Preparation method of ester type fire-resistant hydraulic oil with long service life and high flash point

CN117887507BActive Publication Date: 2026-08-18AN HUI TECHSEA CHEM CO LTD
View PDF 2 Cites 0 Cited by

Patent Information

Application Number
CN202311758283.1
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-12-20
Publication Date
2026-08-18
Estimated Expiration
2043-12-20

AI Technical Summary

Technical Problem

本发明加入自制的抗氧组分,通过反应条件,调节反应进程,解决了氧化安定性差、闪点低的问题,延长了液压油使用寿命,复配其他添加剂使产品的性能达到最优

Benefits of technology

[0018]The beneficial effects of this invention are as follows: The self-made antioxidant component exhibits excellent oxidation stability, outperforming commercially available phenol-amine compounds used alone or in combination, thus solving the problem of short lifespan in ester-based fire-resistant hydraulic oils; the self-made antioxidant component does not affect the flash point of the base oil, enabling the product to reach a flash point above 315℃, which is 15-30℃ higher than that of commercially available ester-based fire-resistant hydraulic oils. The product of this invention is safer to use and is biodegradable.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure BDA0004617737940000021
    Figure BDA0004617737940000021
  • Figure BDA0004617737940000041
    Figure BDA0004617737940000041
  • Figure BDA0004617737940000051
    Figure BDA0004617737940000051
Patent Text Reader

Abstract

The application discloses a preparation method of long-life high-flash-point ester type fire-resistant hydraulic oil and belongs to the technical field of hydraulic oil. 98-99% base oil and 0.5-1.4% self-made antioxidant components are fully dissolved at 80 DEG C, then 0.2-0.5% anti-wear agents, 0.05-0.15% metal deactivators and 0.05-0.15% rust inhibitors are added, and the mixture is fully stirred at 50 DEG C for 0.5h to obtain the long-life high-flash-point ester type fire-resistant hydraulic oil. The self-made antioxidant components have excellent oxidation stability, and the effect is excellent compared with the effect of separately using or mixing using phenolic-amine on the market, and the short service life problem of the ester type fire-resistant hydraulic oil is solved; the self-made antioxidant components do not affect the flash point of the base oil, the flash point of the product reaches more than 315 DEG C, and the flash point of the product is improved by 15-30 DEG C compared with the flash point of the ester type fire-resistant hydraulic oil on the market. The product is safer to use, and the product can be biodegraded.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] This invention belongs to the field of hydraulic oil technology, specifically relating to a method for preparing long-life, high-flash-point ester-type fire-resistant hydraulic oil. Background Technology

[0002] Hydraulic oil is the hydraulic medium used in hydraulic systems that utilize liquid pressure energy. It plays a role in energy transfer, system lubrication, corrosion prevention, rust prevention, and cooling within the hydraulic system. Currently, the main fire-resistant hydraulic oils on the market are water-glycol-based and ester-based hydraulic oils. Water-glycol-based hydraulic oils have limited operating temperatures and poor lubrication, easily causing equipment to rust. Ester-based fire-retardant hydraulic oils, on the other hand, are fully synthetic hydraulic oils made from unsaturated polyol esters as base oils. They feature high flash points and ignition points, good flame retardant properties, high viscosity index, and a wide operating temperature range. They are safe to use and can meet the long-term operating requirements of hydraulic systems.

[0003] However, the base oil of domestic ester-type fire-resistant hydraulic oil is currently unsaturated polyol ester. During use, it is oxidized by high-temperature radiation, which causes it to polymerize and increase its viscosity. Therefore, developing a long-life, high-flash-point ester-type fire-resistant hydraulic oil to replace foreign products is of great significance for improving product utilization and reducing production costs. Summary of the Invention

[0004] The purpose of this invention is to overcome the shortcomings of existing technologies and provide a method for preparing a long-life, high-flash-point ester-type fire-resistant hydraulic oil. This invention incorporates a self-made antioxidant component and, by adjusting the reaction conditions and process, solves the problems of poor oxidation stability and low flash point, thus extending the service life of the hydraulic oil. Furthermore, the addition of other additives optimizes the product's performance.

[0005] The objective of this invention can be achieved through the following technical solutions:

[0006] The preparation method of long-life, high-flash-point ester-type fire-resistant hydraulic oil includes the following steps:

[0007] Dissolve 98-99% base oil and 0.5-1.4% self-made antioxidant components at 80°C, then add 0.2-0.5% anti-wear agent, 0.05-0.15% metal deactivator, and 0.05-0.15% rust inhibitor. Stir and mix thoroughly at 50°C for 0.5 hours to obtain a long-life, high-flash-point ester-type fire-resistant hydraulic oil.

[0008] Furthermore, 98.4% base oil and 1% self-made antioxidant components were fully dissolved at 80°C, followed by the addition of 0.4% anti-wear agent, 0.1% metal deactivator, and 0.1% rust inhibitor. The mixture was stirred thoroughly at 50°C for 0.5 hours to obtain a long-life, high-flash-point ester-type fire-resistant hydraulic oil.

[0009] Furthermore, the base oil is an unsaturated polyol ester.

[0010] Furthermore, the anti-wear agent is one or both of BASF 349 and BASF 353.

[0011] Furthermore, the metal deactivator is one or more of T551, T553 and T561.

[0012] Furthermore, the rust inhibitor is 5-methylbenztriazole.

[0013] The self-made antioxidant component is prepared through the following steps:

[0014] Bisphenol Z (2,2'-methylenebis-(4-methyl-6-tert-butylphenol)) and phosphorus oxychloride were added to a reaction vessel and reacted at room temperature for 1 hour. Then, p-methyl-m-hydroxydiphenylamine was added dropwise, and the temperature was raised to 80°C and reacted for 1-5 hours. The HCl gas generated during the reaction was absorbed with an alkaline solution, and the product was washed with water to obtain a liquid product—the self-made antioxidant component. The molar ratio of bisphenol Z, phosphorus oxychloride and p-methyl-m-hydroxydiphenylamine was 1-2:1:1-2.

[0015] The structural formula of the self-made antioxidant component is shown below, where t-Bu represents tert-butyl:

[0016]

[0017] Hydraulic oil undergoes extensive oxidation reactions and deteriorates under operating, storage, and application conditions, adversely affecting its physicochemical properties and shortening its service life. The self-made antioxidant component prepared in this invention contains both hindered phenolic and aromatic amine structures. These two structures work synergistically, exhibiting excellent oxidation stability, superior to commercially available phenol-amine compounds used alone or in combination. Together, they inhibit the oxidation reaction of hydraulic oil, reduce the catalytic effect of metals on oil oxidation, protect the main components of the hydraulic oil, and delay the oil aging process, thereby extending the hydraulic oil's lifespan. The phenolic hydroxyl groups on the hindered phenolic structure are sterically restricted, allowing hydrogen atoms to easily be stripped from the molecule and combine with peroxide radicals, alkoxy radicals, and hydroxyl radicals, thereby disrupting the free radical self-oxidation chain reaction and preventing the oxidation of the hydraulic oil. The aromatic amine structure is also a free radical terminator with a high operating temperature; therefore, the synergistic effect of these two structures makes the hydraulic oil of this invention difficult to oxidize even at high temperatures. The self-made antioxidant component does not affect the flash point of the base oil, allowing the product's flash point to reach above 315℃, which is 15-30℃ higher than the flash point of commercially available ester-based fire-resistant hydraulic oils, making it safer to use.

[0018] The beneficial effects of this invention are as follows: The self-made antioxidant component exhibits excellent oxidation stability, outperforming commercially available phenol-amine compounds used alone or in combination, thus solving the problem of short lifespan in ester-based fire-resistant hydraulic oils; the self-made antioxidant component does not affect the flash point of the base oil, enabling the product to reach a flash point above 315℃, which is 15-30℃ higher than that of commercially available ester-based fire-resistant hydraulic oils. The product of this invention is safer to use and is biodegradable. Detailed Implementation

[0019] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0020] Example 1

[0021] The specific steps for preparing the homemade antioxidant component are as follows:

[0022] 2,2'-methylenebis-(4-methyl-6-tert-butylphenol) and phosphorus oxychloride were added to a reaction vessel and reacted at room temperature for 1 hour. Then, p-methyl-m-hydroxydiphenylamine was added dropwise. The molar ratio of 2,2'-methylenebis-(4-methyl-6-tert-butylphenol), phosphorus oxychloride and p-methyl-m-hydroxydiphenylamine was 2:1:1. The temperature was raised to 80°C and reacted for 3 hours. The HCl gas generated by the reaction was absorbed by sodium hydroxide alkaline solution, and the mixture was washed with water to obtain the self-made antioxidant component.

[0023] Examples 2-5 and Comparative Examples 1-4

[0024] The specific steps for preparing hydraulic oil are as follows:

[0025] According to the formula in the table below, the base oil and antioxidant components are fully dissolved at 80°C. Then, anti-wear agent, metal deactivator and rust inhibitor are added, and the mixture is stirred and mixed thoroughly at 50°C for 0.5 hours to obtain long-life, high flash point ester-type fire-resistant hydraulic oil.

[0026] The specific formula is shown in the table below:

[0027]

[0028]

[0029] The hydraulic oils prepared according to the above formulas in Examples 2-3 and Comparative Examples 1-4 were subjected to performance tests, and the test results are shown in Table 1 below:

[0030] Table 1. Hydraulic oil performance test results for Examples 2-3 and Comparative Examples 1-4

[0031]

[0032] As shown in the table above, the hydraulic oil prepared according to the embodiments of the present invention has a high flash point and excellent oxidation stability, which is superior to that of commercially available phenol-amine oils used alone or in combination. Furthermore, the self-made antioxidant component of the present invention does not affect the flash point of the base oil, enabling the product to reach a flash point of over 315℃, with a maximum of 323℃, which is 15-30℃ higher than the flash point of commercially available ester-type fire-resistant hydraulic oils.

[0033] The hydraulic oil prepared according to the embodiments of the present invention has a longer service life and a longer oil change cycle, which can greatly save costs.

[0034] In the description of this specification, the references to terms such as "an embodiment," "example," "specific example," etc., indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of the present invention. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples.

[0035] The above description is merely an example and illustration of the present invention. Those skilled in the art can make various modifications or additions to the specific embodiments described, or use similar methods to replace them, as long as they do not deviate from the invention or exceed the scope defined in the claims, all of which should fall within the protection scope of the present invention.

Claims

1. A method for preparing a long-life, high-flash-point ester-type fire-resistant hydraulic oil, characterized in that, Includes the following steps: Dissolve 98-99% base oil and 0.5-1.4% self-made antioxidant components at 80°C, then add 0.2-0.5% anti-wear agent, 0.05-0.15% metal deactivator, and 0.05-0.15% rust inhibitor. Stir and mix thoroughly at 50°C for 0.5 hours to obtain a long-life, high flash point ester-type fire-resistant hydraulic oil. The self-made antioxidant component is prepared through the following steps: 2,2'-methylenebis-(4-methyl-6-tert-butylphenol) and phosphorus oxychloride were added to the reaction vessel and reacted at room temperature for 1 hour. Then p-methyl-m-hydroxydiphenylamine was added and the temperature was raised to 80°C for 1-5 hours. The HCl gas generated by the reaction was absorbed by the alkaline solution and washed with water to obtain the self-made antioxidant component. The base oil is an unsaturated polyol ester.

2. The preparation method of the long-life, high-flash-point ester-type fire-resistant hydraulic oil according to claim 1, characterized in that, 98.4% base oil and 1% self-made antioxidant components were fully dissolved at 80°C. Then, 0.4% anti-wear agent, 0.1% metal deactivator, and 0.1% rust inhibitor were added. The mixture was stirred and mixed thoroughly at 50°C for 0.5 hours to obtain a long-life, high-flash-point ester-type fire-resistant hydraulic oil.

3. The preparation method of the long-life, high-flash-point ester-type fire-resistant hydraulic oil according to claim 1, characterized in that, The molar ratio of 2,2'-methylenebis-(4-methyl-6-tert-butylphenol): phosphorus oxychloride: p-methyl-m-hydroxydiphenylamine in the preparation steps of the self-made antioxidant component is 1-2:1:1-2.

4. The preparation method of the long-life, high-flash-point ester-type fire-resistant hydraulic oil according to claim 1, characterized in that, The anti-wear agent is one or both of BASF 349 and BASF 353.

5. The method for preparing long-life, high-flash-point ester-type fire-resistant hydraulic oil according to claim 1, characterized in that, The metal deactivator is one or more of T551, T553 and T561.

6. The method for preparing long-life, high-flash-point ester-type fire-resistant hydraulic oil according to claim 1, characterized in that, The rust inhibitor is 5-methylbenztriazole.

Citation Information

Patent Citations

  • Stabilized lubricant compositions

    CN101065468A

  • Synthetic ester type fire resistant hydraulic oil

    CN109439404A