Environment-friendly stamping oil and preparation method thereof

Abstract

The invention relates to the field of stamping oil, in particular to environment-friendly stamping oil and a preparation method thereof.The environment-friendly stamping oil is composed of isoparaffin solvent oil, a lubrication enhancer and an extreme pressure anti-wear agent; wherein the extreme pressure anti-wear agent is chlorinated paraffin loaded phosphate type ionic liquid, the environment-friendly stamping oil has excellent use performance, workpiece scratches can be effectively reduced, a mold can be protected, and under extreme high pressure, the oil product can still keep lubrication and prevent sintering.

Description

Technical Field

[0001] This invention relates to the field of super oilstone technology, specifically to an environmentally friendly stamping oil and its preparation method. Background Technology

[0002] Stamping is a type of metal forming, a method of machining parts with specific geometric dimensions, shapes, and properties by applying external force to sheet metal using dies to separate or plastically deform it. It is commonly referred to as sheet metal stamping or sheet metal forming. Stamping has a wide range of applications, from blanking and stamping of different materials (cast iron, aluminum, stainless steel, alloy steel, and even non-metallic materials) and thicknesses in various steel rolling mills. The stamping process offers advantages over other processes in terms of part shape, dimensional accuracy, mechanical strength, production efficiency, and material utilization, making it one of the most important plastic forming methods.

[0003] In stamping processes, the quality of stamping oil and its proper use are crucial to the success or failure of the processing, as well as product quality, mold life, production efficiency, and the smooth operation of subsequent processes. Currently, stamping oils on the market generally suffer from high toxicity, poor stability, and inadequate load-bearing capacity. Summary of the Invention

[0004] Purpose of the invention: To address the above-mentioned technical problems, this invention proposes an environmentally friendly stamping oil and its preparation method.

[0005] The technical solution adopted is as follows: An environmentally friendly stamping oil, composed of isoparaffin solvent oil, lubricant enhancer and extreme pressure anti-wear agent; The extreme pressure anti-wear agent is a chlorinated paraffin-supported phosphate ester type ionic liquid.

[0006] Furthermore, the extreme pressure anti-wear agent is made from chlorinated paraffin, tri-n-octylphosphine, and sodium phosphate salt.

[0007] Furthermore, the structural formula of the sodium phosphate salt is as follows: Among them, R1 and R2 may be the same or different, and each is an independent hydrocarbon group.

[0008] Furthermore, the hydrocarbon group is a straight-chain or branched alkyl group with ≤10 carbon atoms.

[0009] Furthermore, R1 and R2 are the same.

[0010] Furthermore, both R1 and R2 are isopentyl groups.

[0011] Furthermore, the preparation method of the extreme pressure anti-wear agent is as follows: Tri-n-octylphosphine and chlorinated paraffin are added to an organic solvent, heated to react, cooled to room temperature, and then sodium phosphate salt is added. After the reaction continues, the organic solvent is evaporated, and the crude product is purified and dried.

[0012] Furthermore, the mass ratio of the isoparaffin solvent oil, lubricant enhancer, and extreme pressure anti-wear agent is 1:10%-20%:1-3%.

[0013] Furthermore, the lubricant enhancer is composed of tetrameric castor oil ester and pentaerythritol stearate in a mass ratio of 1-9:1-9.

[0014] This invention also provides a method for preparing an environmentally friendly stamping oil: Add isoparaffin solvent oil, lubricant enhancer and extreme pressure anti-wear agent to a stirred tank, maintain the temperature at 30-50℃, stir evenly and then filter.

[0015] The beneficial effects of this invention are: This invention provides an environmentally friendly stamping oil. The isoparaffin solvent oil has good thermal oxidation stability, biodegradability and low-temperature fluidity, and low skin irritation and toxicity, and will not harm the environment and human health. Both tetrameric castor oil ester and pentaerythritol stearate are high-performance lubricant enhancers. Their combination improves the lubrication and extreme pressure performance of stamping oil, while also providing some rust prevention. The chlorinated paraffin in the extreme pressure anti-wear agent readily decomposes at high temperatures, and the resulting chloride ions react chemically with the metal surface to form a lubricating protective film, thus providing anti-wear and extreme pressure protection. This invention introduces a phosphate ester-type ionic liquid into the chlorinated paraffin molecular chain through molecular structure design. The active element phosphorus reacts during friction to form a boundary lubricating film, improving the friction reduction, anti-wear performance, and extreme pressure carrying capacity of the stamping oil. The strongly polar ester oxygen groups in the molecular structure can form a dense adsorption film on the metal surface, also exhibiting excellent anti-wear properties, effectively reducing friction and wear. This environmentally friendly stamping oil exhibits excellent performance, effectively reducing workpiece scratches, protecting molds, and maintaining lubrication even under extreme pressure, preventing sintering. Attached Figure Description

[0016] Figure 1 This is the reaction route diagram for S1 in Example 1.

[0017] Figure 2 This is the reaction route diagram for S2 in Example 1. Detailed Implementation

[0018] Unless otherwise specified in the examples, the conditions were performed under standard conditions or as recommended by the manufacturer. Reagents or instruments whose manufacturers are not specified are all commercially available products. Techniques not mentioned in this invention refer to existing technologies. Unless otherwise specified, the following examples and comparative examples are parallel experiments, using the same processing steps and parameters.

[0019] This invention provides an environmentally friendly stamping oil, which is composed of isoparaffin solvent oil, lubricant enhancer and extreme pressure anti-wear agent; The extreme pressure anti-wear agent is a chlorinated paraffin-supported phosphate ester type ionic liquid.

[0020] Isomerized alkane solvent oils possess excellent thermal oxidation stability, biodegradability, and low-temperature fluidity, and exhibit low skin irritation and toxicity, posing no harm to the environment or human health. Lubricant enhancers can improve the lubrication and extreme pressure performance of stamping oils. Chlorinated paraffin in extreme pressure anti-wear agents readily decomposes at high temperatures, and the resulting chloride ions can chemically react with the metal surface to form a lubricating protective film, thereby providing anti-wear and extreme pressure effects. Through molecular structure design, phosphate ester-type ionic liquids are introduced into the chlorinated paraffin molecular chain, where the active element phosphorus plays a crucial role in the tribochemical reaction. During friction, it reacts to form a boundary lubrication film, improving the friction-reducing, anti-wear performance, and extreme pressure carrying capacity of the stamping oil. The strongly polar ester oxygen groups in the molecular structure can form a dense adsorption film on the metal surface, also exhibiting excellent anti-wear properties, effectively reducing friction and wear.

[0021] The extreme pressure anti-wear agent is made of chlorinated paraffin, tri-n-octylphosphine and sodium phosphate.

[0022] Chlorinated paraffin is electrophilic, while tri-n-octylphosphine is nucleophilic. When heated, the two undergo a nucleophilic substitution reaction, in which tri-n-octylphosphine attacks the carbon-chlorine bond in chlorinated paraffin to generate tri-n-octylphosphine chloride. The tri-n-octylphosphine chloride then undergoes anion exchange with sodium phosphate salt to obtain the target product. In one embodiment of the present invention, the sodium phosphate salt has the following structural formula: Among them, R1 and R2 may be the same or different, and each is an independent hydrocarbon group.

[0023] Wherein, the hydrocarbon group is a straight-chain or branched alkyl group with ≤10 carbon atoms.

[0024] In one embodiment of the present invention, R1 and R2 are the same.

[0025] In one embodiment of the present invention, R1 and R2 are both isopentyl groups.

[0026] In one embodiment of the present invention, the structural formula of the sodium phosphate salt is as follows: The structural formula of the above sodium phosphate salt is as follows: Using toluene as a solvent, bis(hydroxymethyl)phosphonic acid, 4-methylvaleric acid and a catalyst were added, heated to reflux and then returned to room temperature. Saturated sodium carbonate solution was added dropwise to the reaction solution, and after standing, the mixture was filtered. The resulting solid was washed with ethanol to obtain sodium phosphate.

[0027] The preparation method of the extreme pressure anti-wear agent is as follows: Tri-n-octylphosphine and chlorinated paraffin are added to an organic solvent, heated to react, cooled to room temperature, and then sodium phosphate salt is added. After the reaction continues, the organic solvent is evaporated, and the crude product is purified and dried.

[0028] In one embodiment of the present invention, the mass ratio of the isoparaffin solvent oil, the lubricant enhancer and the extreme pressure anti-wear agent is 1:10%-20%:1-3%.

[0029] In one embodiment of the present invention, the mass ratio of the isoparaffin solvent oil, the lubricant enhancer and the extreme pressure anti-wear agent is 1:16%:2%.

[0030] In one embodiment of the present invention, the lubricant enhancer is composed of tetrameric castor oil ester and pentaerythritol stearate in a mass ratio of 1-9:1-9.

[0031] Both tetrameric castor oil ester and pentaerythritol stearate are high-performance lubricant enhancers. When combined, they can improve the lubrication and extreme pressure performance of stamping oil, and also have certain rust-preventive properties.

[0032] In one embodiment of the present invention, the lubricant enhancer is composed of tetrameric castor oil ester and pentaerythritol stearate in a mass ratio of 1:1.

[0033] This invention also provides a method for preparing an environmentally friendly stamping oil: Add isoparaffin solvent oil, lubricant enhancer and extreme pressure anti-wear agent to a stirred tank, maintain the temperature at 30-50℃, stir evenly and then filter.

[0034] Example 1: An environmentally friendly stamping oil is composed of isoparaffin solvent oil IP 95, tetrameric castor oil oleate, pentaerythritol stearate and extreme pressure anti-wear agent in a mass ratio of 1:8%:8%:2%. The extreme pressure anti-wear agent is a chlorinated paraffin-supported phosphate ester type ionic liquid, and its preparation method is as follows: S1: Using 500 ml toluene as solvent, 12.6 g of bis(hydroxymethyl)phosphonic acid (CAS: 2074-67-1), 23.23 g of 4-methylpentanoic acid (CAS: 646-07-1), and 0.5 ml of concentrated sulfuric acid were added. The mixture was stirred and heated to reflux for 5 h, then allowed to return to room temperature. 60 ml of saturated sodium carbonate solution was added dropwise to the reaction solution. After standing for 24 h, the mixture was filtered. The solid was washed with ethanol to obtain the sodium phosphate salt, with a yield of 66.3%. ESI-MS (m / z) (M + Theoretical value: 344.32, measured value: 344.17.

[0035] S2: Add 3.7g of tri-n-octylphosphine (CAS:4731-53-7) and 20g of chlorinated paraffin to a mixed solvent consisting of 100ml of acetonitrile and 100ml of ethanol. Heat to 75℃ and react for 24h. Then cool to room temperature. Add 3.44g of the above sodium phosphate salt and continue stirring for 12h. Remove the organic solvent by vacuum distillation. Dissolve the crude product in 200ml of petroleum ether and filter to remove the precipitated sodium chloride. Distill the filtrate again under vacuum.

[0036] The preparation method of the above-mentioned environmentally friendly stamping oil is as follows: Add isoparaffin solvent oil IP 95, tetrameric castor oil ester, pentaerythritol stearate and extreme pressure anti-wear agent to a stirred tank, maintain the temperature at 40±5℃, stir for 60 minutes to make uniform, and then filter.

[0037] Example 2: An environmentally friendly stamping oil is composed of isoparaffin solvent oil IP 95, tetrameric castor oil oleate, pentaerythritol stearate and extreme pressure anti-wear agent in a mass ratio of 1:10%:10%:3%. The extreme pressure anti-wear agent is a chlorinated paraffin-supported phosphate ester type ionic liquid, and the preparation method is the same as in Example 1.

[0038] The preparation method of the above-mentioned environmentally friendly stamping oil is as follows: Add isoparaffin solvent oil IP 95, tetrameric castor oil ester, pentaerythritol stearate and extreme pressure anti-wear agent to a stirred tank, maintain the temperature at 40±5℃, stir for 60 minutes to make uniform, and then filter.

[0039] Example 3: An environmentally friendly stamping oil is composed of isoparaffin solvent oil IP 95, tetrameric castor oil oleate, pentaerythritol stearate and extreme pressure anti-wear agent in a mass ratio of 1:5%:5%:1%. The extreme pressure anti-wear agent is a chlorinated paraffin-supported phosphate ester type ionic liquid, and the preparation method is the same as in Example 1.

[0040] The preparation method of the above-mentioned environmentally friendly stamping oil is as follows: Add isoparaffin solvent oil IP 95, tetrameric castor oil ester, pentaerythritol stearate and extreme pressure anti-wear agent to a stirred tank, maintain the temperature at 40±5℃, stir for 60 minutes to make uniform, and then filter.

[0041] Comparative Example 1: It is basically the same as Example 1, except that tetrameric castor oil ester is used instead of pentaerythritol stearate.

[0042] Comparative Example 2: It is basically the same as Example 1, except that pentaerythritol stearate is used instead of tetrameric castor oil ester.

[0043] Comparative Example 3: It is basically the same as Example 1, except that no extreme pressure anti-wear agent is added.

[0044] Comparative Example 4: The method is basically the same as in Example 1, except that a commercially available extreme pressure anti-wear agent (BASF extreme pressure anti-wear agent IRGALUBETPPT) is used instead of the self-made extreme pressure anti-wear agent.

[0045] Performance testing: The environmentally friendly stamping oils prepared in Examples 1-3 and Comparative Examples 1-4 of this invention were used as samples for performance testing.

[0046] The wear resistance test of the formulated environmentally friendly aluminum fin stamping oil was conducted using the test method of GB / T 3142-2019. PB: Maximum non-seize load, the highest load under test conditions that does not cause seize, representing the oil film strength. PD: Sintering load, the lowest load under test conditions that causes the steel ball to sinter, representing the ultimate working capacity of the lubricant. Steel ball technical specifications: The GCr15 steel balls used in the test were from the same manufacturer and batch, meeting the GB / T 308.1-2013 standard, with a diameter of 12.7 mm and a hardness of HRC 61-66.

[0047] The test results are shown in Table 1 below: The PB value (maximum non-seize load) refers to the highest load that a lubricant can withstand under four-ball test conditions without the steel balls seizing (no significant wear). It represents the oil film strength of the oil, that is, its ability to form an effective lubricating film under boundary lubrication conditions.

[0048] Wear scar diameter is a core indicator for measuring wear resistance. The smaller the value, the stronger the oil film protection ability, which can effectively reduce direct friction and wear on the surface of the mold and the workpiece, thereby extending the service life.

[0049] The lower the coefficient of friction of stamping oil, the better, because a low coefficient of friction can significantly reduce frictional resistance, reduce wear on molds and workpieces, and extend service life.

[0050] PD value (sintering load) refers to the minimum load at which steel balls sinter at high temperatures due to excessive load under test conditions, as the load continues to increase. It represents the ultimate working capacity of the oil, that is, the failure point of the lubricant under extreme pressure conditions.

[0051] As shown in Table 1 above, the environmentally friendly stamping oil of the present invention has excellent performance, effectively reduces workpiece scratches, protects the mold, and can still maintain lubrication and prevent sintering under extreme high pressure.

[0052] The above embodiments are only used to illustrate the technical solutions of the present invention, and are not intended to limit it. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. An environmentally friendly stamping oil, characterized in that, It is composed of isoparaffinic solvent oil, lubricant enhancer, and extreme pressure anti-wear agent; The extreme pressure anti-wear agent is a chlorinated paraffin-supported phosphate ester type ionic liquid.

2. The environmentally friendly stamping oil as described in claim 1, characterized in that, The extreme pressure anti-wear agent is made of chlorinated paraffin, tri-n-octylphosphine and sodium phosphate.

3. The environmentally friendly stamping oil as described in claim 2, characterized in that, The structural formula of the sodium phosphate salt is as follows: Among them, R1 and R2 may be the same or different, and each is an independent hydrocarbon group.

4. The environmentally friendly stamping oil as described in claim 3, characterized in that, The hydrocarbon group is a straight-chain or branched alkyl group with ≤10 carbon atoms.

5. The environmentally friendly stamping oil as described in claim 4, characterized in that, R1 and R2 are the same.

6. The environmentally friendly stamping oil as described in claim 2, characterized in that, Both R1 and R2 are isopentyl groups.

7. The environmentally friendly stamping oil as described in claim 2, characterized in that, The preparation method of the extreme pressure anti-wear agent is as follows: Tri-n-octylphosphine and chlorinated paraffin were added to an organic solvent, heated to react, cooled to room temperature, and then sodium phosphate salt was added. After the reaction continued, the organic solvent was evaporated, and the crude product was purified and dried.

8. The environmentally friendly stamping oil as described in claim 1, characterized in that, The mass ratio of the isoparaffin solvent oil, lubricant enhancer, and extreme pressure anti-wear agent is 1:10%-20%:1-3%.

9. The environmentally friendly stamping oil as described in claim 1, characterized in that, The lubricant enhancer is composed of tetrameric castor oil ester and pentaerythritol stearate in a mass ratio of 1-9:1-9.

10. A method for preparing an environmentally friendly stamping oil as described in any one of claims 1-9, characterized in that, Add isoparaffin solvent oil, lubricant enhancer and extreme pressure anti-wear agent to a stirred tank, maintain the temperature at 30-50℃, stir evenly and then filter.

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