JPS6322238B2 - - Google Patents

Description

[Detailed description of the invention]

[Field of Application of the Invention] The present invention provides a high-quality steel that can be processed by simply applying lubricating oil to the surface of the steel material or by supplying it with an automatic lubrication device or the like during processing, without requiring chemical conversion treatment on the surface of the steel material subjected to cold working. The present invention relates to a high performance lubricating oil composition for plastic working. [Prior art] Conventionally, as cold working lubricating oil used when drawing, upsetting, forward extraction, and backward extraction processing of steel materials, machining oil is a mixture of mineral oil and ester oil, and the above mixed oil is mixed with wax, dichloromethane, etc. There are processing oils that contain extreme pressure agents such as molybdenum sulfide, graphite, metallic soap, sulfur compounds, phosphorus compounds, and chlorine compounds.
These machining oils are applied to the surface of the steel material or supplied to the machining section using an oil supply device or the like for machining. These processing oils can be adequately applied to molded products with a low degree of workability or small plastic deformation, but when producing molded products with a high degree of workability or large plastic deformation, the oil film strength of the lubricating oil, that is, the resistance Galling and seizure occur due to insufficient loadability and insufficient introduction of solid lubricant to friction surfaces. In addition to the above methods, when processing highly processed molded products or molded products with complex shapes that undergo large plastic deformation, there is a method of coating the surface of the steel material with a lubricating film. Examples of such materials include polyvinyl chloride, nylon, polyethylene chlorosulfonate, a mixture of polysulfide and polyvinyl chloride, and a mixture of graphite fluoride and polyimide. There are also methods of coating the steel surface with a thin film of soft metal such as copper or lead by plating or other methods, but these have drawbacks in workability and finishing accuracy of the molded product surface, and furthermore, it is difficult to remove the film. There are some drawbacks. On the other hand, chemical conversion treatment with a phosphate coating is widely used as a lubricant for cold working steel materials.
Pre-treatment conditions for steel materials, management status of treatment liquid, control of chemical reactions, etc. have a large influence on the formation of lubricating films, and due to the complexity of the treatment process and the pollution problem of waste liquid, high-performance alternatives to phosphate film treatment have been recommended. High performance lubricants are required. After conducting various studies to meet the above-mentioned demands, the present inventors have already proposed a high-performance lubricating oil in which an organic phosphorus compound is blended into an oil based on synthetic oil or a mixture thereof. However, among these organic phosphorus compounds, some of the organic phosphorus compounds whose hydrocarbon number is 6 or less are insoluble in the oil, and some of them cause two-phase separation at an early stage. If lubricating oil is applied to the steel surface using an automatic oil supply device or a roller brush in a two-phase separated state, the organic phosphorus compound will be consumed prematurely and the additive will not be effective, causing seizure.
Therefore, there is a drawback that a stirring device is required to prevent two-phase separation. [Object of the Invention] An object of the present invention is to provide a high-performance lubricating oil composition for metal processing that improves these drawbacks and further improves processing performance. [Summary of the Invention] The metal working lubricating oil composition of the present invention is particularly excellent for cold working. The features of the present invention are: (A) General formula [Wherein, R is a hydrocarbon group having 1 to 18 carbon atoms,
R' is hydrogen or a hydrocarbon group having 6 to 10 carbon atoms,
n is an integer of 1 to 3] 5 to 50% by weight of acidic phosphoric acid ester (B) Alkenyl succinimide dispersant 0.05 to 10% by weight based on component (A) above (C) Lubricating oil, organic solvent or water. In addition, when processing molded products with an extremely high degree of processing or molded products with complex shapes that undergo large plastic deformation, solid lubricants such as nylon, graphite fluoride, graphite, molybdenum disulfide, organic This objective can be achieved by incorporating a lubricant such as molybdenum. Examples of the organic phosphorus compound (A) listed in general formula (1) include diphenyl phosphite, diphenylnonylphenyl phosphite, dibutyl phosphite,
Phosphite esters such as diisodecyl phosphite, didodecyl phosphite, dioleyl phosphite, monobutyl phosphate, monoisodecyl phosphate, methyl acid phosphate, isopropyl acid phosphate, butyl acid phosphate, 2 -ethylhexyl acid phosphate, isodecyl acid phosphate,
At least one acidic phosphoric acid ester such as lauryl acid phosphate, tridecanol acid phosphate, octadecyl acid phosphate, oleyl acid phosphate, etc. is preferably contained in an amount of 1 to 50% by weight based on the total weight of the composition. is 5-30
It is preferable to use it in a proportion of % by weight. If the amount is less than 5% by weight, the effect of adding the organic phosphorus compound will be low, and the processing performance will not be sufficiently improved. On the other hand, even if it exceeds 50% by weight, the effect of addition does not improve significantly and it is not a good idea from a cost standpoint. Examples of the alkenyl succinimide dispersant (B) above include polybutenyl succinic anhydride obtained by maleating polybutene, and polybutenyl succinic anhydride obtained by reacting polybutenyl succinic anhydride with an amine. Imide, polybutenyl succinic ester obtained by reacting polybutenyl succinic anhydride with alcohol, or carbon having a C ₁₂ to _{C 20} linear or branched saturated or unsaturated hydrocarbon chain Acid amides made of acids, etc. are used. The alkenyl succinide dispersant used in the lubricating composition of the present invention is 0.05 to 10% by weight, preferably 0.1 to 5% by weight, based on the blended weight of the organic phosphorus compound.
It is preferable to use it in a proportion of % by weight. If it is less than 0.05% by weight, the dispersion effect is low and phase separation of the lubricating oil and the organic phosphorus compound occurs early. Moreover, if it exceeds 10% by weight, processing performance will deteriorate, which is undesirable. As the lubricating oil in (C) above, mineral oil or synthetic oil is used. Further, as the organic solvent, trichlorethylene, trichlorotrifluoroethylene, etc. are preferable. In addition to the above-mentioned components, the lubricating oil composition of the present invention may optionally contain an antioxidant to improve the thermal stability of the lubricating oil and a rust inhibitor to improve the rust-preventing ability of steel materials. It's okay. A lubricating oil made of the above composition is applied to the surface of a steel material, and if the surface roughness of the steel material is increased in order to improve the retention of the lubricating oil, the workability is further improved. However, if the surface roughness exceeds Hmax30~40μ, a satin pattern will remain on the surface of the molded product after processing.
This may be undesirable for applications where appearance is important. The method for applying lubricating oil to the steel surface is as follows:
There are methods such as dipping coating the steel material in the lubricating oil composition and spray coating. In addition, steel materials from 40 to
If a material preheated to 80°C is used, a lubricating film will be formed better, and the lubrication performance during cold working will be further improved. [Examples of the Invention] Next, Examples and Comparative Examples of the present invention will be given to explain the effects thereof. Example 1 Mineral oil with a viscosity of 60 mm ² /s at 40°C was used with the commercially available product name "OLOA 1200" (manufactured by Chevron Chemical Co., Ltd.) as an alkenyl succinimide-based product, and also with the commercially available product name as a polybutenyl succinate-based product. "Lubrizol 939" (manufactured by Nippon Librizol)
In addition, as an acid amide type, commercially available product name “OLOA
340D" (manufactured by Chevron Chemical Co., Ltd.) with the blended weight of monobutyl phosphate insoluble in mineral oil (20
After adding 0.02 to 20% by weight based on % by weight) and heating and dissolving, the above monobutyl phosphate was added and stirred to obtain an emulsified lubricating oil composition. A certain amount of this lubricating oil composition was taken into a graduated cylinder and allowed to stand, and the time required for phase separation to begin to occur, that is, the dispersion performance was measured. In addition, as a comparative example, no dispersant was used and 4% by weight of an emulsifier (sorbitan monooleate) used in lubricating oil was blended. As is clear from Table 1, the products containing the polyalkenyl succinide dispersant have better dispersibility than those of the comparative examples. Further, the dispersing ability becomes effective when the dispersant content is 0.05% by weight or more.

[Table] Example 2 After heating and dissolving 0.02 to 5.0% by weight of alkenyl succinate Lubrizol 939 (amount based on the added weight of the organic phosphorus compound) in the same mineral oil as in Example 1, an additive insoluble in mineral oil was prepared. 20% by weight of diphenyl phosphite, methyl acid phosphate, and isopropyl acid phosphate were added and stirred to obtain an emulsified lubricating oil composition. The dispersion performance of the dispersant was evaluated using the same method as in Example 1. The results are shown in Table 2. As is clear from Table 2, the dispersion performance is superior to that of the comparative example shown in Example 1.

[Table] Example 3 Addition of polybutenyl succinate ester to synthetic oil of polyα-olefin oil and polyol ester oil
Lubrizol 939 to the amount of organic phosphate added
After blending 0.02 to 20% by weight and heating and dissolving, 20% by weight of additive monobutyl phosphate was added and stirred to obtain an emulsified lubricating oil composition. The dispersion performance of this lubricating oil composition was measured in the same manner as in Example 1. The results are shown in Table 3. As is clear from Table 3, the dispersion performance is superior to that of the comparative example.

[Table] Example 4 After applying the lubricating oil compositions shown in Examples 1 and 2 to a steel material (chromium molybdenum steel, SCM21) with a diameter of φ9.9 shown in FIG. Using the shown mold, the deformation resistance (maximum punch pressure) and processing performance of lubricating oil were evaluated using the forward extrusion processing method. The evaluation results are shown in Table 4. The processing performance of lubricating oil is the mold temperature at which galling or seizure occurs on the surface of the molded product after processing, and the higher this temperature, the better the processing performance. The processing oils of Comparative Examples A and B were conventionally used for cold working, and their compositions are shown below. Comparative example A Mixed oil of mineral oil and ester oil 38.5wt% Fatty oil content 43.5wt% Sulfur content 5.8wt% Chlorine content 12.2wt% Comparative example B Mineral oil 39.7wt% Fatty oil content 50.0wt% Sulfur content 10.3wt% , as follows. 1 Steel material dimensions

【table】 2 Main dimensions of mold

[Table] 3 Deformation resistance Measured with an automatic balance recorder via a pressure transducer installed in the operating oil circuit of the hydraulic press. The punch descending speed during extrusion processing was 15 mm/s. 4 Machining performance A heating band heater is attached to the mold shown in Figure 2, and the temperature of the mold is raised stepwise by 5 to 10°C. At each temperature, the material coated with lubricating oil is processed. The mold temperature at which seizure occurred on the surface of the molded product was measured.

【table】

[Table] As is clear from Table 4, the lubricating oil of the present invention has lower deformation resistance and superior machining performance than the machining oils of Comparative Examples A and B. It is also found that processing performance deteriorates when the amount of dispersant exceeds 10% by weight. Example 5 The same lubricating oil as in Example 1 and Example 2 was used in the third
It is applied to the primary molded product shown in Figure A, and further deep drawn using the deep drawing die shown in Figure 4.
The secondary molded product shown in Figure 3-B was processed and the lubrication effects were compared. The lubrication effect was determined by measuring the presence or absence of seizure on the surface of the molded product and the formation of a lubricating film using an X-ray microanalyzer (XPMA). The results are shown in Table 5. 1 Test conditions (1) Material: Steel plate (SPCE) without annealing Primary molded product dimensions: inner diameter 23 mm, outer diameter 34 mm, height 21
mm, thickness 3mm Secondary molded product dimensions: inner diameter 23mm, outer diameter 27mm, height 30mm
mm, thickness 2mm (2) Processing speed: 200mm/s 2 Evaluation (1) Surface condition 〇: No seizure △: On the verge of seizure ×: Seizure (2) XPMA analysis 〇: Reaction product elements are present on the entire surface It's biased. Δ: The elements of the reaction product are locally polarized. ×: The element of the reaction product is the same as that of the raw material. As is clear from Table 5, the lubricating oil composition of the present invention has a superior lubricating effect compared to the processing oils of Comparative Examples A and B. However, if the amount of the dispersant exceeds 10% by weight, the lubricating film formation tends to deteriorate.

【table】

[Table] Example 6 The organic phosphoric acid esters shown in Table 6, which are insoluble in mineral oil, were added to mineral oil (viscosity 150 mm ² /s at 40°C) at a concentration of 0.5 to
The processing performance of a lubricating oil composition containing 60% by weight of polybutenyl succinate (dispersant: Lubrizol 939) and 1% by weight based on the added amount of the organic phosphate ester was evaluated using the same test method as in Example 4. was evaluated. The results are shown in Table 6. As is clear from Table 6, it can be seen that when the amount of organic phosphoric acid ester added is 1% by weight or more, the processing performance exceeds that of Comparative Examples A and B shown in Example 4. Furthermore, when the amount of organic phosphate added exceeds 10% by weight, the effect of addition does not change much.

[Table] Example 7 The processing performance of a lubricant composition consisting of the additives and solvent shown in Table 7 was evaluated under the same conditions as in Example 4. The amount of additives is the remaining amount of the solvent, which is the total amount of 100. The evaluation results are shown in Table 7.

〔Effect of the invention〕

The lubricating oil composition according to the present invention allows molded products with a high degree of workability to be processed simply by applying the lubricating oil to the surface of the steel material. Furthermore, since the organic phosphate ester, which is insoluble in lubricating oil, has an excellent dispersion effect in oil, a stirring device can be eliminated.

[Brief explanation of the drawing]

Figure 1 is a side view of the material used to evaluate the processing performance of lubricating oil, Figure 2 is a vertical cross-sectional view of the forward extrusion die used to evaluate the processing performance of lubricating oil, and Figure 3 The figure is a longitudinal cross-sectional view of the material used for deep drawing.
FIG. 4 is a longitudinal sectional view of the deep drawing die. 1...Punch, 2...Mold, 3...Material, 4...
...Heating heater, 5...Upper notch out pin, 6
... Shank, 7 ... Mold holder, 8 ... Mold holder, 9 ... Stripper, 10 ... Punch holder, 11 ... Fixing stand.

Claims (1)

[Claims] 1 (A) General formula [Wherein, R is a hydrocarbon group having 1 to 18 carbon atoms,
R' is hydrogen or a hydrocarbon group having 6 to 10 carbon atoms,
n is an integer of 1 to 3] 5 to 50% by weight of an acidic phosphoric acid ester. (B) Alkenyl succinimide dispersant 0.05 to 10% by weight based on component (A) above. (C) One or more residues selected from lubricating oil, organic solvent, or water. A lubricant composition for metal processing consisting of.