) continuously rising the temperature to 75-100 DEG C, and adding a unitary long-chain organic acid; (4) after the unitary long-chain organic acid is completely dissolved, adding residual mixed alkali solution of calcium hydroxide and lithium hydroxide monohydrate to carry out saponification reaction; and (5) heating to rise the temperature to 180-250 DEG C, carrying out high-temperature refining, cooling, adding the balance of the base oil, adding a necessary additive, and carrying out circulation shearing homogenization, degassing and filtering to obtain a finished product. By adopting the preparation method of the lithium-complex calcium lubricating grease provided by the invention, the mass ratio of the calcium hydroxide to the lithium hydroxide can be arbitrarily blended, and the problems of volatilization of the small molecule acid, incomplete saponification reaction and the like are solved at the same time. The obtained lubricating grease product has the advantages of higher dropping point, better mechanical stability, better water spray resistance and more stable comprehensive properties.

Description

technical field [0001] The invention belongs to lubricating grease and a preparation method thereof. Background technique [0002] Composite calcium-based grease is the earliest high-temperature grease synthesized and used. It has the characteristics of wide source of raw materials, low price, and excellent performance. However, it has the problem of surface hardening under storage and high-temperature use conditions. Introducing lithium soap into complex calcium-based grease to prepare lithium-complex calcium-based grease can effectively solve the hardening problem of complex calcium-based grease and improve the mechanical stability of complex calcium-based grease. [0003] CN 104449983A proposes a preparation method of lithium complex calcium-based lubricating grease. In the preparation process, 12-hydroxystearic acid and lithium hydroxide are first added to react to prepare lithium soap, and then small molecular acid, calcium hydroxide and remaining A certain amount of 1...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C10M169/02C10M169/06C10M177/00C10M117/04C10M117/06C10M117/10C10M123/02
CPCC10M113/00C10M117/02C10M117/04C10M117/06C10M117/10C10M123/02C10M169/02C10M169/06C10M177/00C10M2201/0856C10M2201/0876C10M2203/1006C10M2207/1225C10M2207/1236C10M2207/1245C10M2207/1426C10N2020/02C10N2010/02C10N2010/04
Inventor 姚潇孙洪伟陈政何懿峰郑会段庆华刘中其姜靓
Owner CHINA PETROLEUM & CHEM CORP
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