JPS63215797A - Lubrication method for cold drawing - Google Patents

Abstract

PURPOSE:To improve the surface grade of a work piece after cold working, by applying a particular lubricating oil to a pickled wire, rod or pipe of carbon steel or alloy steel prior to cold drawing. CONSTITUTION:5-40pts. dialkyl polysulfide (A) of the formula (wherein R is a 6-12C alkyl; and x is 3-6) which has a sulfur content of at least 30wt.% and 20-70pts. member selected from among a compd. of a fat or oil having a sulfur content of at least 30wt.% with an olefin, a higher ester compd. of an unsatd. higher fatty acid having a sulfur content of at least 15wt.% with an unsatd. higher alcohol and a compd. of a higher ester compd. having a sulfur content of at least 15% with an olefin are mixed together, thereby preparing a thickener. This thickener is mixed with a fat or oil, a synthetic oil and a higher fatty acid (amine salt) to prepare a lubricating oil having a viscosity of 100-3,000cps (20 deg.C). The lubricating oil thus obtd. is applied to a pickled wire, rod or pipe of carbon steel or alloy steel, washed with water, neutralized and dried, followed by cold drawing.

Description

DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a method of lubrication during cold drawing of carbon steel 1 alloy steel wires, rods, and tubes.

More specifically, 1. The present invention is, for example, a method suitable for cold drawing with a degree of hard working in which the area reduction rate is 30% or more, and it also provides a method for making the surface of the product after drawing smooth and glossy. The purpose is

[Prior Art] In the cold drawing process of carbon steel and alloy steel (hereinafter referred to as steel), it is necessary to use drawing tools and materials. a Reduce chafing,
Lubrication is important to reduce tool wear and prevent seizure flaws.

Conventionally, when cold drawing steel wires, rods, and tubes at a high degree of processing (area reduction rate of 30% or more), a phosphate film is formed on the surface of the wire, rod, or tube, and then soap treatment is performed on the surface of the wire, rod, or tube. Lubrication methods have been widely used. However, in this method, phosphate treatment and soap treatment are usually performed at a high temperature of 75 to 80°C, which requires time and effort to raise the temperature and involves extra energy consumption.

In addition, the processing steps are as many as 8 steps as shown in Table 1.

An even simpler and faster lubrication treatment method is desired.

For more high-grade drawn products, one part of the surface of the product after cold drawing is
11 Smoothness and gloss are desired, but phosphate treatment corrodes the steel surface due to a chemical reaction, making it difficult to improve the surface grade.

Extreme pressure additives to improve surface grade.

For example, lubricating oils containing sulfurized mineral oil, sulfurized fatty acids, sulfurized fats and oils (8 to 15% sulfur content), dibenzyl sulfide, polyphenylene sulfide, etc. are used as sulfur-based lubricants, but these are low-processing, cold oils. Although thinning processing is possible, there is a problem in that the strength of the oil film is insufficient at high processing degrees, and seizure occurs, resulting in scratches on the drawing tool and the workpiece material.

[g! [Problems to be Solved by Akira] The present invention is capable of processing steel wires, rods, and tubes with a high degree of processing (area reduction rate of 3
The purpose is to carry out the lubrication treatment during cold drawing with less than 0%) in an energy-saving and shortened processing process shown in Table 2, and to further improve the surface grade of the workpiece after cold working. It is said that

[Means for solving problems] The lubricating oil used for the lubrication treatment in Table 2 in the present invention is as follows.

A compound of 5 to 40 parts of dialkyl polysulfide with a sulfur content of 30% by weight or more (in this specification, the weight% of the compound blend is expressed as part), an oil and fat and an olefin with a sulfur content of 15% or more, sulfur A higher ester compound of an unsaturated higher fatty acid and an unsaturated higher alcohol having a content of 15% by weight or more.

20 to 70 parts of one or more selected from olefin and higher ester compounds with a sulfur content of 15 or more are mixed, and the viscosity is 100 to 30 at 20°C.
Thickeners, oils, synthetic oils, etc. to achieve 00cm voice.
A lubricating oil prepared with mineral oil, higher fatty acids, and their amine salts.

The present invention will be explained in more detail below.

The dialkyl polysulfide having a sulfur content of 30% by weight or more in the present invention has the following general formula.

-5x-R However, R: alkyl group (carbon number: 6 to 12), Sx:
Sulfur vt (x: 3-6).

The alkyl group is 2-6f of ethylene or propylene! use your body to This synthesis involves, for example, reacting an alkyl mercaptan compound and sulfur in the presence of a basic catalyst (e.g. di-n-butylamine) at 140 to 150°C for 3 hours, and then performing vacuum distillation to remove unreacted fractions. The product is further aerated at 80°C to remove hydrogen sulfide.

The compound of oil and fat with a sulfur content of 15% by weight or more and olefin of the present invention can be prepared by adding, for example, 1 mole of an olefin mercaptan compound and sulfur to 1 mole of unsaturated animal or vegetable oil in the presence of a basic catalyst (for example, di-n-butylamine). 150~
After reacting at 160°C for 3 hours, vacuum distillation is performed to remove unreacted fractions, and hydrogen sulfide is removed by aeration at 80°C.

The higher ester compound of an unsaturated higher fatty acid and an unsaturated higher alcohol with a sulfur content of 15 or more is prepared by mixing sulfur with a higher ester compound and heating it at 160-190°C for 5 to
After reacting for 8 hours, the mixture was aerated at 80°C to remove hydrogen sulfide.

The compound of a higher ester compound containing 15% by weight or more of sulfur and an olefin according to the present invention is produced by adding a mercaptan compound of an olefin and sulfur to a higher ester compound in the presence of a basic catalyst in the same manner as described above.

In the present invention, the viscosity is adjusted to 100 to 3000 CP (centipoise) at 20°C, and the thickeners used include polyisobutylene with an average molecular weight of 5000 to 300,000, and olefin copolymer (ethylene-propylene-based) with an average molecular weight of 10,000 to 1,000,000. butylene type) and polymethacrylate type with an average molecular weight of 20,000 to 15oooooo, but polymethacrylate type is preferable. As the polymethacrylate, one or more selected from polymethacrylates having the following general formula are used.

However,, R: C, ~C,,, R': H or CH
,,X: Polar group The polar monomer for the polar group in the above structural formula is diethylaminoethyl methacrylate (■).

Examples include amines such as 2-methyl-5-vinylpyridine (II), amide polyalkylene glycol esters (1v) such as N-vinylpyrrolidinone (III), and maleic anhydride (V).

Examples of fats and oils include rapeseed oil, lard oil, coconut oil, castor oil, and beef tallow.

Examples of synthetic oils include dioctyl sebacate and pentaerythol derivatives.

Examples of mineral oil include machine oil, and examples of higher fatty acids include animal and vegetable fatty acids and synthetic fatty acids, specifically caprylic acid and capric acid.

Examples include lauric acid, myristic acid, palmitic acid, stearic acid, oleic acid, linoleic acid, and nilukaic acid.

The amines include primary amines having 12 to 22 carbon atoms.

Oleylamine is good.

The present invention uses talc as a solid lubricant as a component of the lubricating oil.

The addition of powders such as graphite, boron nitride, calcium carbonate, and molybdenum disulfide is not prohibited. A solid lubricant is introduced between the extraction tool and the workpiece to prevent direct contact and prevent seizure from occurring.

Further, in the present invention, a surfactant may be used to improve the removal efficiency of alkaline degreasing of the lubricating oil after drawing.

The drawing tools used for cold working are usually made of tungsten carbide cemented carbide, but in order to improve the seizure resistance, the drawing tools are made of titanium carbide, titanium nitride, boron-titanium, etc. The use of coatings such as those based on sintered ceramics, boron-zirconium based coatings, or drawing tools made of sintered ceramics is not prohibited.

In cold drawing of steel, a film formed on the surface of the workpiece is less likely to seize than a pickled surface. Scale and the like also have the effect of preventing seizure, but in the present invention, pickling treatment is performed before lubricating oil treatment in order to improve the surface grade after cold drawing.

Examples of the pickling liquid in the present invention include a 5-20% sulfuric acid aqueous solution, a 5-20% hydrochloric acid aqueous solution, a 5-20% phosphoric acid aqueous solution, and the like. The temperature of the pickling solution is 35°C in the case of a sulfuric acid aqueous solution.
~60℃, room temperature ~40℃ for hydrochloric acid aqueous solution, and 35~60℃ for phosphoric acid aqueous solution.The treatment time is necessary to remove rust and scale from the surface of the treated material, but usually Soak for 10 to 30 minutes.

- The neutralizing solution after pickling may be, for example, a 0.2-5% aqueous sodium hydroxide solution, a 0.2-5% aqueous sodium carbonate solution, or a 0.2-5% aqueous sodium carbonate solution.
A 2-5% sodium borate aqueous solution, a 0.2-5% sodium phosphate aqueous solution, a 0.2-10% lime aqueous solution, etc. are used. The neutralization treatment can be performed by immersion at room temperature to 90'C for 5 seconds to 5 minutes.

The lubricating oil may be applied by dipping, pouring, spraying, or the like.

[Function] When performing cold drawing of steel using lubricating oil, the higher the viscosity of the lubricating oil, the more easily the lubricating oil will be carried between the drawing tool and the workpiece, improving slipperiness and anti-seizure properties. Sexuality also changes.

When the viscosity is less than 100 CP, less lubricant is introduced between the tool and the workpiece. Therefore, in the present invention, the viscosity is adjusted to 100CP or more. Also, the viscosity is 3oooc
If it exceeds p, the amount of lubricating oil brought in will increase and the lubricity will improve, but it will be difficult to apply to the material and handle it, resulting in a decrease in workability. Therefore, in the present invention, the viscosity of the lubricating oil is adjusted to 100 to 3000 CP at 20°C;
A viscosity of 1500 CP is particularly preferred.

When cold working conditions are severe 1 For example, when the drawing speed is high or the area reduction rate is large, the surface temperature of the workpiece increases, and the oil film becomes thinner in the lubrication area at the boundary between the tool and the workpiece. It becomes easy to seize. For this purpose, a sulfur-based extreme pressure additive is used to coat the surface of the workpiece with FeS, which has a low shearing force.
In the present invention, the dialkyl polysulfide containing 30% by weight or more of sulfur is decomposed in the low temperature range of 160 to 280°C to form a compound of iron and sulfur. If the proportion of dialkyl polysulfide is less than 5 parts, FeS, F
Since the amount of e25 produced is small, it is easy to seize, and if the blending ratio exceeds 40 parts, the odor is strong and the working environment is poor, resulting in a decrease in workability. Therefore, in the present invention, the blending ratio of dialkyl polysulfide is 5 to 40 parts, but 15 to 30 parts is particularly preferred.

When cold working conditions are severe and the surface temperature of the workpiece during cold drawing increases, dialkyl polysulfide containing 30% by weight or more of sulfur quickly reacts with iron to form sulfides, preventing seizure. However, dialkyl polysulfide has a high coefficient of friction and poor sliding properties, so heat accumulates in the drawing tool during continuous processing, causing seizure.

In order to improve this, the present invention uses a compound of oil and fat containing 15% by weight or more of sulfur and an olefin, a higher ester compound of an unsaturated higher fatty acid and an unsaturated higher alcohol containing 15% or more of sulfur, and a compound containing 15% or more of sulfur by weight. A compound of a higher ester compound and an olefin is blended by weight or more. These have good reactivity with iron and sulfur, although they are slightly inferior to dialkyl polysulfides, and have a low coefficient of friction and good slipperiness, which reduces heat accumulation in the extraction tool and improves seizure resistance. This makes it possible to prevent the occurrence of abnormal noises, that is, scraping, during cold drawing. The sulfur content of each compound is 15% by weight or more, but the maximum sulfur content is almost determined by the molecular weight and iodine value of oils and fats, higher esters, olefins, etc., and is about 35% by weight or less for oils and fats and olefins. The content is about 30% by weight or less for higher esters, and 35% by weight or more for higher esters and olefins. Furthermore, if the amount added to the lubricating oil is less than 20 parts, staleness is likely to occur, and if it exceeds 70 parts, a bad odor will be strong and workability will be reduced. Therefore, in the present invention, the amount is set at 20 to 70 parts, but 30 to 50 parts is particularly preferred.

The higher the total sulfur content in the lubricating oil composition in the present invention, the better; however, on the other hand, the bad odor will be stronger and the working environment will be worse. For this reason, a range of 15 to 30% by weight is appropriate.

[Example] Example-1 Using lubricant number 1.2.3 in Table 3, carbon-containing-1
Cold drawing of carbon steel sheet steel pipes with dO of 1% was carried out under the conditions shown in Table 4. This result is No.1 in Table 5.

As shown in 2.3, there was no seizure in the steel pipe and the lubricity was good, and the surface of the steel pipe after drawing was dense and smooth, making it suitable for high-grade finishing.

Example-2 Using lubricant number 1.2.3 in Table 3, carbon-containing lubricant
4 Table Cold drawing conditions for steel pipes 5 Table Cold drawing process for steel pipes ×: Offensive odor, Mu: Moderate odor, Δ: Mild odor, 0: None content 0.7
%tT! Wire drawing of 411A was performed under the conditions shown in Table 6.

As shown in No. L, 2.3 of Table 7, this result is 3.
There was no seizure in Bathro, and the lubricity was good.

Comparative Example-1 Using lubricant numbers 4.5.6 in Table 3, the same carbon steel seamless steel pipe as in Example 1 was drawn under the same conditions as in Table 4. As shown in Table 5, No. 3.4.5, seizure occurred in the steel pipe, and in No. 4.5, a bad odor occurred.

Table 6 Steel Wire Drawing Conditions Comparative Example-2 Using lubricant number 4.5.6 in Table 3, the same steel wire as in Example 2 was drawn under the same conditions as in Table 6.

This result is 3 as shown in No. 4.5.6 of Table 7.
0: Abnormal, NG: Burn-in occurred in the pass. Further, in No. 4.5, a bad odor occurred.

[Effects of the Invention] The cold drawing lubrication method of the present invention has a short lubrication process and
Raising the temperature of the lubricating solution is also almost unnecessary.

There is little odor during cold drawing, there is no seizure, and the surface finish of the workpiece after drawing is extremely excellent.

Claims (5)

[Claims] (1) When cold drawing carbon steel or alloy steel wire, rod, or tube, add 5 to 40 parts of dialkyl polysulfide having a sulfur content of 30% by weight or more to the pickled wire, rod, or tube, and sulfur content. Compounds of oils and fats and olefins with a sulfur content of 15% by weight or more, higher ester compounds of unsaturated higher fatty acids and unsaturated higher alcohols with a sulfur content of 15% by weight or more, higher ester compounds with a sulfur content of 15% by weight or more and olefins. 20 to 70 parts of one or more compounds selected from the group consisting of thickeners, fats, oils, synthetic oils, mineral oils, high-grade A cold drawing lubrication method characterized by applying a lubricating oil prepared with a fatty acid and its amine salt. (2) The cold drawing lubrication method according to claim 1, wherein the dialkyl polysulfide having a sulfur content of 30% by weight or more is a dialkyl polysulfide in which the alkyl group has 6 to 12 carbon atoms. (3) The compound of an oil or fat with a sulfur content of 15% by weight or more and an olefin is one of rapeseed oil, cottonseed oil, tung oil, lard oil, beef tallow, chicken oil, or a mixture of two or more, and the olefin is an olefin having 6 to 12 carbon atoms, and a higher ester compound of an unsaturated higher fatty acid with a sulfur content of 15% by weight or more and an unsaturated higher alcohol is a compound in which the unsaturated higher fatty acid has 14 to 22 carbon atoms. is an unsaturated higher fatty acid, the unsaturated higher alcohol is an unsaturated higher alcohol having 14 to 22 carbon atoms, is a higher ester compound, and is a compound of a higher ester compound with a sulfur content of 15% by weight or more and an olefin, Higher ester compound has 14 carbon atoms
A higher ester compound consisting of ~22 unsaturated higher fatty acids and an unsaturated higher alcohol having 14 to 22 carbon atoms,
The cold drawing lubrication method according to claim 11, wherein the olefin is a compound having 6 to 12 carbon atoms. (4) Cold drawing lubrication according to claim 1, 2, or 3, wherein the thickener is polyisobutylene, olefin copolymer, polymethacrylate, or a mixture of two or more thereof. Method. (5) Claim 1 or 2, wherein the pickling treatment is a pickling treatment consisting of the steps of pickling-water-washing-neutralization-drying.
The cold drawn lubrication method of paragraph 3 or paragraph 4.