JPH10259392A - Lubricant for high-temperature plastic working - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a lubricant for high-temp. plastic working which does not cause the seizure, abrasion, and roughening on a tool surface in the high- temp. plastic working of a steel material or a nonmetallic material by incorporating a solid lubricant surface-treated with a titanium-based and/or an aluminum- based surface-treating agent into the same. SOLUTION: A dispersion prepd. by dispersing a solid lubricant (e.g. calcium carbonate, graphite, talc, glass, boron nitride, or mica) having a particle size of 20 μm or lower in a solvent (e.g. hexane or benzene) is mixed under stirring with 0.5-2.0 wt.% titanium-based and/or aluminum-based surface-treating agent at 10-30 deg.C for 10-30 min. Then, the solvent is removed from the dispersion and the resultant product is dried, thus giving a surface-treated solid lubricant contg. titanium and/or aluminum, the active component of the surface-treating agent, in a concn. of 1.5×10<-3> wt.% or higher. The objective lubricant is prepd. by mixing 1-90 wt.% surface-treated solid lubricant above-obtd. with 10.0-99.9 wt% bas grease comprising a base oil (e.g. mineral oil or a synthetic ester) and/or a thickener and a mineral oil.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to high-temperature plastic working of steel and non-ferrous metal materials, and more particularly, to lubrication for high-temperature plastic working which prevents seizure of steel on tool surfaces, wear and roughening of tool surfaces, and the like. And a high-temperature plastic working method.

[0002]

2. Description of the Related Art In recent years, high-temperature plastic working such as hot rolling, hot forging, hot die working, and hot pressing of steel materials such as carbon steel and stainless steel and non-ferrous metal materials such as aluminum and titanium has been carried out by using tools. In order to protect the lubrication, a lubricant for high-temperature plastic working has been used to reduce the effect. Examples of the lubricant include solid lubricants such as graphite, glass, boron nitride, mica, molybdenum disulfide, iron oxide, fluorinated graphite, and calcium carbonate, which have a lubricating effect at high temperatures; sulfurized oils and fats, sulfurized olefins, zinc dialkyldithiophosphates , An extreme pressure agent such as a phosphate ester; an oiliness improver such as a mineral oil, a fat or oil, a fat polymer or a synthetic ester; at least one kind of an adhesion improver such as a methacrylate copolymer or a butylene butadiene copolymer and a pour point depressant; In addition, antioxidants (alpha naphthylamine, di-tert-butylphenol, etc.)
Is generally used.

In the above-mentioned high-temperature plastic working, the temperature of a material to be processed such as a steel material or a non-ferrous metal is in a range of 700 to 1200 ° C. At such a temperature, the extreme pressure agent or the oiliness improver causes oxidation or thermal decomposition, and cannot exert a sufficient effect on a lubricating surface. Therefore, it is more difficult to obtain a sufficient lubricating effect in high-temperature plastic working than in low-temperature plastic working. JP-B-62-39198 and JP-B-62-39199 disclose hot-rolling lubricants containing calcium carbonate powder whose surface has been modified with a surfactant.
Japanese Patent No. 234991 discloses a lubricant for high-temperature plastic working containing calcium carbonate and iron oxide particles, but the lubricating performance of these lubricants is not always sufficient.

[0004]

SUMMARY OF THE INVENTION An object of the present invention is to provide high-temperature plastic working, such as hot rolling, hot forging, hot die working, and hot pressing, of a work material such as a steel material or a non-ferrous metal material. Provides a lubricant for high-temperature plastic working that does not cause roughening or wear of the tool due to insufficient lubrication when lubricated by direct application or air spray method, water injection method, etc. to both or one of the tool and the material It is to be.

[0005]

The object of the present invention is attained by a lubricant for high-temperature plastic working characterized by containing a solid lubricant surface-treated with a titanium-based and / or aluminum-based surface treating agent. . The lubricant for high-temperature plastic working of the present invention preferably contains at least one of a base oil and a base grease, and a solid lubricant surface-treated with a titanium-based and / or aluminum-based surface treatment agent.

[0006]

DESCRIPTION OF THE PREFERRED EMBODIMENTS Base oils used in the present invention include mineral oils (spindle oil, machine oil, cylinder oil, etc.) and synthetic esters (fatty acid octyl ester, trimethylolpropane fatty acid ester, pentaerythritol fatty acid ester, etc.). Or a mixture of two or more kinds of oils and fats (eg, rapeseed oil, beef tallow, lard, etc.) and polymerized oils and fats (eg, soybean polymerized oil, rapeseed polymerized oil, castor polymerized oil, etc.). Each of these base oils has a function of forming a lubricating film between a roll and a lubricant, lowering a coefficient of friction, and suppressing roughening and seizure of a tool.

The base grease used in the present invention includes:
Metal soaps such as lithium soap and aluminum soap, and non-soap thickeners such as polyurea and organic bentonite are used as thickeners, and mineral oil and dioctyl sebacate and Among the synthetic oils such as pentaerythritol laurate tetraester, those using one or more base oils are desirable. Each of these base greases has a function of forming a lubricating film between a roll and a lubricant, lowering a coefficient of friction, and suppressing roughening and seizure of a tool. In the lubricant of the present invention, the amount of base oil and / or base grease to be added is preferably 10.0% by weight or more, more preferably 100.0% by weight or less.
0 to 99.0% by weight. When adding the base grease to the lubricant, it is preferable that the thickener is present in the lubricant in an amount of 0.1% by weight or more.

The solid lubricant used in the present invention includes particles such as calcium carbonate, graphite, carbon black, talc, glass, boron nitride, mica, molybdenum disulfide, iron oxide, and fluorinated graphite. The particle size is
It is 20 μm or less. When adding and dispersing in a lubricant,
This is because the smaller the particle size, the more stable the dispersion. Most preferred is calcium carbonate.
Hereinafter, the present invention will be described with reference to an example in which calcium carbonate is used as a solid lubricant, but the present invention is not limited to this. The calcium carbonate used in the present invention may be a known substance, either heavy calcium carbonate obtained from nature or precipitated calcium carbonate obtained by synthesis, or a mixture thereof. The particle size of the calcium carbonate is preferably 20 μm
The thickness is more preferably 10 μm or less.

The solid lubricant used in the present invention is obtained by treating the particle surface with a metal surface treating agent. Specific examples of such metal-based surface treatment agents include titanium-based and aluminum-based surface treatment agents. In the present invention, a solid lubricant surface-treated with a titanium-based surface treating agent and a solid lubricant surface-treated with an aluminum-based surface treating agent can be mixed and used. The metal-based surface treatment agent more preferably has at least one of a functional group such as an alkoxy group, a hydroxyl group, an acetate group, and a pyrophosphate group.

Examples of commercially available titanium-based surface treating agents include isopropyl triisostearoyl titanate (K
R-TTS: Ajinomoto Co., Ltd.), bis (dioctyl pyrophosphate) titanate (138S: Nippon Soda Co., Ltd.), isopropoxy (2-ethylhexanediolato) titanium (TOG: Nippon Soda Co., Ltd.) , Tetraisopropoxytitanium (A-1: Nippon Soda Co., Ltd.), tetra-n-butoxytitanium (B-1: Nippon Soda Co., Ltd.)
And tetrakis (2-ethylhexyloxy) titanium (TOT: manufactured by Nippon Soda Co., Ltd.). Examples of commercially available aluminum-based surface treating agents include acetoalkoxyaluminum diisopropylate (ALM: Ajinomoto). Co., Ltd.).

In order for the solid lubricant surface-treated with such a surface treatment agent to exhibit a sufficient lubricating effect, it is necessary that the surface-treated solid lubricant be an effective component in the surface treatment agent. , Titanium and / or aluminum is preferably 1.5 × 10 ^-3 % by weight in the surface-treated solid lubricant
Above, more preferably 1.0 × 10 ^{-2 to} 3.0 × 10
^-1 % by weight is desirable.

The method of treating the surface of the solid lubricant particles with this surface treatment agent is not particularly limited, and may be a wet method, a dry method, a spray method, etc., which have been conventionally performed as this type of surface treatment method. Can be adopted. For example, a specific method will be described by taking a case where the surface treatment is performed by a wet method as an example.First, a solid lubricant powder is dispersed in a predetermined solvent such as hexane or benzene, and a predetermined amount in the dispersion, for example, , 0.5 to 2.0% by weight of a surface treatment agent, and stirred at 10 to 30 ° C. for 10 to 30 minutes.
By removing the solvent in a constant temperature bath and drying at 80 ° C. for 24 hours, a surface-treated solid lubricant powder can be easily obtained. These surface-treated solid lubricants are preferably contained in the lubricant for high-temperature plastic working of the present invention in an amount of preferably 1% by weight or more, more preferably 3 to 80% by weight. When the amount is less than 1% by weight, the effect of the addition is not sufficiently exhibited. The upper limit is not particularly limited, but is usually 90% by weight or less.

The lubricant for high-temperature plastic working of the present invention can further improve lubricity by adding a lubricating oil additive. Specific examples of such additives include extreme pressure agents (zinc dialkyldithiophosphate, molybdenum carbamate, zinc such as cobalt octylate,
Oil-soluble organometallic compounds containing molybdenum, cobalt, etc., sulfur compounds such as sulfurized oils and fats, and sulfur compounds such as didodecyl polysulfide, phosphorus compounds such as phosphate esters, phosphite esters and acid phosphate esters), viscosity index improvers (poly Isobutylene, polymethacrylate, etc.) and antioxidants (alpha-naphthylamine, ditert-butylphenol, etc.). Specifically, one or more of these are added and dispersed for use. The amount of these additives is not particularly limited, but is usually 1 to 3 in the high-temperature plastic working lubricant.
30% by weight.

According to the high-temperature plastic working method of the present invention, the lubricant of the present invention is sprayed onto both or one of the roll materials by a gear type or plunger type pump generally used as a lubricant pump. , Refueling by water injection method,
This makes it possible to prevent high-temperature plastic working of the steel material, for example, seizure, abrasion, and roughening of the roll during hot rolling. It is appropriate that the refueling amount is about 0.01 to 1.0 L / min.

The lubricant of the present invention comprises a stainless steel heating pot having a stirrer, a base oil, a base grease, a solid lubricant surface-treated with a titanium-based and / or aluminum-based surface treatment agent, a lubricant additive, and the like. , At the desired weight ratio, 50
It can be easily produced by stirring at ８０80 ° C. for 30 minutes to 2 hours.

[0016]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be described below by way of examples, taking hot rolling of steel as an example, but the present invention is not limited thereto. In a stainless steel heating pot having a stirrer, solid lubricants, base oils, and base greases shown in Tables 1 to 5 were added.
5 and the mixture was stirred at 60 ° C. for 1 to 2 hours to produce the lubricants of Examples 1 to 17 and Comparative Examples 1 to 9. The lubricant was supplied to the roll surface of a double hot rolling mill using a lubricant oil supply system of an air spray method using a gear pump under the following hot rolling conditions and lubricant oil supply amount.

Hot Rolling Conditions and Lubricating Oil Amount Rolling Roll High Carbon High Alloy Cast Iron Roll 150mmΦ × 150mmL Rolled Material SUS430 Steel Plate Thickness 4mm Width 25mm Length 100mm 200 Rolls (Rolled at the Same Location of Roll) Speed 10%, 14mpm Steel heating temperature 1000 ° C Finished thickness 3.6mm Lubricating oil amount A total of 0.1 L / min for upper and lower rolls Lubricating oil pump model Gear pump

[0018]

The lubricant of the present invention is more effective in controlling the seizure, wear and roughening of the tool than in the conventional hot rolling lubricant, especially in hot rolling of steel.

[0019]

[Table 1] Composition of lubricant Example 1 2 3 4 5 6 Solid lubricant Heavy calcium carbonate (1)------(2)---50--(3) 350 88--- (4) - - - - 50 - (5) - - - - - 50 Base oil (1) 97 50 12 - - 50 (2) - - - 50 - - (3) - - - - 50 - extreme pressure agent − − − − − − Lubricant consistency grade No. − 00 3 00 00 00 Lubricant viscosity 100 − − − − − Roughness ○ ○ ○ ○ ○ ○ Wear ○ ○ ○ ○ ○ ○ Burn-in ○ ○ ○ ○ ○ ○

[0020]

[Table 2] Composition of lubricant Example 7 8 9 10 11 12 Solid lubricant Heavy calcium carbonate (1)------(2)------(3)--50.0 50.0 50.0 80.0 (6) 50.0----- (7)-50.0---- Base oil (1) 50.0 50.0--38.0-(2)-----10.0 (3)-----10.0 grease ( 1)--50.0---(2)----10.0- (3)---50.0-- Extreme pressure agent----2.0- Lubricant consistency grade No. 00 00 222 Agent viscosity ------Roughness ○ ○ ○ ○ ○ ○ Abrasion ○ ○ ○ ○ ○ ○ Seizure ○ ○ ○ ○ ○ ○

[0021]

[Table 3] Composition of lubricant Example 13 14 15 16 17 Solid lubricant Heavy calcium carbonate (1)-----(2)-----(3)---1.5-(7) 3.0 − − − − (8) − 3.0 − − − Mica (1) − − 1.5 1.5 3.0 (2) − − 1.5 − − Base oil (1) 97.0 97.0 97.0 97.0 − Base grease (1) − − − − 97.0 pole Pressure agent − − − − − Lubricant consistency grade No. − − − − 0 Lubricant viscosity 100 100 100 100 − Roughness ○ ○ ○ ○ ○ Wear ○ ○ ○ ○ ○ Seizure ○ ○ ○ ○ ○

[0022]

[Table 4] Composition of lubricant Comparative example 1 2 3 4 5 6 Solid lubricant Heavy calcium carbonate (1)---50.0--(2) 0.5-----(3)------ (4)-0.5---- (5) ------(6)--0.5---(9)----50.0- (10)-----50.0 Base oil (1) 99.5 99.5 99.5 50.0 50.0 50.0 Extreme pressure agent − − − − − − Lubricant consistency grade No. − − − 00 00 00 Lubricant viscosity 60 60 60 − − − Roughness × × × × × × Wear × × × × × × Burn-in × × × × × ×

[0023]

[Table 5] Composition of lubricant Comparative example 7 8 9 10 Solid lubricant Heavy calcium carbonate (1)--50.0- (8)-50.0-- Mica (1) 0.5 ---Base oil (1) 99.5 50.0 − −Base grease (1) − − 50.0 −Extreme pressure agent − − − −Lubricant consistency grade No. −00 00 −Lubricant viscosity 60 − − −Roughness × × × × Wear × × × × Seizure × × × ×

Heavy calcium carbonate (1) Isopropyl triisostearoyl titanate (KR-TTS: manufactured by Ajinomoto Co., Inc.) (Amount of surface treating agent in solid lubricant (adsorption amount) = 0.01% by weight; Solid lubrication titanium amount = 5.1 × 10 ^-4 wt%) in the dosage (2) isopropyl titanate (KR-TTS: Ajinomoto Co., Ltd.) (the amount of the surface treatment agent in a solid lubricant (adsorption ) = 0.03% by weight; the amount of titanium in the solid lubricant = 1.6 × 10 ⁻³ % by weight) (3) Isopropyl triisostearoyl titanate (KR-TTS: manufactured by Ajinomoto Co., Inc.) (solid lubricant) Amount (adsorption amount) of surface treatment agent in the liquid = 0.80% by weight; amount of titanium in the solid lubricant = 4.2 × 10 ^-2 % by weight) (4) Isopropyl triisostearoyl titanate (KR-TTS: Ajinomoto Co., Inc. (Amount of surface treatment agent in solid lubricant (adsorption amount) = 3.50% by weight; Amount of titanium in solid lubricant = 1.8 × 10 ^-1 % by weight) (5) Bis (dioctyl pyrophosphate) ) Titanate (138S: manufactured by Nippon Soda Co., Ltd.) (Amount of surface treating agent in solid lubricant (adsorption amount) = 0.20% by weight; Amount of titanium in solid lubricant = 9.2 × 10 ⁻³⁾ weight%)

(6) Bis (dioctyl pyrophosphate) titanate (138S: manufactured by Nippon Soda Co., Ltd.) (Amount of surface treating agent in solid lubricant (adsorption amount) = 2.00% by weight; (Amount of titanium = 9.2 × 10 ^-2 wt%) (7) Acetoalkoxyaluminum diisopropylate (ALM: manufactured by Ajinomoto Co.) (Amount (adsorption amount) of surface treatment agent in solid lubricant = 1. 50% by weight; amount of aluminum in solid lubricant = 2.0 × 10 ^-1 % by weight) (8) γ-aminopropyltriethoxysilane (TSL)
8331: Toshiba Silicone Co., Ltd.) (Amount of surface treatment agent in solid lubricant (adsorption amount) = 1.00% by weight; Amount of titanium or aluminum in solid lubricant = 0% by weight) (9) Olein Acid (amount of surface treatment agent in solid lubricant (adsorption amount) = 1.00% by weight; amount of titanium or aluminum in solid lubricant = 0% by weight) (10) No surface treatment

Mica (1) Isopropyl triisostearoyl titanate (KR-TTS: manufactured by Ajinomoto Co.) (Amount of surface treating agent in solid lubricant (adsorption amount) = 0.50% by weight; (Amount of titanium = 2.6 × 10 ⁻² wt%) (2) Acetoalkoxyaluminum diisopropylate (ALM: manufactured by Ajinomoto Co.) (Amount (adsorption amount) of surface treatment agent in solid lubricant = 0. 50% by weight; amount of titanium in solid lubricant = 6.7 × 10 ^-2 % by weight) Base oil (1) Mineral oil (ISO VG46) (2) Trimethylolpropane triolate (3) Rapeseed oil

Base grease (1) Lithium soap grease using mineral oil as base oil (contains 3% by weight of thickener lithium soap) NLGI consistency
No. 0 (2) Lithium soap grease using mineral oil as base oil (Thickening agent containing 11% by weight of lithium soap) NLGI consistency No. 3 (3) Bentonite grease using mineral oil as base oil (thickening agent) Contains 4% by weight of bentonite) NLGI consistency No.
0 Extreme Pressure Agents Zinc dialkyldithiophosphate lubricants have an NLGI consistency grade at 25 ° C. The viscosity of the lubricant is at 25 ° C. (unit is centipoise). Roughness: indicates the presence or absence of roughening on the roll surface after rolling. ：: No rough surface, ×: There is rough surface Abrasion: Indicates the presence or absence of abrasion on the roll surface after rolling. ：: no abrasion, ×: abrasion seizure: the presence or absence of seizure on the roll surface after rolling. ○: No burn-in, ×: Burn-in

Continued on the front page (51) Int.Cl. ⁶ Identification code FI C10M 117: 00 103: 06 139: 00) C10N 10:02 10:04 10:06 10:08 20:06 30:06 30:08 40: 24 50:10

Claims (5)

[Claims] 1. A lubricant for high-temperature plastic working, comprising a solid lubricant surface-treated with a titanium-based and / or aluminum-based surface treatment agent. 2. The high-temperature plastic working lubricant according to claim 1, comprising at least one of a base oil and a base grease, and a solid lubricant surface-treated with a titanium-based and / or aluminum-based surface treatment agent. 3. A solid lubricant surface-treated with a titanium-based and / or aluminum-based surface treating agent is used to convert titanium and / or aluminum to 1.5 × 10 ^-3 % by weight or more based on the total weight of the solid lubricant. 3. The lubricant for high-temperature plastic working according to claim 1, wherein the solid lubricant is a titanium and / or aluminum component originally contained). 4. The lubricant for high-temperature plastic working according to claim 1, wherein the solid lubricant is calcium carbonate. 5. The high-temperature plastic working lubricant according to any one of claims 1 to 4, which is lubricated to a tool surface during high-temperature plastic working of a material to be processed, thereby seizing, abrasion, and roughening of the tool surface. , A high-temperature plastic working method characterized by preventing.