JPH1150078A - Lubricant for metal plastic working - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain a lubricant manifesting excellent lubricity in the plastic working of a steel material and a nonferrous metal, and capable of preventing tool wear or the like by including highly basic alkaline earth metal salicylate and a load bearing additive. SOLUTION: This lubricant includes (A) a highly basic alkaline earth metal salicylate and (B) a load bearing additive (for example, a metal carboxylate, an organometallic extreme-pressure additive, and a sulfur-based extreme pressure agent). In the lubricant, the base number of the entire composition is preferably >=90 mgKOH/g, and when the component A with 100-400 mgKOH/g base number is used, the content of component A becomes 30-90 wt.%. The content of component B is preferably 1-40 wt.%. The lubricant or the like for the warm forging comprising 30-95 wt.% component A, 5-40 wt.% component B, and the remainder of the lubricant base oil, and having >=90 mgKOH/g base number of the entire composition are cited as a preferable example of the lubricant.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a metal plastic working which exhibits excellent lubricity in the plastic working of steel and non-ferrous metal, and can prevent seizure of a work material on a tool surface and tool wear. It concerns lubricants.

[0002]

2. Description of the Related Art In plastic working such as forging, rolling, die working and press working of steel materials and non-ferrous metal materials, lubricants for metal plastic working have been conventionally used to protect tools. For warm and hot working, a black solid lubricant such as graphite or molybdenum disulfide dispersed in oil is used. Lubricants dissolved therein have been used. But,
Due to the increasing interest in environmental issues in recent years, the contamination of the working environment derived from black solid lubricants, the carcinogenicity of chlorine-based load-bearing additives themselves and the waste oil combustion treatment of lubricants containing them have Dioxin generated is a problem.

[0003]

SUMMARY OF THE INVENTION In order to solve this problem, the present invention does not use a black solid lubricant and a chlorine-based load-carrying additive, and provides lubrication characteristics equivalent to or better than those using them. An object of the present invention is to provide a lubricant for metal plastic working.

[0004]

SUMMARY OF THE INVENTION The present invention provides a lubricant for metal plastic working containing a highly basic alkaline earth metal salicylate and a load-bearing additive.

[0005]

BEST MODE FOR CARRYING OUT THE INVENTION The lubricant for metal plastic working of the present invention preferably has a base number of at least 90 mgKOH / g, more preferably at least 150 mgKOH / g, most preferably at least 200 mgKOH / g. . Accordingly, the highly basic alkaline earth metal salicylate used in the present invention has a sufficiently high base number such that the base number of the entire composition to which the load-bearing additive and optionally the base oil are added is 90 mgKOH / g or more. It is desirable to use a high one.

Particularly preferred examples of the highly basic alkaline earth metal salicylate used in the present invention are those represented by the following formula. [R ¹ R ² C ₆ H ₂ (OH) -COO-M ¹ -OOC-C ₆ H ₂ (OH) R ³ R ⁴ ] n ・ (M ² CO ₃ ) m where M ¹ and M ² are the same And may be different, and represent an alkaline earth metal (eg, calcium, magnesium, barium). Although the same effect can be obtained by using any of the alkali metals, calcium is most preferable from the viewpoint of economy. R ¹ and R ³ may be the same or different and represent an alkyl group having 5 to 28 carbon atoms or an aryl group having 6 to 30 carbon atoms, and R ² and R ⁴ may be the same or different and each have a hydrogen atom And an alkyl group having 1 to 28 carbon atoms or an aryl group having 6 to 30 carbon atoms. m / n is 0.2 to 12. Commercially available highly basic alkaline earth metal salicylates include OSCA 438B and OSC
A435B, OSCA463, OSCA431B, SAP005 manufactured by Shell Chemical Company, and the like.

The load-bearing additive used in the present invention includes metal carboxylate; organometallic extreme pressure additive; sulfur extreme pressure agent; polycarboxylic acid or its anhydride having an effect of improving adhesion. No. As the metal carboxylate,
C 6-34 aliphatic carboxylic acid or C 7-34
And a metal salt of an aromatic carboxylic acid having 6 to 3 carbon atoms.
Examples of the aliphatic carboxylic acid of 4 or the aromatic carboxylic acid having 7 to 34 carbon atoms include caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, stearic acid, behenic acid, lignoceric acid, serotinic acid, and oleic acid. Acid, linoleic acid, linolenic acid, ricinoleic acid, palmitoleic acid, 2-ethylhexylic acid, branched pelargonic acid, branched lauric acid, branched tridecanoic acid, branched palmitic acid, branched oleic acid, branched stearic acid, naphthenic acid, dimer acid, benzoic acid Examples include acids, hydroxybenzoic acid, isophthalic acid, terephthalic acid, and benzoic acid having an alkyl group having 5 to 24 carbon atoms. In addition, each carboxylic acid may be single or a mixture. Examples of the mixture include, for aliphatic carboxylic acids, natural fats and oils (tallow, lard, palm oil, etc.) directly saponified and decomposed into tallow, lard,
It is also possible to use palm oil direct fatty acids and the like. Examples of the metal salts include alkali metal salts (lithium salt, sodium salt, potassium salt, etc.), alkaline earth metal salts (magnesium salt, calcium salt, barium salt, etc.), and other metal salts (eg, zinc, tin, etc.). Aluminum, lead, copper,
Metal salts such as nickel and molybdenum).

As an organometallic extreme pressure additive, dialky
Metal salt of dithiophosphoric acid, gold dialkyldithiocarbamate
Genus salt, 2-mercaptobenzothiazole metal salt, alk
Tin sulfide and the like.
Nesium, calcium, barium, zinc, tin, aluminum
Metal salts such as lead, copper, nickel and molybdenum
Can be As sulfur-based extreme pressure agents, powdered sulfur, sulfurized fats and oils,
Sulfurized olefin, sulfurized mineral oil, dialkyl disulfite
And dialkyl polysulfides. Adhesion
Polycarboxylic acid and its anhydride with the effect of improving the durability
The carbon number of 8 to 200, preferably 12 to 100
And especially preferred are aliphatic carboxylic acid anhydrides. For example,
Octenyl succinic anhydride, dodecenyl succinic anhydride
Thing, C₁₃Alkenyl succinic anhydride, C₂₈Alkenylco
Succinic anhydride, C₄₃Alkenyl succinic anhydride, C₇₂A
Lucenyl succinic anhydride, C₉₀Alkenyl succinic anhydride
Thing, C ₁₀₀Succinic anhydrides such as alkenyl succinic anhydride
Alkenyl having at least one alkenyl group bonded to an acid
Succinic anhydride is preferred. These succinic anhydrides are public
Known ones such as polyisobutylene α-olefin
Such as those produced by maleating
Can be

Examples of lubricant base oils used in the present invention include medium and heavy mineral oils such as spindle oil, machine oil, dynamo oil, motor oil, cylinder oil, bright stock oil; tallow, lard, whale oil Animal and vegetable fats and oils such as palm oil, coconut oil, rapeseed oil, rice bran oil, soybean oil;
Esters of two fatty acids and monohydric or polyhydric alcohols; synthetic oils such as poly-α-olefins, polybutenes, silicone oils, and fluorine oils; and mixtures thereof.

In the lubricant of the present invention, the content of the highly basic alkaline earth metal salicylate is such that the base number of the whole composition is preferably at least 90 mgKOH / g, more preferably at least 150 mgKOH / g, most preferably at least 200 mgKOH / g. / g or more. Commercially available, base number is 100
When a highly basic alkaline earth metal salicylate of ~ 400 mg KOH / g is used, its content is preferably
It is 99% by weight, more preferably 30 to 95% by weight. The content of the load-bearing additive is preferably 1 to 4
0% by weight, more preferably 5 to 40% by weight. If the base number of the whole composition is less than 90 mgKOH / g, the seizure resistance may not be sufficient, and if the content of the load-bearing additive is less than 1% by weight, the seizure resistance may also be insufficient. There is. In addition, even if the content of the load-bearing additive exceeds 40% by weight, the effect corresponding to the increase in the added amount cannot be expected and it is not economical. Preferred examples of the lubricant of the present invention include 30 to 95% by weight of a highly basic alkaline earth metal salicylate, 5 to 40% by weight of a load-carrying additive, and the remainder consisting of a lubricant base oil. A lubricant for warm forging, a lubricant for hot forging, and a lubricant for cold forging, each having a base number of 90 mgKOH / g or more.

The lubricant of the present invention can be easily produced by mixing and stirring the above components in a suitable container. The lubricant of the present invention may further contain ordinary amounts of additives used in ordinary lubricants, such as solid lubricants, viscosity index improvers, and antioxidants. The lubricant of the present invention thus obtained can be supplied to a mold by a gear pump, a plunger pump, or the like generally used as a lubricant pump. Further, the coating may be performed with a brush or the like without using a pump.

[0012]

The present invention will be described more specifically with reference to examples and comparative examples. Examples 1-26, Comparative Examples 3-8 A highly basic calcium salicylate, a load-bearing additive, and a base oil were placed in a stainless steel heating kettle equipped with a stirrer, as shown in Tables 1 to 6.
6 was added, and the mixture was stirred for 10 minutes to 1 hour until it became uniform at a dissolution temperature (50 to 180 ° C.) specific to each load-bearing additive to produce a lubricant. Comparative Example 2 The components shown in Table 5 were charged into a stainless steel heating pot equipped with a stirrer, slurried, and then subjected to two passes at 350 kgf / cm ² with a Monton-Gaulin homogenizer to produce a lubricant. A performance test was performed on the above lubricant and a commercially available lubricant dispersed in graphite oil (Comparative Example 1) by the following method. The results are shown in Tables 1 to 6. Examples 1 to 22 and Comparative Examples 1 to 6 are lubricants for warm and hot forging.
3 to 26 and Comparative Examples 7 and 8 are lubricants for cold forging.

Formability test (backward extrusion test) (for warm and hot working) Forging was carried out using a 160-ton press under the following conditions, and the load (ton) during working and the dimensions (mm) of the work ) And forging formability is determined from the presence or absence of seizure. The smaller the value of the load and the size and the less the seizure, the better the performance as a lubricant. (Test conditions)-Press machine: KOMATSU MAYPRES (MKN-160)-Die material: Carbide-Die size: Punch diameter 25mmφ, Die inner diameter 30mmφ-Test piece: S45C (diameter 30mm, thickness 16mm) ・ Processing speed: 32.5 mm / sec ・ Cross-sectional reduction rate: 70% ・ Workpiece dimension setting: The bottom thickness (bottom thickness) of the cup processed with the sample of Comparative Example 2 is 3.35 mm (at 750 ° C.) 2.35mm (11
(At 00 ° C).

(Evaluation) Moldability: In correspondence with Comparative Example 2, at 750 ° C.
Bottom thickness 3.35mm or less, load 90t or less. 1100 ° C, bottom thickness 2.
35mm or less, load 45t or less. -Seizure resistance: The seizure state of the die after the forging test was observed and evaluated according to the following five grades. (If it is 問題 to □, there is no practical problem.) ：: There is no seizure at all. ：: almost no burn-in □: Burn-in is slightly recognized. Δ: Burn-in is recognized. X: Burning is remarkably observed.

[0015] Lubricity test (Soda type four-ball test) (for cold working) Test method: Soda type four-ball test (JIS K 2519) Test steel ball: SUJ-2 Advanced 3/4 (basic diameter 19.05mm) (JIS B 1
501) Test condition: 1000 rpm × 10 min × 3 kgf / cm ² Evaluation: Wear scar diameter After performing the test under the above test conditions, the wear scar diameter of the fixed sphere was measured by using a microscope and the sliding direction and the direction perpendicular to it. To 0.01
The average value was rounded to the nearest 0.01 mm, and this was taken as the wear scar diameter. The seizure state of the mold after the seizure resistance forging test was observed and evaluated according to the following five grades. (◎
If it is ~ □, there is no practical problem. ◎: No image sticking. ：: almost no burn-in □: Burn-in is slightly recognized. Δ: Burn-in is recognized. X: Burning is remarkably observed.

High Temperature Adhesion Confirmation Test (for Warm and Hot Working) A test piece assuming a mold is heated to a specified temperature, 0.1 ml of a lubricant is dropped with a syringe, and the upper limit temperature at which adhesion is possible is confirmed. . (Evaluation) ：: adheres even at 500 ° C. or higher. Δ: adhered in the range of 450 ° C. or more and less than 500 ° C. ×: No adhesion at 450 ° C. or higher. Contamination around equipment (for warm and hot working)

[0017]

[Table 1] Examples1 2 3 4 5 6 Highly basic Ca salicylate ¹⁾ 97 97 75 75 75 75 Load-bearing additive zinc 2-ethylhexylate--20---aluminum oleate 1--10--aluminum stearate----10-sodium tallow fatty acid sodium fatty acid-----20 calcium naphthenate--- 5 − − Zinc dialkyldithiophosphate − − − − − − Dialkyl polysulfide − 3 − − − − Sulfurized oil and fat − − − − − − Alkyl tin sulfide − − − − − − −Alkenyl succinic anhydride------ Base oil Refined mineral oil (VG460) 2 − 5 − − −Trimethylol propane triolate − − − 10 15 5 Base number of composition (mgKOH / g) 310 310 240 240 240 240 Formability (bottom thickness mm / load t) Warm (750 ° C) 3.28 / 80 3.28 / 79 3.28 / 79 3.28 / 78 3.26 / 77 3.28 / 79 Hot (1100 ℃) 2.29 / 39 2.27 / 39 2.28 / 38 2.28 / 38 2.27 / 37 2.27 / 37 Burning (750 ℃ / 1100 ℃) ◎ / ◎ ◎ / ◎ ◎ / ◎ ◎ / ◎ ◎ / ◎ ◎ / ◎ High temperature adhesion ○ ○ ○ ○ ○ ○ Contamination around equipment ○ ○ ○ ○ ○ ○ 1) Highly basic calcium salicylate (base value 320mgKOH / g)

[0018]

[Table 2] Examples7 8 9 10 11 12 Highly basic Ca salicylate ¹⁾ 75 75 75 75 75 75 Load-bearing additive zinc 2-ethylhexylate------aluminum oleate------aluminum stearate-----10 sodium tallow fatty acid sodium fatty acid------calcium naphthenate--- − − − Zinc dialkyldithiophosphate 10 − − − 15 Dialkyl polysulfide − 10 − − − − Sulfurized oil and fat − − 5 − − − Alkyl tin sulfide − − − 20 − −Alkenyl succinic anhydride------ Base oil Refined mineral oil (VG460) 15 15 10 5 24 −Trimethylol propane triolate − − 10 − − 10 Base number of composition (mgKOH / g) 240 240 240 240 240 240 Formability (bottom thickness mm / load t) Warm (750 ° C) 3.26 / 77 3.26 / 78 3.30 / 82 3.28 / 79 3.30 / 82 3.25 / 76 Hot (1100 ℃) 2.28 / 37 2.27 / 37 2.31 / 40 2.28 / 39 2.31 / 40 2.26 / 37 Burning (750 ℃ / 1100 ℃) ◎ / ◎ ◎ / ◎ ◎ / ◎ ◎ / ◎ ◎ / ◎ ◎ / ◎ High temperature adhesion ○ ○ ○ ○ ○ ○ Contamination around equipment ○ ○ ○ ○ ○ ○

[0019]

[Table 3] Examples13 14 15 16 17 18 Highly basic Ca salicylate ¹⁾ 75 50 50 30 30 30 Load-bearing additive zinc 2-ethylhexylate--5 10 40-aluminum oleate------aluminum stearate-----3 sodium tallow fatty acid sodium fatty acid------calcium naphthenate 20 10- 10--Zinc dialkyldithiophosphate------Dialkyl polysulfide 5-----Sulfurized oil------Alkyl tin sulfide------Alkenyl succinic anhydride------ Base oil Refined mineral oil (VG460)-20 45 50 30 57Trimethylol propane triolate − 20 − − − 10 Base number of composition (mgKOH / g) 240 160 160 96 96 96 Formability (bottom thickness mm / load t) Warm (750 ° C) 3.26 / 77 3.32 / 85 3.32 / 86 3.32 / 86 3.29 / 82 3.33 / 86 Hot (1100 ℃) 2.26 / 38 2.33 / 41 2.32 / 42 2.23 / 42 2.28 / 39 2.34 / 42 Burn-in (750 ° C / 1100 ° C) ◎ / ◎ ◎ / ◎ ◎ / ◎ ○ / ◎ ○ / ◎ ○ / ◎ High temperature adhesion ○ ○ ○ ○ ○ ○ Contamination around equipment ○ ○ ○ ○ ○ ○

[0020]

Example 19 20 21 22 Highly basic Ca salicylate ¹⁾ 30 75 75 75 Load-bearing additive zinc 2-ethylhexylate----Aluminum oleate----Aluminum stearate--10-Tallow direct Fatty acid sodium salt---5 Calcium naphthenate----Zinc dialkyldithiophosphate--5 10 Dialkyl polysulfide 5---Sulfurized oil-20--Alkyl tin sulfide---- Alkenyl succinic anhydride-5 5 5 Base oil Refined mineral oil (VG460) 50 − − − Trimethylol propane triolate 15 − 55 Base number of composition (mgKOH / g) 96 240 240 240 Formability (bottom thickness mm / load t) Warm (750 ° C) 3.28 / 80 3.28 / 79 3.25 / 76 3.26 / 77 Hot (1100 ℃) 2.27 / 38 2.27 / 38 2.24 / 35 2.25 / 36 Burn-in (750 ℃ / 1100 ℃) ○ / ◎ ◎ / ◎ ◎ / ◎ ◎ / ◎ High temperature adhesion ○ ○ ○ ○ Contamination around equipment ○ ○ ○ ○

[0021]

[Table 5] Comparative example1 2 3 4 5 6 Highly basic Ca salicylate ¹⁾ --40 60 20- Graphite (particle size 5μ) − 30 − − − − − Base oilMineral oil A (ISO VG 46)-70 60 40 80 100 Base number of composition (mgKOH / g) − − 128 192 64 0 Formability (bottom thickness mm / load t) Warm (750 ° C) 3.27 / 78 3.35 / 90 3.34 / 89 3.33 / 86 3.36 / 92 3.47 / 101 Hot (1100 ℃) 2.27 / 38 2.35 / 45 2.35 / 43 2.34 / 42 2.37 / 45 2.45 / 49 Burning (750 ℃ / 1100 ℃) ◎ / ◎ △ / □ △ / △ △ / □ × / □ × / × High temperature adhesion ○ △ ○ ○ △ × Contamination around equipment × × ○ ○ ○ ○ Comparative Example 1 is a commercially available lubricant dispersed in graphite oil.

[0022]

[Table 6] Example Comparative example23 24 25 26 7 8 Highly basic Ca salicylate ¹⁾ 40 40 40 40 − − Load-bearing additive Zinc dialkyldithiophosphate 10 10 5 −10 − Dialkyl polysulfide − − − 5 − − Sulfurized fat (S = 10%) − − − − 20 10Chlorinated paraffin (Cl = 50%) − − − − 40 40 Base oil Refined mineral oil (ISO VG40) 40 − 45 45 20 25 Refined mineral oil (ISO VG8) − 40 − − − 25 Trimethylol propane triolate 10 10 10 10 − −Refined rice bran oil − − − − 10 − Composition base number (mgKOH / g) 128 128 128 128 − − Lubricity (wear scar diameter: mm) 0.60 0.59 0.59 0.68 1.53 1.64 Seizure resistance ◎ ◎ ◎ ○ × ×

[0023]

Since the lubricant of the present invention does not use a black component such as graphite and a chlorine-based load-carrying additive, it does not pollute the working environment and the natural environment. In addition, the forgeability and other performance as a lubricant are equal to or higher than those of the graphite-based forging lubricant and the chlorine-based forging lubricant.

──────────────────────────────────────────────────の Continued on the front page (51) Int.Cl. ⁶ Identification code FI C10M 135/18 C10M 135/18 135/22 135/22 135/36 135/36 137/10 137/10 A 139/00 139 / 00 Z 163/00 163/00 // C10N 10:02 10:04 10:06 10:08 20:00 30:04 30:06 30:08 40:24

Claims (13)

[Claims] 1. A lubricant for metal plastic working comprising a highly basic alkaline earth metal salicylate and a load-bearing additive. 2. A highly basic alkaline earth metal salicylate of 30 to 99% by weight, a load-bearing additive of 1 to 40% by weight,
The balance consists of a lubricant base oil and the base number of the entire composition is 90
The lubricant for metal plastic working according to claim 1, wherein the lubricant is not less than mgKOH / g. 3. A highly basic alkaline earth metal salicylate of 30 to 95% by weight, a load-bearing additive of 5 to 40% by weight,
The remainder is composed of a lubricant base oil and is for warm forging.
The lubricant for metal plastic working as described above. 4. A highly basic alkaline earth metal salicylate of 30 to 95% by weight, a load-bearing additive of 5 to 40% by weight,
The remainder is composed of a lubricant base oil and is for hot forging.
The lubricant for metal plastic working as described above. 5. A highly basic alkaline earth metal salicylate of 30 to 95% by weight, a load-bearing additive of 5 to 40% by weight,
The remainder is composed of a lubricant base oil and is for cold forging.
The lubricant for metal plastic working as described above. 6. The lubricant base oil comprises at least one selected from the group consisting of mineral oils, synthetic oils, fats and oils and fatty acid esters.
The lubricant for metal plastic working according to any one of claims 1 to 5, comprising a seed. 7. The load-bearing additive comprises at least one selected from the group consisting of a metal carboxylate, a sulfur-based extreme-pressure additive, and an organometallic extreme-pressure additive. 2. The lubricant for metal plastic working according to claim 1. 8. The load-bearing additive is an aliphatic and / or aromatic monocarboxylic acid having 8 to 28 carbon atoms, Na, Ca,
The lubricant according to any one of claims 1 to 7, wherein the lubricant is a salt of Mg, Al, Zn, Ba, or Sn. 9. The lubricant for metal plastic working according to claim 1, wherein the load-bearing additive contains at least one selected from the group consisting of dialkyl polysulfides and sulfurized oils and fats. 10. The load-bearing additive may be a metal dialkyldithiophosphate, a metal dialkyldithiocarbamate,
The lubricant for metal plastic working according to any one of claims 1 to 7, comprising at least one selected from the group consisting of a metal salt of mercaptobenzothiazole and an alkyltin sulfide. 11. The lubricant according to claim 1, wherein the load-bearing additive is an aluminum carboxylate. 12. The lubricant for metal plastic working according to claim 1, wherein the load-bearing additive is a zinc dialkyldithiophosphate. 13. The method according to claim 1, which comprises a polycarboxylic acid or an anhydride thereof having an effect of improving adhesion.
A lubricant for metal plastic working as described in the above item.