JP2706735B2 - Dry lubricant for drawing metal materials - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to iron, steel, stainless steel, molybdenum steel, high carbon chromium steel, titanium steel, nickel chromium alloy, aluminum alloy, copper alloy, and iron and steel. The present invention relates to a dry lubricant for drawing wires, rods, pipes, etc. (hereinafter collectively referred to as metal materials) made of copper, zinc, brass, nickel, and the like.

[Conventional technology]

When a metal material is drawn, the metal surface is physically or chemically descaled in advance and then drawn as it is, or it is further subjected to a pretreatment coating (eg, a lime soap coating, a phosphate coating, a borax coating, a resin coating). System coating, oxalate coating, metal plating coating, etc.) and then drawing.

Lubricants used in these drawing processes are roughly classified into three types: a water-soluble wet lubricant, an oil-based lubricant, and a dry lubricant (powder). The present invention relates to the dry lubricant among these. .

Conventional dry lubricants are made of known metal soaps or alkali soaps, or made of these soaps added with extreme pressure additives and inorganic additives that act like rollers.

Examples of the metal soap include Ca, Ba, Al, Mg, Zn, Fe, Pb, and Sn salts of higher fatty acids (mainly stearic acid, balmitic acid, oleic acid, erucic acid, lauric acid, etc.), and alkali soaps. Are typically Na, K, and Li salts of higher fatty acids.

Extreme pressure additives or inorganic additives such as sulfur, borax,
Graphite, molybdenum disulfide, tungsten disulfide, carbon fluoride, boron nitride, calcium phosphate, calcium borate, slaked lime, talc, mica, titanium oxide, magnesium oxide, zinc oxide, calcium carbonate, sodium carbonate, zinc phosphate,
Metal salts of isopropyl acid phosphate, powdered paraffin chloride, chlorinated resin powder, fluorinated resin powder and the like are known.

[Problems to be solved by the invention]

These conventional dry lubricants have drawbacks such as an inability to increase the drawing speed, a reduction in total area reduction, and difficulty in rationalizing the pre-processing and post-processing steps for drawing. Furthermore, sulfur conventionally used as an extreme pressure additive is also harmful to the human body where odor is severe. Molybdenum disulfide, tungsten disulfide, glue graphite, etc. are expensive and difficult to handle because they are black fine powder, and at the same time, the finished surface of the wire is black, so degreasing after drawing is extremely difficult. There are disadvantages.

It is therefore an object of the present invention to remedy the disadvantages of these conventional dry lubricants.

[Means for solving the problem]

The present invention relates to a dry lubricant comprising the above-mentioned conventional dry lubricant mainly composed of metallic soap or alkali soap and further added with an adduct (powder) of melamine and isocyanuric acid or cyanuric acid. This is because the drawability has been dramatically improved.

The adduct of melamine and isocyanuric acid or cyanuric acid used in the present invention is not particularly limited to a production method, but as an example, melamine and one or both of cyanuric acid or isocyanuric acid are in a solid state in an aqueous solvent. The most preferred is a melamine / (iso) cyanuric acid adduct obtained by reacting in the state of being dispersed in the above, and having a molar ratio of 1: 1. These production methods are described in
54-141792 can be referred to.

Commercially available adducts of melamine with cyanuric acid or isocyanuric acid include melamine cyanurate MC-SW and MC White of Nissan Chemical Industries, Ltd., or melamine cyanurate MCA-C-1 of Yuka Melamine Co., Ltd. For the physical properties of these materials, refer to the catalogs of both companies and Material Technology, Vol.
Pages from page 11 to page 11 can be referred to.

As a method of adding an adduct of melamine and isocyanuric acid or cyanuric acid (hereinafter referred to as MCA) to a dry lubricant, it is added during metal soap production or alkali soap production and then pulverized, or metal soap or alkali soap is added. May be added together with other additives after pulverization, and may be uniformly mixed using a powder mixer.

The amount of MCA added depends on the type of metal soap or the type of alkali soap and the type and amount of other additives.
1-30% by weight, preferably 2-10% by weight is optimal.

When the amount is less than 0.1% by weight, no significant difference in lubricating performance from the conventional dry lubricant appears, and when the amount is more than 30% by weight, the lubricating effect is not further improved, resulting in high cost and economical cost. It is only a disadvantage.

Conventionally, in the case of dry drawing of a stainless wire, a chlorine-based or fluorine-based resin coating or a oxalate coating is applied to the surface of the wire before drawing, and then a black extreme pressure additive (eg, MoS ₂ , WS ₂ , wire drawing using a dry lubricant containing graphite. For this reason, the drawn skin becomes very black skin, so that the original white skin of stainless steel is obtained, and the generation of corrosive gas or clogging of the annealing pipe in the bright annealing furnace in the later process is to be prevented. Therefore, a sufficient degreasing step is required. However, the use of the dry lubricant of the present invention not only eliminates the necessity of these pretreatment agents prior to wire drawing, but also makes the wire drawing black without blackening, making degreasing very easy to finish. Becomes Since no corrosive gas is generated, annealing can be performed without performing degreasing.

High carbon bearing steel (JIS SUJ, SKH
Etc.) (for example, processing from 5.5 mm to 4.5 mm wire diameter)
In the conventional dry lubricant, it was possible to draw only at a maximum speed of 60 m / min, but by using the dry lubricant of the present invention, it was possible to double the speed to 120 m / min. Become. Also, for example, a PC steel wire with a wire diameter of 10 mm coated with phosphate is used.
When drawing at 200m / min, up to 4.0mm, the average dry dry lubricant from 70 to 80 tons per die was
By using the lubricant of the present invention, the production can be increased to an average of 150 to 200 tons per die.

The bright annealed stainless wire (SUS-304) can be drawn up to 86% with the dry lubricant of the present invention, while the conventional dry lubricant has a total area reduction rate of at most 80%.

Similarly, a brightly annealed 2.0 mm diameter stainless steel wire (SUS
-304) for wire drawing up to 0.6mm in diameter, conventionally coated with chlorine-based or fluorine-based resin, then drawn using a normal dry lubricant, degreased with chlorinated organic solvent, and bright annealed doing. In this step, if the dry lubricant of the present invention is used,
Wire drawing can be performed sufficiently without applying a pretreatment agent coating as in the conventional process, and if a pretreatment agent is not required, solvent degreasing after wire drawing is naturally unnecessary.

It goes without saying that these can not only rationalize the work, but also reduce the running cost and improve the quality of the drawn wire.

In addition, the dry lubricant of the present invention can be used for a phosphate-coated or borax-coated steel wire (wire rope, piano wire, steel cord busbar, bead wire, etc.), or lime soap-coated iron wire, and mechanical descaling. It can be applied to dry drawn wire such as iron wire, zinc plated steel wire, zinc or copper plated iron wire, Ni plated stainless steel wire, or copper alloy wire, aluminum alloy wire, nichrome wire etc. .

〔Example〕

 Hereinafter, the present invention will be described with reference to examples.

Example 1 A stainless steel reaction vessel was charged with 568 g (2 mol) of stearic acid and heated. When the temperature of the contents reached 100 to 120 ° C, 15.5 g of MCA was added and stirred. Continue heating 13
When the temperature reaches 0 to 140 ° C, 81.4 g of calcium hydroxide (1.1
mol) was slowly added to react. After the complete reaction, the content was taken out and cooled, and then pulverized so that the 50-mesh sieve passing rate became about 50%. 18 g of slaked lime was added to 82 g of the pulverized product, and mixed with a kneader to obtain a dry lubricant.

Example 2 568 g of stearic acid was charged into a stainless steel reaction vessel and heated. When the content reached 140 ° C., 188.5 g (1.1 mol) of barium hydroxide was gradually added to allow a complete reaction. Then, the reaction mixture was taken out of the vessel, cooled, and ground as in Example 1.

In another reaction vessel, 282 g (1.0 mol) of oleic acid was charged,
188 g of water was added and heated. When the temperature of the contents reached 80 to 90 ° C., 80 g (1.0 mol) of 50% NaOH was gradually added and reacted. The hydrous sodium oleate as a reaction product was taken out of the container, dried until the water content became 1.0% or less, and then pulverized in the same manner as the above barium stearate.

40 g of barium stearate, 20 g of sodium oleate, 33 g of slaked lime, 5 g of powdered sulfur, and 2 g of MCA obtained as described above were mixed in a kneader to obtain a dry lubricant.

Example 3 As in Example 1, 568 g of stearic acid was charged into a reaction vessel, and after heating, 33 g of MCA was added. Then calcium hydroxide 8
1.4 g was added for complete reaction. The obtained product was pulverized, and 45 g of slaked lime was added to 55 g of the pulverized product and mixed to obtain a dry lubricant.

Example 4 Stearic acid (568 g) was charged into a stainless steel reaction vessel and heated. At a temperature of 130 to 140 ° C., 81.4 g of slaked lime was gradually added to allow a complete reaction. The reaction product was taken out of the vessel, and after cooling, pulverized so that the 50-mesh sieve passage rate became 50 to 60%. 40 g of the pulverized product, 20 g of the pulverized barium stearate obtained by the production method of Example 2, 35 g of slaked lime, and 5 g of MCA were mixed with a kneader to obtain a dry lubricant.

Example 5 As in Example 1, 568 g of stearic acid was charged and heated.
46 g of MCA was added. Thereafter, 81.4 g of calcium hydroxide was added to allow a complete reaction, and then pulverized.

284 g of stearic acid and 190 g of water were added to another reaction vessel and heated. At a temperature of 90 to 100 ° C., 80 g of 50% NaOH was gradually added and reacted. The reaction product was taken out of the container, dried until the water content became 1.0% or less, and then pulverized.

58 g of the MCA-containing calcium stearate, 30 g of sodium stearate, and 5 g of anhydrous borax powder obtained as described above were mixed in a kneader to obtain a dry lubricant.

Example 6 A stainless steel reaction vessel was charged with 564 g (2 mol) of oleic acid and heated at a temperature of 150 to 180 ° C. at 44.3 g (1.1 g of magnesium oxide).
mol) was added slowly to complete the reaction. The reaction product was taken out, cooled, and then pulverized so that a 50 mesh sieve passing ratio was 50 to 60%.

15 g of the pulverized product, 55 g of the pulverized calcium stearate obtained in the same manner as in Example 4, 10 g of slaked lime, 5 g of powdered calcium phosphate, 5 g of powdered zinc oxide, and 10 g of MCA were mixed with a mixer to obtain a dry lubricant.

Example 7 60 g of the powdered sodium stearate obtained in Example 5, 30 g of the powdered sodium oleate obtained in Example 2, and 10 g of MCA were mixed by a moderator to obtain a dry lubricant.

Comparative Example A 20 g of slaked lime was added to 80 g of the powdered calcium stearate obtained in Example 4 and mixed to obtain a dry lubricant of Comparative Example A.

Comparative Example B 40 g of barium powder barium stearate obtained in Example 2, 20 g of powdered sodium oleate obtained in Example 2, 33 g of slaked lime, 2 g of powdered molybdenum disulfide, and 5 g of powdered sulfur were mixed with a kneader to obtain Comparative Example B. A dry lubricant was obtained.

Comparative Example C Dry lubricant of Comparative Example C was obtained by mixing 55 g of molybdenum disulfide-containing calcium stearate powder obtained by adding 5 g of powdered molybdenum disulfide instead of MCA in Example 3 with 45 g of slaked lime.

Comparative Example D Powdered calcium stearate 55 obtained by the production method of Example 4
g, powdered magnesium oleate 2 obtained by the method of Example 6
5 g, slaked lime 10 g, powdered anhydrous borax 5 g, and powdered zinc oxide 5 g were mixed with an kneader to obtain a dry lubricant of Comparative Example D.

Comparative Example E Powdered sodium stearate 60 obtained by the same method as in Example 5
g, 30 g of powdered sodium oleate obtained by the same method as in Example 2,
7 g of powdery molybdenum disulfide and 3 g of powdered sulfur were mixed with an kneader to obtain a dry lubricant of Comparative Example E.

Comparative Example F Powdered calcium stearate obtained by the same method as in Example 4
45 g, slaked lime 40 g, and powdered molybdenum disulfide 15 g were mixed in a kneader to obtain a dry lubricant of Comparative Example F.

The above Examples 1 to 7 and Comparative Examples A to F are summarized and shown in Table 1 below.

Test Example 1 When a JIS standard SUS-304 stainless steel wire is dry-wired, a wire is conventionally drawn after a pretreatment coating (chlorine or fluorine resin coating) has always been applied. This is performed to enhance the lubrication effect. If the performance of the dry lubricant is sufficient, this pretreatment agent can be removed, and at the same time, the degreasing process performed after drawing is very easy. Becomes

 For this purpose, a test was performed under the following drawing conditions.

Test material: JIS standard SUS-304 Wire diameter of test material: 5.5mm Finished wire diameter: 2.2mm Total area reduction rate: 84% Number of dies: 8 Drawing speed: 150m / min Conventionally before drawing work Chlorine resin coating (resin concentration 15 ~
20%), wire-drawing was performed with a dry lubricant such as Comparative Example C or F in Table 1, and then degreased by steam cleaning of trichlene.

Under the same drawing conditions without applying a pretreatment coating, Table 1
When the dry lubricant of Example 5 was used, it was found that wire drawing could be performed as in the conventional process.

In addition, since the lubricants of the conventional comparative examples C and F contain molybdenum disulfide, the drawn wire becomes greenish black, and thus, at the present time, degreasing is repeated several times by steam cleaning with trichlene. However, the surface of the wire rod drawn only with the lubricant of the present invention (Example 5) does not use a chlorine-based resin as a pretreatment agent, so that this resin does not remain, and the MCA is white. Therefore, it is not necessary to degrease trichlene after drawing to finish the drawn skin white, and it can be passed to the next annealing step as it is, but even more clean can be easily degreased by simple alkali degreasing. done.

Test Example 2 Drawing of stainless steel wire for spring of JIS standard SUS-304 is conventionally performed under the following drawing conditions.

Test material: JIS standard SUS-304 material Bright solid solution heat treated, Ni-plated Pretreatment agent: Fluoro resin coating treatment Test material wire diameter: 2.0 mm Finished wire diameter: 0.6 mm Number of dies: 9 Linear speed: 250 m / min Under the drawing conditions, the wire was conventionally drawn using the dry lubricant of Comparative Example D, or the dry lubricant of Example 4 of the present invention was used without applying the fluorine resin coating. When used and subjected to wire drawing under the same drawing conditions, the wire drawing could be performed without any change from the conventional process, and at the same time, the spring workability in the subsequent process was almost the same.

This eliminates the need for expensive fluorous pretreatment agents,
This eliminates the need for treatment with a fluorine-based or chlorine-based solvent, thus eliminating the problem of pollution.

Test Example 3 Wire drawing of special steel (high carbon bearing steel, JIS standard SUJ material) has conventionally been performed by applying a phosphoric acid coating or a lime soap coating before drawing after descaling by pickling. In recent years, except for this pretreatment step, shot blasting is performed as it is, but the load on the lubricant is large, so the desired processing rate can not be obtained, the linear speed is very poor, and the die life is short And other problems have occurred.

For this purpose, the lubricant of the present invention was used under the following drawing conditions.

Test material: JIS standard SUS-2 material Pretreatment agent: Shot blast Wire diameter of test material: 7.5 mm or 5.5 mm Finished wire diameter: 6.25 mm or 4.5 mm Number of dies; 1 wire speed; 60 m / min → 120 m / min The conventional lubricant under the above wire drawing conditions used the lubricant of Comparative Example E containing molybdenum disulfide, sulfur, and the like, and was able to achieve a maximum linear velocity of only 60 m / min. However, when the lubricant of Example 7 of the present invention was used, the linear velocity could be increased to a maximum of 120 m / min.
Also, because it does not contain molybdenum disulfide, it has a beautiful finished skin. At the same time, it was confirmed that the rust-prevention performance of the drawn wire, which is greatly affected by the sulfur content, was also greatly enhanced.

Test Example 4 Drawing of PC steel rod with phosphate coating (under the following conditions)
In the prior art, the lubricant of Comparative Example F was used, and the drawn amount until the tolerance of the finished super steel dies increased by 3/100 was 70 to 80 tons on average, but the lubricant of Example 3 of the present invention was used. The average die life was increased to 150 to 200 tons (i.e., the finished die life was doubled on average).

In Comparative Example F, a large amount of molybdenum disulfide was contained, so that the finished skin was very black and it was difficult to find a dice mark. The mark has been found.

Test material: PC steel rod (SWRS-77B) Pretreatment agent: Phosphate coating Wire diameter of test material: 10.0 mm Finished wire diameter: 4.0 mm Total area reduction rate: 84.0% Number of dies; 8 pieces Pulling speed: 200 m / Min Test example 5 In the drawing of a steel cord busbar (72C material), a rod having a diameter of 5.5 mm was pickled, a phosphate coating was applied, and the lubricant of Comparative Example B was used to draw a 2.6 mm diameter rod. Normal drawing was followed by soft annealing, acid wire, phosphate coating or borax coating, followed by secondary drawing to a diameter of 1.6 mm.

By using the lubricant of Example 2 of the present invention in this working step, the intermediate annealing was not performed and the diameter was reduced from 5.5 mm to 1.6 mm.
It is now possible to process up to mm (see Table 2).

Test Example 6 Mechanical descaler for iron wire (SWRM-6)
In D), the dry lubricants of Comparative Example C and Example 3 were examined under the following drawing conditions.

Test material: SWRM-6 Pre-treatment process: Borax treatment after passing through bending roller Wire diameter of test material: 5.5 mm (scale-adhered material) Finished wire diameter: 1.6 mm Number of dies: 9 (including coiler dies) 700 m / min When the lubricant of Comparative Example C is used, the maximum speed is up to 700 m / min, and the surface of the finished wire is also finished in black. However, when the lubricant of Example 3 was used, the speed could be increased up to a maximum of 900 m / min, and the finished state was very smooth and a white line was obtained.

Test Example 7 In the case of wire drawing of nichrome wire, it is extremely difficult to draw, so after descaling by conventional pickling, pre-treatment with ethylene tetrafluoride resin or ethylene trifluoride chloride resin, and then dry drawing Is lined.

If the dry lubricant of Example 6 of the present invention was used in this step, it was possible to draw sufficiently without applying a tetrafluorinated or trifluorinated ethylene resin.

 The experimental drawing conditions are as follows.

Test material: Nichrome wire (JIS standard, HCHW-1) Pretreatment step: Pickling-water-lime neutralization Lime diameter: 5.5mm or 2.9mm Finished wire diameter: 2.9mm or 1.1mm Number of dies; 5 or 9 wire speed; 130-150m / min, 300350m / min Comparative Example 8 Copper alloy wire such as JIS standard C-2600W, C-2700W (brass wire)
Is usually annealed, acid-washed and rinsed every time one pass is drawn. By using the lubricant of Example 1 in this step, wire drawing can be performed two passes at a time.

For example, as shown in the following Table 33, in the case of the conventional dry lubricant (Comparative Example A), the intermediate process was performed for each pass, but in the present invention (Example 1), from 8.3 mm to 4.6 mm (total area reduction rate). 69.3%)
Processing can be performed at once without an intermediate step. This has led to a great deal of work streamlining and running cost reduction.

[Effects of the Invention] When the dry lubricant according to the present invention is used, as is clear from the data of the above-mentioned test examples, improvement in drawing speed, increase in area reduction, omission of pre-treatment and / or post-treatment, Various excellent effects such as prevention of contamination are achieved.

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Claims (1)

(57) [Claims] 1. A dry lubricant for drawing metallic materials, characterized in that an additive of melamine and isocyanuric acid or cyanuric acid is added to a dry lubricant for drawing which contains metal soap or alkali soap as an output component. .