JPH0368697A - Water-base lubricant for cold plastic working of metal - Google Patents

Abstract

PURPOSE:To obtain a stable, water-base lubricant for cold plastic working of metal, which can impart very excellent lubricity, by using a metallic soap, a solid lubricant, and a surface active agent as constituents. CONSTITUTION:The title lubricant contains 4-160g/l of a metallic soap (e.g. calcium stearate), 50-400g/l of a solid lubricant (e.g. molybdenum disulfide), and 0.5-40g/l of a surface active agent (any of nonionic, anionic, cationic, and ampholytic surface active agents can be used). This lubricant serves to impart lubricity far superior to that obtainable with any conventional water-base lubricant. If a colloidal titanium is incorporated therein in addition in an amount sufficient to provide a titanium content of at least 10ppm the lubricant can form a lubricating film with enhanced lubricating performance and it can also prevent rusting when used in cold working of steel, etc.

Description

DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention applies cold plastic working (forging, pipe drawing, etc.) to metal materials such as steel, titanium and titanium alloys, copper and copper alloys, aluminum and aluminum alloys.

The present invention relates to a water-based lubrication treatment liquid (hereinafter abbreviated as water-based lubrication treatment liquid) for cold plastic working of metal materials, which is applied to wire drawing, etc.

[Prior Art] The water-based lubrication treatment liquid includes, for example, a solid lubricant such as molybdenum disulfide or graphite, and one or more selected from inorganic binders and organic binders;
Those consisting of surfactants are known.

During cold plastic working, which involves a relatively small degree of working, a water-based lubricant treatment liquid is brought into direct contact with the surface of the oil-free metal material, and then dried to form a solid lubricant film. In addition, during cold plastic working, which involves a large degree of processing, a chemical conversion film is formed on the surface of the metal material, and then the surface is brought into contact with a water-based lubricant and dried, or a solid lubricant powder is applied to the surface. A method has been adopted in which a lubricating film is formed on the chemical conversion film by means such as attaching a lubricating film. However, when solid lubricants are used in powder form, there are problems such as the dust worsening the working environment.6 When considering workability, it is most preferable to use a water-based treatment liquid, but the existing water-based solid lubricant treatment Liquids often have unstable and insufficient lubrication performance, and often cause problems such as seizing and galling, and are also used on steel materials after lubrication treatment or after lubrication treatment and plastic working. If left untreated, there is also the problem that rust will develop on the steel to be treated.

[Problems to be Solved by the Invention] The present invention provides a water-based solid lubricant treatment liquid that has better and more stable lubrication performance than conventional water-based solid lubricant treatment liquids, and that is less likely to cause rust even when used on steel materials. Our goal is to provide a water-based lubricant treatment liquid.

[Means and Effects for Solving the Problems] The present inventors applied a water-based lubrication treatment liquid consisting of a metal soap, a solid lubricant, and a surfactant to a metal surface. It was discovered that a lubricating film with excellent lubrication performance, which could not be achieved with lubricating treatment liquids, could be formed.

In addition, the present inventors have found that by incorporating colloidal titanium into this water-based lubrication treatment liquid, a lubricating film with even better lubrication performance is formed, and furthermore, when it is used for cold working of steel materials, it is possible to prevent the formation of rust. I found it.

Furthermore, the present inventors have developed a water-based lubrication treatment liquid containing the aforementioned metal soap, a solid lubricant, and a surfactant, and a water-based lubrication treatment liquid containing a metal soap, a solid lubricant, a surfactant, and colloidal titanium. It has been discovered that by adding a binder to the product, the lubrication performance can be further enhanced due to the synergistic effect with the metal soap and colloidal titanium.

The present inventors have accomplished the present invention based on these findings.

That is, the water-based lubricating treatment liquid according to claim (1) of the present invention contains 4 to 160 g/Q of metal soap and 50 to 400 g of solid lubricant.
/l and a surfactant of 0.5 to 40 g/fi.

Metal soaps are salts of fatty acids and metals. Examples of fatty acids include lauric acid, myristic acid, valmitic acid, stearic acid, behenic acid, and bitroxystearic acid.

Preferred is stearic acid. The metal salt may be one or more selected from calcium salts, aluminum salts, magnesium salts, barium salts, zinc salts, and the like.

Wet calcium stearate obtained by the double decomposition method described in Japanese Patent Publication No. 60-45680 is extremely preferred as a metal soap.

Metal soap has a solid content of 4 to 1 in the water-based lubricating treatment liquid.
60g/Q is added. The amount of metal soap added is 4g/a
If the amount is less than 160 g/α, a satisfactory effect cannot be exhibited, and even if more than 160 g/α is added, it is difficult to expect any further improvement in lubricity, but rather impedes the lubrication performance of the solid lubricant.

The solid lubricant is one or more types selected from molybdenum disulfide, graphite, tungsten disulfide, graphite butt, boron nitride, talc, etc., and the content is 50 to 50% of the water-based lubrication treatment liquid. The range is 400g/Q. If it is less than 50 g/Q, the formation of a solid lubricating film on the metal material tends to be insufficient, and if it is added in excess of 400 g/Q, the lubricating effect will be saturated and no further performance improvement can be expected, and the water-based lubricant treatment liquid Cost increases. 150
A more preferable content is g/l to 250 g/n.

In the present invention, the blending amount of metal soap and solid lubricant is as follows:
When the solid lubricant is selected in a weight ratio of 2=5 to 1:50, an extremely excellent lubrication effect can be obtained.

The surfactant is added to disperse the solid lubricant in water, and the present invention does not specify its type.

Examples of nonionic surfactants include polyoxyethylene alkyl ethers, polyoxyethylene alkylphenyl ethers, polyoxyethylene alkyl esters, polyoxyethylene sorbitan alkyl esters, and the like.

Examples of the anionic surfactant include fatty acid salts, alkyl sulfate salts, alkyl sulfonate salts, alkyl phosphate salts, and alkyl dithiophosphate salts.

Examples of cationic surfactants include aliphatic amine salts and quaternary surfactants.
Examples include grade ammonium salts.

Examples of amphoteric surfactants include amino acid type and betaine type carboxylates, sulfate ester salts, sulfonates, and phosphate ester salts.

In the present invention, the content of surfactant is 0.5g/l to 40g/l.
a, and this content is usually added proportionally to the content of the solid lubricant. If the surfactant content is less than 0.5 g/ffi, the wetting effect on the solid lubricant tends to be insufficient, and even if more than 40 g/α is added, the effect will not be improved. , usually about 5 to 10 g/41.

The aqueous lubrication treatment liquid of the present invention may further contain polymeric dispersants, antifoaming agents, antirust additives, and the like.

The water-based lubrication treatment liquid according to claim (2) further contains colloidal titanium in the water-based lubrication treatment liquid according to claim (1).

Colloidal titanium is a cloudy white liquid obtained by neutralizing, for example, a compound of sulfuric acid and titanium or a compound of phosphoric acid and titanium with caustic soda, caustic potash, or the like.

Colloidal titanium has a titanium concentration of at least 10p
The aqueous lubrication treatment liquid contains at least pm, more preferably at least 50 ppm. At less than 10 ppm, it is difficult to clearly recognize the effect of improving lubrication performance or imparting rust prevention performance by adding colloidal titanium, but by adding colloidal titanium at a titanium concentration of 10 pp+m or more, improvement of lubrication performance and rust prevention performance were confirmed. , these performances further improve as the concentration of titanium increases. In the present invention, the upper limit of the concentration of colloidal titanium is not specified, but is set at the highest concentration possible in adjusting the water-based lubricating treatment liquid. be.

The water-based lubrication treatment liquid according to claim (3) further comprises one or more selected from inorganic binders and organic binders in addition to the water-based lubrication treatment liquid according to claim (1) or claim (2). This is a characteristic feature.

The type of inorganic binder is not limited, but one or more of the following borate, phosphate, and silicate compounds can be selected and used.

Phalate -HBO,,H,BO,,H4B2O5,H,
B,O,,HB,OI.

H, B, O□. -o, alkali metal salts, alkaline earth metal salts and ammonium salts such as Ba o13.

Phosphate-)1. PO,, opoa, H, P, O,
, H3PO3, H4F, O,.

HPO,,H,PO,,)1. P-o! Alkali metal salts, alkaline earth metal salts and ammonium salts, polyphosphoric acids 1 such as H, P, O, H, P, O□. , H
, P2O3, alkali metal salts, alkaline earth metal salts, and ammonium salts.

Silicates - General formula M, O.chiSin, where M is an alkali metal or alkaline earth metal, and chi is a positive integer from 1 to 5.

The type of organic binder is not specified, but
Water-soluble polymer compounds are preferred, and specifically, starch, seaweed, plant mucilage, animal protein, natural polymer starch such as fermented mucilage, semi-synthetic polymers such as cellulose, polyvinylpyrrolidone, and polyethylene glycol. and synthetic polymers such as polyvinyl alcohol.

The content of one or more selected from inorganic binders and organic binders is 5 to 150 in terms of solid content.
g/a range. The binder is added depending on the content of the solid lubricant, but when it is added in an amount of 5 g IQ or more, the binding force of the film is strengthened and an excellent lubrication effect is exhibited. However, if more than 150 g/Q is added, the viscosity of the aqueous lubrication treatment liquid increases, resulting in an excessive amount of lubricant adhering to the surface of the metal material, resulting in problems such as clogging of lubricant scum in the mold. A more preferable content is 10 to 50 g/Q.

The aqueous lubrication treatment liquid of the present invention can be used as is as a lubricant treatment liquid if the concentration of the components contained therein is relatively low. In addition, when the concentration of the contained components is high, depending on the type of metal material, type of cold plastic working, degree of working, etc., it may be used as is or diluted with an appropriate amount of water.

The water-based lubrication treatment liquid of the present invention can be used in the immersion method, but the liquid temperature at that time is maintained at a temperature of room temperature to 80°C. If the temperature of the water-based lubricant treatment liquid is increased, the metal material will also be heated, and the drying properties of the lubricant film attached to the surface of the metal material will be improved.

However, if the liquid is heated to an excessively high temperature, the viscosity and concentration of the aqueous lubrication treatment liquid will change, making bath management such as water replenishment complicated.

The aqueous lubrication treatment liquid of the present invention can be used, for example, in the steps of degreasing → washing with water → aqueous lubrication treatment of the present invention → drying. Degrease as necessary.

For example, degreasing → water washing → pickling → water washing → aqueous lubrication treatment of the present invention → drying
It can also be used in the process.゛Pickling causes rust.

For example, degreasing → water washing → pickling → water washing → chemical conversion treatment → aqueous lubrication treatment according to the present invention → drying.
For example, it can be used in the steps of degreasing → washing with water → chemical treatment → washing with water → aqueous lubrication treatment of the present invention → drying.

As the metal material to be treated, it is also possible to use materials that have been subjected to shot blasting or sand blasting.

The chemical conversion treatment is carried out depending on the type of metal material, for example, iron phosphate coating treatment, iron oxalate coating treatment, cuprous oxide coating treatment, aluminum fluoride coating treatment, titanium fluoride coating treatment, etc.

These processes are appropriately selected and carried out depending on the type of material, surface condition, type of cold plastic working, working strength, etc.

[Function and Examples] Diameter of 843C (carbon steel, JISG4051) 30 m
A cold forging test and a rust prevention performance test were conducted using various lubrication treatments on a steel bar of 50 m. Each test material was subjected to lubrication treatment in the following steps.

Degreasing → water washing → pickling → water washing → chemical conversion treatment → water washing → lubrication → dry degreasing is 20g/Q Fine Cleaner 4360 (
Degreaser.

In a processing solution containing Nippon Bar Power Ising ■).

An immersion treatment was performed at 70°C for 10 minutes. All washings were performed with running tap water for 1 minute. Pickling is done with Ibit 700A (
Asahi Chemical Co., Ltd.) was used for chemical conversion treatment at room temperature for 10 minutes.
PB 181
/ 1 by immersion in a solution at 80°C for 15 minutes. However, test material No. 7.8.20.21.22 in Table 1
No chemical conversion treatment was applied to ゜28.

Lubrication was performed by immersing the sample in each of the 80° C. liquids listed in Table 1 under water-based lubrication treatment liquid types for 3 minutes. However, test pieces N027 and 32
was immersed in a solution at 70°C for 3 minutes.

Normally, it is sufficient to leave the drying process natural, but this time we used 120°C.
Drying was carried out by blowing hot air at ℃ for 10 minutes.

The lubrication performance of test materials lubricated using these methods was
Cold forging test (rear hole extrusion test) according to the procedure shown in the table
Evaluated by.

The lubrication performance was evaluated using the backward perforation extrusion shown in Table 2.

The maximum perforation depth that could be processed without generating vertical galling defects on the inner wall surface of the cup in the punched portion was measured, and this value is shown in the Good perforation depth column of Table 1, respectively. In addition, the rust prevention properties of the test materials on which the lubricating film was formed were evaluated by the rust prevention test as shown in Table 3.

The evaluation of rust prevention performance is: O: No rust, O: Surface area of 20
% rust occurs, Δ: rust occurs on 20 to 50% of the surface area, ×: rust occurs on more than 50% of the surface area, and the results are shown in the rust prevention performance column of Table 1. It was shown to.

In Table 1, No. 1 = No. 8 is an example of claim (1), but the content of metal soap is 4 g/(No.
22~N.

26 or solid lubricant content of less than 50g/ffi
Good drilling depth compared to O23 and N027 16 to 30 ■ 1 When the water-based lubrication treatment liquid of claim (1) of the present invention is used, excellent lubrication performance that could not be obtained with conventional water-based lubrication treatment liquids is achieved. It is clear that this can be obtained. Furthermore, claim (1)
), No. 2 to No. 6 containing 5 g/fi or more of binder have a good drilling depth of 34 to 48 mm, and N containing no binder has a good drilling depth of 34 to 48 mm.
The good drilling depth is larger than that of 32 mm for OL, indicating that the lubrication performance is improved by including the binder. Note that No. 7 and No. 8 are examples in which the chemical conversion coating was not formed in advance, but the good drilling depth was 30 to 34 m.
5+, the lubrication performance is slightly inferior to No. 2 to No. 6, which have a chemical conversion film formed in advance, but the lubricity is equal to or better than the conventionally used No. and No. 27, demonstrating the excellence of the product of the present invention. It shows.

In Table 1, Nos. 9 to 21 are examples of claim (2) characterized by colloidal titanium. No. 9 to No. 21 have good drilling depths of 36 to 54 mm, and No. 2 of claim (1) does not contain colloidal titanium. ~No6 30~48
It is clear that the good drilling depth is large compared to mm, and even better lubrication performance can be obtained by containing colloidal titanium. In addition, No. 28 to No. 32 are claims (
As a comparative example of 2), No. 28 has a solid lubricant content of less than 50 g/2, and No. 29 to No. 32
Because the content of either metal soap or colloidal titanium, or both, does not reach the content of claim (2), the good drilling depth is 16 to 32 mm, and the lubrication performance is insufficient.

In addition, in No. 9 to No. 21 which are examples of claim (2), the good drilling depth of No. 15 to No. 019 containing a binder is 40 to 54 mm, and the good drilling depth of No. 15 to No. 21 containing a binder is 40 to 54 mm.
Good drilling depth is larger than No. 36 to No. 48 of o9 to No. 14, and the lubrication performance is improved by containing the binder. Further, No. 20 and No. 21 are examples in which no chemical conversion treatment was performed, and although their lubrication performance is slightly inferior, they are superior to No. 32, which have been used conventionally.

In Table 1, No. 1 that does not contain a specified amount of colloidal titanium
~No8, No22~No27, No29. No.31.
The rust prevention performance of No. 32 was between × and Δ, and rust was observed in all of them in the constant temperature and humidity test, but No. 32, which is an example of claim (2),
The rust prevention performance of Nos. 9 to 21 is all O-O, and it can be seen that the rust prevention performance is significantly improved by containing 10 ppm or more of colloidal titanium in the water-based lubricating treatment liquid.

Example 2 SUS410L (13Cr stainless steel, JIS
A cold forging test was conducted using various lubrication treatments on a steel bar with a diameter of 30 mm (G4303). The summary is in the 4th section.
Shown in the table.

Each test material was subjected to lubrication treatment in the following steps.

Degreasing → water washing → pickling → water washing → chemical treatment → water washing → lubrication → dry degreasing is fine cleaner 436020g/Q,
70℃ for 10 minutes, washing with running water for 1 minute, pickling for 1 minute (NO, 7%)
, HF3%.

10 minutes at room temperature.

The chemical conversion treatment is F B AI (1, phosphate film conversion agent,
Nippon Parriki Uising ■) 40g/l and FBA2 (L
Oxalate film conversion aid 1 Made by Nippon Bar Power Ising ■) 2
The sample was immersed for 15 minutes in a solution at 90° C. containing 0 g/ffi and Ig/l of AC-16 (L, phosphate film formation accelerator, manufactured by Nippon Parr Ising Co., Ltd.).

Lubrication was performed by immersing the sample in each of the water-based lubrication solutions listed in Table 4 at 80° C. for 3 minutes. However, No. 10 and No. 14 are 7.
It was immersed in a solution at 0°C for 3 minutes.

The lubrication performance of the test materials treated by these methods was evaluated by the same cold forging test as shown in Table 2 above.

The results are shown in the good drilling depth column of Table 4.

In Table 4, Nos. 1 to 8 are examples of claim (1), but the good drilling depths are 38 to 54 mm, and Nos. 8 to 10 and No. 14, 28 to 3211, which are conventional water-based lubrication treatments.
The water-based lubrication treatment liquid of claim (1) of the present invention has a larger good drilling depth than Il, and even when used for stainless steel,
It is clear that excellent lubrication performance that could not be obtained with conventional water-based lubrication treatment liquids can be obtained. No. 4 to No. 0 in Table 4
No. 7 is an example of claim (2) characterized by colloidal titanium, but the good drilling depth is 44 to 58 mm, and is a comparative example of claim (2). Na1l~No14 with insufficient content is 28
32 mm, it shows excellent lubrication performance. Further, No. 4 to No. 4 which are embodiments of claim (2)
Since No. 7 contains a predetermined amount of colloidal titanium, it can be seen that it has even better lubrication performance than No. 1 to No. 8, which are examples of claim (1).

Example 3 A wire with a diameter of 3cm made of titanium type 2 (JIS H4600),
A cold wire drawing test was conducted after applying various lubrication treatments. The summary is shown in Table 5.

A lubricating film was formed on each test material in the following process.

Degreasing → Water washing → Pickling → Water washing → Chemical treatment → Water washing → Lubrication → Dry degreasing, Fine cleaner 436020g/Q,
70℃, 10 minutes, pickling, 1 (No, 7%, ) IP
3%, RT 1 minute.

The chemical conversion treatment was performed by immersing the sample in a 60° C. solution containing 36 g/u of MET-3851 (compound film forming agent, manufactured by Nippon Parr Ising ■) for 3 minutes.

Lubrication was performed by immersing the sample in each of the water-based lubrication solutions listed in Table 5 at 80° C. for 3 minutes. However, No. 8 in Table 5 is 70.
The sample was immersed in a solution at ℃ for 3 minutes.

The lubrication performance of the test materials treated by these methods was evaluated by a cold wire drawing test as shown in Table 6.

The lubrication performance was evaluated by observing f7R on the surface of each bath shown in Table 6, and evaluating O: no flow occurred, ×: flow occurred.

The results are shown in Table 5 under wire drawing flaw types.

As shown in Table 5, even in wire drawing of titanium materials, No. 4 to No. 4 using the water-based lubricating treatment liquid of the present invention did not generate any flaws even after 5 passes of wire drawing, and no flaws occurred after the 5th pass. An excellent lubricating film was formed compared to Comparative Examples No. 5 to No. 8 in which this occurred.

Table 6 [Effects of the Invention] When the water-based lubrication treatment liquid of the present invention is used, significantly superior lubricity can be imparted compared to the case where conventional water-based lubrication treatment liquids are used. Further, by using the water-based lubrication treatment liquid of the present invention, it is possible to prevent rusting, which has been a problem with conventional water-based lubrication treatment liquids, to obtain products with excellent quality, and to greatly improve workability.

Claims (4)

[Claims] (1) Metal soap 4~160g/l and solid lubricant 50~4g/l
An aqueous lubrication treatment liquid for cold plastic working of metal, containing 0.00 g/l and a surfactant of 0.5 to 40 g/l. (2) Metal soap 4~160g/l and solid lubricant 50~4g/l
An aqueous lubrication treatment liquid for cold plastic working of metal, which contains 0.00 g/l, a surfactant of 0.5 to 40 g/l, and colloidal titanium with a titanium concentration of 10 ppm or more. (3) Further, 5 to 150 g of one or more selected from inorganic binders and organic binders as solid content.
The aqueous lubrication treatment liquid for cold plastic working of metal according to claim (1) or (2), wherein the aqueous lubrication treatment liquid contains: /l. (4) Metal soap: solid lubricant in a weight ratio of 2:5 to 1:5
0. The aqueous lubrication treatment liquid for cold plastic working of metal according to claim (1), (2), or (3).