A preparation method of phosphated polyester lubricant

By preparing phosphated polyester lubricant as an additive for titanium alloy cutting fluid, the problems of wear and short tool life during titanium alloy processing are solved, and the lubricating performance and tool service life are significantly improved.

CN119751828APending Publication Date: 2025-04-04NANJING KERUN LUBRICANTS +2
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Patent Information

Application Number
CN202411966025.7
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-30
Publication Date
2025-04-04

AI Technical Summary

Technical Problem

During the mechanical processing, titanium alloys have problems such as poor thermal conductivity, large elastic deformation, large chemical activity and strong affinity, which leads to high processing difficulty, and often have problems such as hardening of processing surfaces, wear, accumulation and short tool life.

Method used

By preparing a phosphated polyester lubricant, it is added to the titanium alloy cutting fluid as a lubricating additive, and is added to the titanium alloy cutting fluid to improve its lubricating performance. The lubricant has better oil film strength and friction resistance by reacting fatty alcohol polyoxyethylene ether and tetrapolymer ricinoleate with phosphorus pentoxide at high temperature and hydrolyzing it.

Benefits of technology

It significantly improves the lubricating performance of titanium alloy cutting fluid, reduces wear of titanium alloy workpieces, extends the service life of cutting tools, and extends the service life of the tool by at least 33%.

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Abstract

The invention discloses a method for preparing a phosphated polyester lubricant, comprising the following steps: (1) mixing fatty alcohol polyoxyethylene ether and tetrapolyricinoleate, slowly adding phosphorus pentoxide to the mixture at high temperature for reaction, and adding distilled water thereto for hydrolysis after the reaction; (2) cooling to room temperature after the hydrolysis, separating the oil phase and the water phase, and obtaining the phosphated polyester lubricant. The phosphated polyester lubricant prepared by the invention can be added to a titanium alloy cutting fluid to significantly enhance its lubrication performance, thereby greatly improving the processing performance of the titanium alloy cutting fluid and extending the service life of the tool.
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Description

Technical Field

[0001] The invention relates to a method for preparing a phosphating polyester lubricant. Background Art

[0002] Titanium alloys have the characteristics of high specific strength, good heat resistance, strong corrosion resistance, good low temperature performance and good biocompatibility. Therefore, they are widely used in aerospace, medical, automotive industry, electronic equipment, chemical industry and marine engineering. In the field of aerospace, titanium alloys are important structural materials and can be used to manufacture aircraft engine components, frames, skins, fasteners and landing gear, etc., which can effectively reduce the weight of aircraft and enhance structural strength and reliability. In the medical field, titanium alloys are often used to manufacture medical devices and implants such as artificial joints, fracture fixation plates, dental implants, and spinal implants. With its good biocompatibility, high strength and strong corrosion resistance, it helps patients recover their health and improve their quality of life. In the automotive industry, titanium alloys are used in automobile engine systems, such as manufacturing engine parts such as titanium valve springs, which can reduce the inertial mass of moving parts, increase free vibration, reduce the vibration of the car body, and increase the engine speed and output power. In the field of electronic equipment, titanium alloys are used to make mobile phone middle frames, hinges, camera rings and other parts. With its high strength and low density, it can reduce the thickness and weight of mobile phones and improve the overall structural strength. In the fields of chemical industry and marine engineering, titanium alloys are widely used in chemical equipment, seawater desalination equipment, offshore platforms, etc. They can resist the erosion of corrosive media such as acids, alkalis, and salts, and extend the service life of the equipment.

[0003] Due to the disadvantages of poor heat conduction, large elastic deformation, high chemical activity and strong affinity in the machining process of titanium alloy, it is difficult to process and often has problems such as surface hardening, wear, chip accumulation and short tool life. The above problems can be overcome by improving the lubricity of cutting fluid, so it is necessary to develop a special additive that can improve the lubricity of titanium alloy cutting fluid. Summary of the invention

[0004] Purpose of the invention: The purpose of the present invention is to provide a method for preparing a phosphated polyester lubricant. The phosphated polyester lubricant prepared by the method is added to a titanium alloy cutting fluid as a lubricating additive, which can greatly improve the lubrication performance of the titanium alloy cutting fluid. On the one hand, it can greatly reduce the wear problem of the titanium alloy workpiece during the processing, and on the other hand, it can greatly extend the service life of the cutting tool, so that the service life of the tool can be extended by at least 33%.

[0005] Technical solution: The preparation method of the phosphated polyester lubricant of the present invention comprises the following steps:

[0006] (1) mixing fatty alcohol polyoxyethylene ether and tetrapolyricinoleate, slowly adding phosphorus pentoxide to the mixture at high temperature for reaction, and adding distilled water to the mixture for hydrolysis after the reaction. Adding distilled water can hydrolyze free by-products. The hydrolysis of by-products can improve the product yield and reduce the content of free acid;

[0007] (2) After hydrolysis, the mixture is cooled to room temperature, and the oil phase and the water phase are separated to obtain a phosphated polyester lubricant.

[0008] Wherein, in step (2), the monoester content of the obtained phosphated polyester lubricant is 54-58wt.%, and the diester content is 35-40wt.%.

[0009] Wherein, in step (1), the fatty alcohol polyoxyethylene ether is an isomeric decanol polyoxyethylene ether polyoxypropylene ether block polymer, and its molecular structure is: R-(EO) n -(PO) m -(EO)o-OH, wherein n=3, m=4, o=2.

[0010] The product model of the isomeric decanol polyoxyethylene ether polyoxypropylene ether block polymer is SURFALINEOX 10M08.

[0011] Wherein, in step (1), the added mass ratio of fatty alcohol polyoxyethylene ether, tetrapolyricinoleate and phosphorus pentoxide (P2O5) is 1.5-2.0:0.5-1.0:1.0.

[0012] Wherein, in step (1), the reaction temperature is 60-75°C, preferably 65-70°C, and the reaction time is 3-3.5h. If the reaction temperature is too high, the reaction product will decompose and all monoester compounds will be generated.

[0013] Wherein, in step (1), the amount of distilled water added is 3-5% of the total mass of the reaction materials (the total amount of fatty alcohol polyoxyethylene ether, tetrapolyricinoleate and phosphorus pentoxide added).

[0014] Wherein, in step (1), the hydrolysis temperature is 60-70° C. and the hydrolysis time is 1-2 h.

[0015] The above-mentioned phosphated polyester lubricant is used as a lubricating additive for titanium alloy cutting fluid.

[0016] Wherein, in the titanium alloy cutting fluid, the added amount of the phosphated polyester lubricant is 3-6% of the mass of the titanium alloy cutting fluid.

[0017] The phosphate group in the phosphated polyester lubricant of the present invention is adsorbed on the surface of the titanium alloy through chemical bonds, and a hydrophobic group is polymerized at the other end, thereby having better oil film strength and anti-friction ability.

[0018] Beneficial effects: Compared with the prior art, the present invention has the following significant advantages: the phosphated polyester lubricant prepared by the present invention can be added to the titanium alloy cutting fluid to significantly enhance its lubrication performance, especially for the face milling and side washing processes of titanium alloys, the lubrication effect can be significantly enhanced, thereby improving the processing performance of the titanium alloy cutting fluid and extending the service life of the tool. DETAILED DESCRIPTION

[0019] Example 1

[0020] The preparation method of the phosphated polyester lubricant of the present invention comprises the following steps:

[0021] (1) Add 56 g of SURFALINE OX 10M08 and 14 g of tetrapolyricinoleate into a reaction container, stir and mix evenly, raise the temperature to 65° C., slowly add 28 g of phosphorus pentoxide (P2O5) thereto, and react for 3 hours; then add 4.9 g of distilled water thereto, and hydrolyze at 65° C. for 1 hour;

[0022] (2) After cooling to room temperature, the water at the bottom of the reaction vessel is separated (the water phase and the oil phase are separated) to obtain a phosphated polyester lubricant. The phosphated polyester lubricant has a monoester content of 58 wt.% and a diester content of 35 wt.%.

[0023] 3 g of the phosphated polyester lubricant prepared in Example 1 was added to 97 g of a semi-synthetic cutting fluid (the product model of the semi-synthetic cutting fluid is Kerun KR-C8028), and stirred until completely dissolved; then diluted with pure water to a working fluid with a mass concentration of 8%.

[0024] The lubrication performance of the cutting fluid obtained in Example 1 was measured:

[0025] Milling processing was carried out on a machine tool, the material was TC4, the hardness was 35HRC, the lubricating and cooling medium was 8wt.% of a semi-synthetic cutting fluid (without adding a phosphated polyester lubricant) (A) and the working fluid of Example 1 with 8wt.% of a semi-synthetic cutting fluid added with a phosphated polyester lubricant (B).

[0026] Face milling: cutting speed 75m / min, rotation speed 3980r / min, feed speed 995mm / min;

[0027] Side milling: cutting speed 150m / min, rotation speed 8000r / min, feed speed 3640mm / min; the processing results of the two are shown in Table 1.

[0028] Table 1

[0029] Cutting fluid Face milling tool life (m) Side milling tool life (m) A 40 61 B 62 99

[0030] It can be seen from Table 1 that compared with the semi-synthetic cutting fluid base fluid, after adding phosphating polyester lubricant, the face milling tool life is increased by about 55%, and the side milling tool life is increased by about 62%.

[0031] Example 2

[0032] The preparation method of the phosphated polyester lubricant of the present invention comprises the following steps:

[0033] (1) Add 42 g of SURFALINE OX 10M08 and 28 g of tetrapolyricinoleate to a reaction container, stir and mix evenly, raise the temperature to 70° C., slowly add 28 g of phosphorus pentoxide (P2O5) thereto, and react for 3.5 hours; then add 3.9 g of distilled water thereto, and hydrolyze at 70° C. for 2 hours;

[0034] (2) After cooling to room temperature, the water at the bottom of the reaction container is separated (the water phase and the oil phase are separated) to obtain a phosphated polyester lubricant. The phosphated polyester lubricant has a monoester content of 54 wt.% and a diester content of 40 wt.%.

[0035] 6 g of the phosphated polyester lubricant prepared in Example 2 was added to 94 g of a fully synthetic cutting fluid base fluid (the product model of the fully synthetic cutting fluid base fluid is Kerun KR-C9060), and stirred until completely dissolved; then diluted with pure water to a working fluid with a mass concentration of 8%.

[0036] The lubrication performance of the cutting fluid obtained in Example 2 was measured:

[0037] Milling processing was carried out on a machine tool, the material was TC4, the hardness was 35HRC, the lubricating and cooling medium was 8wt.% of a fully synthetic cutting fluid (without adding a phosphated polyester lubricant) (C) and the working fluid of Example 2 with 8wt.% of a fully synthetic cutting fluid added with a phosphated polyester lubricant (D).

[0038] Face milling: cutting speed 75m / min, rotation speed 3980r / min, feed speed 995mm / min;

[0039] Side milling: cutting speed 150m / min, rotation speed 8000r / min, feed speed 3640mm / min; the processing results of the two are shown in Table 2.

[0040] Table 2

[0041] Cutting fluid Face milling tool life (m) Side milling tool life (m) C 40 45 D 55 60

[0042] It can be seen from Table 2 that compared with the fully synthetic cutting fluid base fluid, after adding phosphating polyester lubricant, the face milling tool life is increased by about 37.5%, and the side milling tool life is increased by about 33%.

[0043] Comparative Example 1

[0044] A method for preparing a phosphated polyester lubricant comprises the following steps:

[0045] (1) Add 60 g of SURFALINE OX 10M08 and 20 g of tetrapolyricinoleate into a reaction container, stir and mix evenly, raise the temperature to 70° C., slowly add 20 g of phosphorus pentoxide (P2O5) thereto, and react for 4 hours; then add 4.0 g of distilled water thereto, and hydrolyze at 70° C. for 2 hours;

[0046] (2) After cooling to room temperature, the water at the bottom of the reaction vessel is separated (the water phase and the oil phase are separated) to obtain a phosphated polyester lubricant, in which the monoester content is 36 wt.%, and the diester content is 58 wt.%. At this time, the diester ratio in the phosphated polyester lubricant is greatly increased, so that its solubility in the cutting fluid becomes poor and it cannot be effectively dissolved in the cutting fluid base liquid.

[0047] Comparative Example 2

[0048] A method for preparing a phosphated polyester lubricant comprises the following steps:

[0049] (1) Add 56 g of SURFALINE OX 10M08 and 14 g of tetrapolyricinoleate into a reaction container, stir and mix evenly, raise the temperature to 80° C., slowly add 28 g of phosphorus pentoxide (P2O5) thereto, and react for 4 hours; then add 4.9 g of distilled water thereto, and hydrolyze at 65° C. for 1 hour;

[0050] (2) After cooling to room temperature, the water at the bottom of the reaction vessel is separated (the water phase and the oil phase are separated) to obtain a phosphated polyester lubricant and an olefin mixture, and the product color is deepened. The phosphated polyester lubricant obtained has a monoester content of 51% and a diester content of 30%.

[0051] 3 g of the phosphated polyester lubricant prepared in Comparative Example 2 was added to 97 g of a semi-synthetic cutting fluid (the product model of the semi-synthetic cutting fluid is Kerun KR-C8028), and stirred until completely dissolved; then diluted with pure water to a working fluid with a mass concentration of 8%.

[0052] The lubrication performance of the cutting fluid obtained in Comparative Example 2 was measured:

[0053] Milling processing was carried out on a machine tool, the material was TC4, the hardness was 35HRC, the lubricating and cooling medium was 8wt.% of a semi-synthetic cutting fluid (without adding a phosphated polyester lubricant) (A) and the comparative example 2 with 8wt.% of a semi-synthetic cutting fluid added with a phosphated polyester lubricant (E).

[0054] Face milling: cutting speed 75m / min, rotation speed 3980r / min, feed speed 995mm / min;

[0055] Side milling: cutting speed 150m / min, rotation speed 8000r / min, feed speed 3640mm / min;

[0056] The processing results of the two are shown in Table 3.

[0057] Table 3

[0058] Cutting fluid Face milling tool life (m) Side milling tool life (m) A 40 61 E 53 82

[0059] Comparative Example 3

[0060] A method for preparing a phosphated polyester lubricant comprises the following steps:

[0061] (1) Add 56 g of SURFALINE OX 10M08 and 14 g of tetrapolyricinoleate into a reaction vessel, stir and mix evenly, raise the temperature to 65° C., slowly add 28 g of phosphorus pentoxide (P2O5), react for 3 hours, and stop heating;

[0062] (2) After cooling to room temperature, the water at the bottom of the reaction container is separated (the water phase and the oil phase are separated) to obtain a phosphated polyester lubricant. The phosphated polyester lubricant has a monoester content of 53% and a diester content of 32%.

[0063] 3 g of the phosphated polyester lubricant prepared in Comparative Example 3 was added to 97 g of a semi-synthetic cutting fluid (the product model of the semi-synthetic cutting fluid is Kerun KR-C8028), and stirred until completely dissolved; then diluted with pure water to a working fluid with a mass concentration of 8%.

[0064] The lubrication performance of the cutting fluid obtained in Comparative Example 3 was measured:

[0065] Milling processing was carried out on a machine tool, the material was TC4, the hardness was 35HRC, the lubricating and cooling medium was 8wt.% of a semi-synthetic cutting fluid (without adding a phosphated polyester lubricant) (A) and the comparative example 3 with 8wt.% of a semi-synthetic cutting fluid added with a phosphated polyester lubricant (F).

[0066] Face milling: cutting speed 75m / min, rotation speed 3980r / min, feed speed 995mm / min;

[0067] Side milling: cutting speed 150m / min, rotation speed 8000r / min, feed speed 3640mm / min;

[0068] The processing results of the two are shown in Table 4.

[0069] Table 4

[0070] Cutting fluid Face milling tool life (m) Side milling tool life (m) A 40 61 F 55 89 。

Claims

1. A method for preparing a phosphated polyester lubricant, characterized in that: The steps include: (1) mixing fatty alcohol polyoxyethylene ether and tetrapolyricinoleate, slowly adding phosphorus pentoxide to the mixture at high temperature for reaction, and adding distilled water to the mixture for hydrolysis after the reaction; (2) After hydrolysis, the mixture is cooled to room temperature, and the oil phase and the water phase are separated to obtain a phosphated polyester lubricant.

2. The preparation method according to claim 1, characterized in that: In step (1), the fatty alcohol polyoxyethylene ether is an isomeric decanol polyoxyethylene ether polyoxypropylene ether block polymer, and its molecular structure is: R-(EO) n -(PO) m -(EO)o-OH, wherein n=3, m=4, o=2.

3. The preparation method according to claim 1, characterized in that: In step (1), the mass ratio of the fatty alcohol polyoxyethylene ether, tetrapolyricinoleate and phosphorus pentoxide added is 1.5-2.0:0.5-1.0:1.

0.

4. The preparation method according to claim 1, characterized in that: In step (1), the reaction temperature is 60-75° C. and the reaction time is 3-3.5 h.

5. The preparation method according to claim 1, characterized in that: In step (1), the amount of distilled water added is 3-5% of the total mass of the reaction materials.

6. The preparation method according to claim 1, characterized in that: In step (1), the hydrolysis temperature is 60-70° C. and the hydrolysis time is 1-2 h.

7. The preparation method according to claim 1, characterized in that: In step (2), the phosphated polyester lubricant obtained has a diester content of 54-58 wt.%, and a monoester content of 35-40 wt.%.

8. Use of the phosphated polyester lubricant prepared by the preparation method according to claim 1 as a lubricating additive for titanium alloy cutting fluid.

9. The use according to claim 8, characterized in that: In the titanium alloy cutting fluid, the added amount of the phosphating polyester lubricant is 3-6% of the mass of the titanium alloy cutting fluid.