JPH01110596A - Lubricating oil for cold processing - Google Patents

Abstract

PURPOSE:To provide the above lubricating oil capable of forming films of outstanding heat and load resistances and lubricating, also capable of preventing occurrence of baking, especially suitable for the plastic working of steel material, comprising each specific urea-based lubricant, phosphorus-based high- pressure agent and octanoic acid-based metallic soap. CONSTITUTION:The objective lubricating oil comprising (A) a urea-based lubricant with a particle size of pref. 64-177mum, consisting of a diurea compound of formula I, II or III, triurea compound of formula IV, or tetraurea compound of formula V (R is isocyanate; R1 and R2 are each alkyl; R3 is alkyl or allyl), (B) a mixture of a secondary phosphite of formula VI (R is 6-24C alkyl) and polyphosphoric acid in the ratio of 1/1-1/4, and (C) an octanoic acid-based metallic soap of formula VII (M is Al, Ca, Co, Mg, Mn, Zn etc.) in the preferable weight ratio of 2-15%, 5-20% and 8-20% for the components A, B and C, respectively.

Description

[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a liquid lubricant used when manufacturing mechanical parts by plastic working, and in particular to a cold working lubricant suitable for plastic working of steel materials. Regarding.

[Conventional technology]

Conventionally, liquid lubricants,
Alternatively, there are chemical conversion coating treatments such as phosphoric acid coating and ten-metal soap coating treatment. The liquid lubricant is mineral oil, synthetic oil, or
For example, petroleum product additives (Saiwai Shobo,
Oiliness improvers such as resin acids and beef tallow, phosphorus, sulfur, and chlorine-based extreme pressure agents, such as those listed in
Products containing organometallic extreme pressure agents such as zinc dithiophosphate (Zn-DTI'), solid lubricants such as graphite and molybdenum disulfide, and those that improve the machining performance of liquid lubricants. Japanese Patent Publication No. 60-54998 contains 3 to 15% by weight of sulfur.

The viscosity at 40°C is 200 to 5000 na/5 (C5
The sulfurized oil and fat of t) is used as a base oil, and this is
There is a liquid lubricant for plastic working that contains 5 to 30% by weight of thermoplastic polymer powder of micrometer or less. These liquid lubricants can be used in deep drawing, rolling, or drawing processes with low machining rates, but they are not suitable for lubrication in machining with high machining rates, where friction surfaces are at high temperatures and surface pressures, or machining with complex shapes. Seizing occurs because the heat resistance and load resistance of the film, as well as the formation of a smooth film on the new surface, are insufficient. As a lubricant with a high processing rate, for example, as shown in JP-A-53-113745, a synthetic resin is diluted with a solvent, or a solid lubricant is dispersed in a dissolved liquid and applied to the surface of the material. As described in the method for forming a lubricating film and in Japanese Patent Publication No. 32-3711, the surface of the material is treated with a phosphate film, and then the surface is treated with a treatment liquid containing sodium stearate as the main component, and metal soap is applied to the surface of the material. After the chemical conversion coating treatment to form a coating, plastic working is performed. Further, there is a method of applying an oxalate film treatment instead of the phosphoric acid film treatment and then applying a metal soap film treatment to the surface thereof. These chemical conversion coatings have better anti-seizure properties than the liquid lubricants mentioned above, and are therefore generally used as lubricants for cold working of steel materials. But 1
Methods such as forming a lubricating film on the surface of a material by synthetic resin film treatment or chemical conversion film treatment require sufficient pretreatment and strict process control. For example, when performing a metal soap film treatment on top of a phosphate film treatment, the film is formed by degreasing a material such as steel and then immersing it in a phosphate bath at a predetermined concentration. After that, it requires a complicated process of washing with water, neutralizing it, crushing it in a metal soap dissolving bath of a predetermined concentration, and drying it. In addition, it has the problem that the treatment of waste liquid is troublesome.

The above-mentioned conventional techniques each have their own advantages, but they have problems in seizure resistance under processing conditions that involve heat of deformation, increased exposure of newly formed surfaces, and high surface pressure. In addition, chemical conversion coating treatment is a complicated process and involves many additional operations such as waste liquid treatment, requiring a great deal of labor and expense.

[Problem that the invention seeks to solve]

The purpose of the present invention is to take advantage of the advantages of liquid lubricants, eliminate the need for chemical conversion coating treatment, and eliminate the need for conventional chemical conversion coatings by simply supplying liquid lubricant to the material surface or mold using a known method. The object of the present invention is to provide a lubricant for cold working that has anti-seizing properties comparable to those obtained by processing methods and improved dispersion stability of organic solid lubricants.

[Means for solving problems]

The above purpose is to obtain a diurea compound having the urea bond -N HCN H- of component A, general formula % formula %, or a triurea compound, general formula RIN HCN H-R-N HCN H-R-N H
CN HR2 or tetraurea compound, general formula % formula % (R: isocyanate group, R1, R2: alkyl group, R
3: powder of alkyl group or allyl group (hereinafter referred to as urea-based lubricant) and phosphorus-based extreme pressure agent of component B, secondary phosphite, general formula O (RO)P-(OH ) 2 (R: alkyl group having 6 to 24 carbon atoms) and a mixture of condensed phosphoric acid (mixing ratio 1 = 1 to 1:4) and a dispersant for preventing sedimentation of urea-based lubricant Component C C7Ht 6C○OM ( M: Gold yt such as AQ, Ca, Co, Mg, Mn, Zn, etc.
This is a lubricating oil for cold working that contains an octylic acid metal soap consisting of:

The lubricating oil of the present invention is simply supplied by a known method such as spraying 9 drops onto the surface of the material or mold, and forms a thick lubricating film on the surface of the material due to deformation heat and frictional heat during processing. It is designed to prevent seizure even when processing products with complex shapes or high processing rates.

The urea-based lubricant of the A component of the present invention is in a volatile organic solvent,
For example, after reacting inocyanate as a raw material with an amine in toluene, the solvent is removed, and the reaction product is pulverized. The diisocyanates used in the reaction include, for example, diphenylmethane 4,4'-diisocyanate, tolylene diisocyanate, naphthylene 15-diisocyanate, and tolydine diisocyanate.
, or a diisocyanate having two can be used.

The amines are aliphatic monoamines having 8 to 20 carbon atoms, alicyclic monoamines, or aliphatic diamines. Preferably, an aliphatic monoamine, an alicyclic monoamine, or an aliphatic diamine having 12 to 18 carbon atoms is used. The particle size of the urea-based lubricant powder should be arbitrarily selected depending on the processing conditions, but is usually 0.5 to 5000 μm.
In particular, for processing conditions such as backward extrusion where the appearance of new surfaces is large, the preferred particle size is in the range of 64 to 177 μm. Phosphite esters such as secondary phosphites such as phyto, di-laurylhydrodiene phosphite and di-oleylhydrodiene phosphite, and condensed phosphoric acids include pyrophosphoric acid and polyphosphoric acid. The dispersant of component C is octylate metal soap, and its metals are AQg Ca, Go, Fe, Mg+ Mn.
Examples include tPb, Zn, Zr, etc., among which Ca octylate is particularly preferred.

The lubricating oil to which components A, B, and C are added is mineral oil, diester oil, or synthetic oil such as α-olefin oil or neopentyl polyol ester oil.

A mixture of these oils is used. The viscosity of the lubricating oil should be selected arbitrarily depending on the machining conditions and working conditions. Generally speaking, the viscosity of the lubricating oil is 10 to 300 m/s (set) at 40°C.
A range of is preferred.

The blending ratio of components A, B, and C added to the lubricating oil may be appropriately selected depending on the processing rate of the molded part, but usually component A is 2 to 15% by weight, and component B is 5 to 20% by weight. %, the C component is preferably in the range of 8 to 20% by weight.

If the amount of the additives A, B, and C used in the present invention is less than the above-mentioned range, the effect of the addition will be reduced and the anti-seize property will be reduced. Further, if the amount is too large, no further effect will be observed, so the above-mentioned mixing ratio is preferable.

Powder particle size of urea-based lubricant as component A used in the present invention: 0.5
The reason why the range is 500 μm is that if it is less than 0.5, the amount remaining on the friction surface during machining will be small and seizure will occur. Furthermore, if the thickness exceeds 500 μm, depending on the processing conditions, it may be difficult to draw the material into the friction surface and seizure may occur.

In order to improve the thermal stability of the lubricating oil for cold working of the present invention, additives such as antioxidants and rust preventives may be added.

[Effect]

Before explaining the effects of the constituent components of the lubricating oil for cold working of the present invention, the lubrication mechanism of the liquid lubricant used in deep drawing, rolling, drawing, etc. will be explained. Regarding the lubrication mechanism, see “Lubrication” Vol. 18, No. 3 (p. 193-201)
and “Plasticity and Processing” Volume 9, No. 87 (p202-214
), the liquid 'IIJ lubricant carried between the two surfaces of the material and the mold is sealed in the recesses on the surface of the material during processing. As the plastic change progresses, the surface convexities are rolled down, and the liquid lubricating oil remaining in the concave parts is forcibly discharged and supplied to the flat surface (friction surface) that has been corrected for rolling down, forming an oil film. When liquid lubricating oil contains extreme pressure agents such as phosphorus, chlorine, and sulfur, an extreme pressure film is formed on the surface of the material by plastic deformation heat, frictional heat, etc. to prevent seizure. Machining in which the processing rate is high and the surface area is expanded greatly also employs the above-mentioned lubrication mechanism, but since the friction surfaces are exposed to high temperatures and pressures, a sufficient extreme pressure film is not formed and seizure occurs.

During processing, the powdered urea-based lubricant of component A, which is one of the constituent components of the present invention, is brought to the friction surface with lubricating oil adsorbed on the surface of the powder, creating many recesses and causing the polarization of component B. Trapped together with pressure agent. As plastic deformation progresses, the extreme pressure agent reacts with the material surface to form an extreme pressure film. On the other hand, it has been found that the urea-based lubricant of component A is dissolved or extruded onto the friction surface while being rolled to form a film. That is, the lubricating oil of the present invention has significantly improved seizure resistance due to the formation of a film formed by component A and a film formed by component B on the surface of the material. Also, C
The ingredients are necessary to uniformly disperse the urea-based lubricant in the oil for a long period of time.

〔Example〕

Hereinafter, one example of the cold working lubricating oil of the present invention will be described together with a comparative example.

<Examples 1 to 18> The raw materials used for the urea-based lubricant of component A are the isocyanates shown in Table 1 and amines reacted in toluene, and the powder of the reaction product after removing the solvent, the average particle size. 10% by weight of a 105 μm urea compound, 20% by weight of a mixture of pyrophosphoric acid and dioleylhydrodiene phosphite (mixing ratio 1:3) as an extreme pressure agent for component B, and calcium octylate (offtope Ca) as a dispersant for component C. , (Hope Pharmaceutical Co., Ltd.) and 10 wt% of paraffinic mineral oil (40 wt%).
℃ kinematic viscosity 150+nm/s (set)). Table 2 shows the processing performance and dispersion stability of the obtained cold working lubricating oil.

The processing performance was evaluated by attaching a band heater 3 to the mold (cemented carbide) for the forward extrusion process shown in Figure 1 and the backward extrusion process shown in Figure 2, and increasing the mold temperature in steps of 5 to 20°C. The material coated with lubricating oil is machined one thousand blocks at a time, and the maximum temperature of the mold 2 that can be machined without causing seizure marks on the machined surface (hereinafter referred to as the machining limit temperature) is determined. □ Processing was performed under the following conditions.

In the case of forward extrusion processing, the material dimensions are chromium-molybdenum steel with a diameter of 20 mm and a length of 30 mm, with an extrusion angle of 120 degrees,
Processing was performed with a drawing diameter of 10.2 nwn (processing rate of 75%).

The rear extrusion process uses the same material as the front extrusion process,
Machining was performed using a punch 4 with a diameter of 17° and 4 m (processing rate of 75%). The drilling depth of molded article 1 is 52+am. punch 4
The rate of descent of both is 8.8 pus/S.

As a comparative example, the composition of a conventionally used lubricant for cold working is shown below.

Comparative example Nα1 Phosphate film treated soil metal soap film Comparative example Nα2 Lubricant composition Base oil: Contains sulfur content of 15% by weight, viscosity (40”C) 30
Sulfurized oil and fat of 0 cSt; 80% by weight, nylon powder with particle size: 105 μm; 20% by weight Dispersion stability evaluation method is 50% by weight.
40 mQ of lubricating oil was placed in an mQ Scouriou tube, and the tube was placed in a constant temperature bath maintained at 30° C. The state of sedimentation of the urea-based lubricant of component A was visually examined, and the time required for sedimentation was measured.

Examples 1 to 18 according to the present invention as evident from Table 2
Comparing Comparative Examples 1 and 2 using conventional lubricants, the processing limit temperature is high in all extrusion processing, and the processing performance is excellent. Furthermore, the dispersion stability of the urea-based lubricant as component A is also excellent.

<Examples Nα19 to 38> Dispersion of component C using Nα5, 11 and 17 in Table 1 as raw materials, 10% by weight of urea lubricant as component A, and extreme pressure agent as component B at the blending ratio shown in Table 3. Calcium octylate 21941
Table 4 shows the results of evaluating the processing performance and dispersion stability of the cold working lubricant of the present invention in which 0% by weight was added to the same lubricating oil as in Example 1.

As is clear from Table 4, the dispersion stability and processing performance are excellent compared to Comparative Examples 1 and 2.

<Example Na 39> 10% by weight of the B component shown in Example Na22 and 30, C
Ingredient dispersant Calcium octylate 10% binding,
Urea-based lubricants made from Nα5, 11 and 17 shown in Table 1 were added to the same lubricating oil as in Example 1 to investigate the effect of the blending amount. The results are shown in Figure 3.

As is clear from FIG. 3, the effect of adding the urea-based lubricant as component A becomes apparent when the blending amount exceeds 2% by weight in backward extrusion processing where processing conditions are severe. When it is 5% by weight or more, the performance is higher than the processing limit temperature of Comparative Example Na 1. If it exceeds 15% by weight, no better performance can be obtained.

<Example Nα40> The B component of Examples Nα22 and Nα30 shown in Table 3 was added to the same lubricating oil as in Example 1 at the mixing ratio to examine the influence of the blending amount on processing performance. The results are shown in Figure 4. The A component is a urea lubricant of Nα5 in Table 1, and the dispersant C is calshu octylate 11, and the amount of each is 10% by weight. As is clear from FIG. 4, the effect of addition appears when the blending amount of component B becomes 3% by weight. When it reaches 5% by weight, it becomes the same level as the processing limit temperature of Comparative Example Nα1. If the focus level exceeds 20%, no further effect can be obtained.

<Example Nα41> Using the same lubricating oil as in Example 1, the A and B component compounds and the blending amounts were the same as in Example Nα40, and the dispersion examples of C component, calcium octylate and aluminum octylate, were used to reach 1 dispersion stability. The effect of the amount added was investigated. The results are shown in FIG. As is clear from the results shown in FIG. 5, when the blending amount is 5% by weight or more, the dispersion stability improves as the blending amount increases. Conditions for Use of Lubricating Oil 2 Considering work conditions, etc., it is desirable that the dispersion stability is one day or more. Therefore, the blending amount is preferably 8% by weight or more. At 10% by weight, stability for more than a year can be obtained.

<Example Nα42> Viscosity at 40°C is 100 cxa/s (cst
) using α-olefin oil, NαG, 1 in Table 1
The relationship between powder particle size and processing performance was investigated for urea-based lubricants using the compounds shown in Nos. 2 and 15 as raw materials. The results are shown in Figure 6. The extreme pressure agent of component B was a mixture of pyrophosphoric acid and dioleylhydrodiene phosphite at a mixing ratio of 1:3, and the amount thereof was 10ffi, and the component C was 410% by weight of calshu octylate. As is clear from the results shown in FIG. 6, the processing limit temperature begins to rise when the grain size becomes 0.5 μm or more, and reaches saturation when it reaches 64 μm.

〔Effect of the invention〕

For cold working, the lubricating oil contains the urea-based lubricant of the A component of the present invention, the B component of the mixed extreme pressure agent of condensed phosphoric acid and secondary phosphite, and the C component with octylate metal soap as a dispersant. Simply apply lubricating oil to the surface of materials such as steel or molds using known methods.

During processing, a lubricating film with excellent heat resistance, load resistance, and lubricity is formed on the friction surface, preventing seizure.
It is effective in extending mold life and reducing production costs.

[Brief explanation of the drawing]

Fig. 1 is a vertical cross-sectional view of a mold according to an embodiment of the present invention used for forward extrusion processing, Fig. 2 is a longitudinal cross-sectional view of a mold used for backward extrusion processing, and Fig. 3 is a urea containing component A. A diagram showing the dependence on the blending amount of the system lubricant, FIG. 4 is a diagram showing the dependence on the blending amount of the extreme pressure agent B component, and FIG. 5 is a diagram showing the dependence on the blending amount of the C component.
FIG. 6 is a diagram showing the relationship between powder particle size and processing performance of a urea-based lubricant. 1... Molded product, 2... Mold, 3... Band heater, 4... Figure 1, Figure 2, Figure 3.

Claims (1)

[Claims] 1. The additives A, B, and C components contained in the lubricating oil each have a diurea compound of component A having the general formula R_1-NHCNH-R-NHCNH-R_2▲ mathematical formula,
There are chemical formulas, tables, etc. ▼-NHCNH-R-NHCN
H-▲There are mathematical formulas, chemical formulas, tables, etc.▼▲There are mathematical formulas, chemical formulas, tables, etc.▼-NHCNH-R-NHCNH-R
The triurea compound of _1 or A component has the general formula R_1-NHCNH-R-NHCNH-R-NHCNH
-R_2 or the tetraurea compound of component A has the general formula R_3-N
HCNH-R-NHCNH-R_3-NHCNH-R-
Powder of NHCNH-R_3 (R: isocyanate group, R_1, R_2: alkyl group, R_3: alkyl group or allyl group), phosphorus extreme pressure agent of component B, general formula▲Mathematical formula, chemical formula, table, etc.▼ (R: alkyl group having 6 to 24 carbon atoms) is a mixture of secondary phosphite and condensed phosphoric acid (mixing ratio 1:1 to 1:4)
The dispersant for component C is octylate metal soap C_7H_1_5COOM (M: metals such as Al, Ca, Co, Mg, Mn, and Zn)
A lubricating oil for cold working characterized by: 2. The particle size of the urea compound powder of component A is 0.5 to 500.
Claim 1 characterized in that the range is in the range of μm.
Lubricating oil for cold working as described in section. 3. Component A is 2-15% by weight, component B is 5-20% by weight
The lubricating oil for cold working according to claim 1, characterized in that the lubricating oil contains 8 to 20% by weight of component C.