JPH03263497A - Water-soluble hot lubricant composition - Google Patents

Abstract

PURPOSE:To obtain the title composition having excellent adhesion in a high- temperature range, reducing coefficient of friction between a tool or mold and a material, comprising a boric ester, obtained by reacting boric acid (anhydride) with an alkanolamine, as an essential component. CONSTITUTION:The objective composition comprising a boric ester, obtained by reacting (A) boric acid or boric anhydride with (B) an alkanolamine such as monoisopropanolamine or triethanolamine and/or a polyhydric alcohol such as ethylene glycol or neopentyl glycol, as an essential component.

Description

[Detailed description of the invention] [Industrial application field] The present invention relates to a lubricant for metal working.

For more details, for hot processing of metals, for more details, forging,
This relates to lubricants for steel pipe manufacturing and rolling.

[Prior Art] Generally, a lubricant for hot working is used for the purpose of reducing the coefficient of friction between a tool and a material and between a material and a mold during processing, and smoothing out the processing.

There are various types of lubricants, and they are roughly divided into oil-soluble and water-soluble. The former consists of mineral oil, fatty acids, animal and vegetable oils,
Some contain esters and extreme pressure additives, and if necessary, oil-based graphite is dispersed therein. The latter consists mainly of water with addition of alkali metal salts or amine salts of fatty acids (-basic acids, dibasic acids, or polybasic acids), water-soluble polymers, and extreme pressure additives, and as necessary. Some have inorganic salts or water-soluble graphite dispersed in them. However, in recent years, oil-soluble type lubricants have a high risk of fire, so there is a shift to water-soluble oils, but in hot working, the workpiece material
Water-soluble oils containing only organic substances have poor lubricity at high temperatures because they are heated to temperatures between 00 and 1,200 degrees Celsius, and if inorganic substances or graphite are added too much, the working environment deteriorates. 1. Product: It is undesirable because it leads to 1st sieve.

Problem 1 to be solved by the present invention The problem to be solved by the present invention is 1- In view of the current situation, what is the high temperature range during hot working? , Koyori-do 4 = 1 Excellent adhesion, 1 for tools / molds and material amount? Improved work environment by reducing the coefficient of friction and preventing wear of tools and molds. There is a lubricant that contributes significantly to this.

[Bottom page for solving the problem] In order to achieve ``1-4'' in item 1'', the inventors of Niki and others have conducted intensive research and found that a specific solution must be used. Otsu 1'
Depending on the organic and inorganic compounds, graphite, water-soluble items, etc. Schiff 1 discovered that a lubricant could be obtained and completed the present invention.

Accordingly, the present invention provides: (1) a boi'noic acid; a boi'noic acid or anhydride;
Reacting lukanolamine and at least one polyhydric alcohol having more than 10 hydric alcohols, the essential component c1-L, is characterized by having the essential component c1-L, '6-, and the bol'noic acid gostyl obtained by -1. 1. A water-soluble hot lubricant composition.

(2) The water-soluble hot lubricant composition according to the above (1), wherein the above-mentioned nistyl borate is contained in water at a concentration of 5 to 70%.

(3) Lubricated sleep! -+, the water-soluble hot lubricant composition according to (2), in which the components are further dispersed.

(4) Lubricant 11wjj, ingredients are Grapheye 1, metal.
2. The water-soluble 1:1 hot lubricant composition according to item 2 (1), (2) or (3), which is a lubricating powder such as solenoid, molybdenum sulfide, and other lubricating powders.

This is related to C4'.

[Function 11fi and structure of the invention] In the present invention, the above-mentioned boric acid or anhydride boric acid J
゛, alkanolamine and polyvalent alkyl-1- of divalent or higher valence
1. By dissolving and dispersing at least one type of boric acid eswort obtained by reacting with at least one type of boric acid ester in 5 to 70% by weight water, 1. An oil with excellent adhesion and lubricity in hot conditions. In cases where high adhesion and lubricity are not required, it has been conventionally done to add graphite, metal p-nogen, -27 L-bdenum sulfide, and other organic/inorganic powders, which serve as lubricity additive components. It's here. but,
When dispersing graphite, organic/inorganic powders, etc. in water, a considerable amount of water-soluble products (dispersants) were required, which led to a deterioration of the working environment. By using esters in combination with these lubricating ingredients,
For example, boric acid (old × 4
%) can be added in an amount of 5 to 20% or more, and the above-mentioned boric acid, ]-ster, etc., which should contribute to the lubrication of graphite in the hot state (900'C or higher), can be added. When used together, Q is more common than in the case of German and German, and it also has an advantage in terms of lubrication. , - These are "Boric acid esters act as good solvents for boric acid, and when supplied in a hot state, undergo thermal decomposition and release inorganic boron compounds.
t composition, 2. Combined with the aforementioned boric acid, it forms an adsorption film on the surface of the J shell and mold, contributing to the reduction of the coefficient of friction. In addition, when used in combination with graphite, 17
The decomposed inorganic boron compound envelops graphite 4 and works to prevent the graphite from flying and falling, and prevents the low temperature of Junyitake 7 (
-7. The required g amount of graphite can be significantly reduced, contributing to the improvement of the working environment.

The components of the present invention will be explained in detail below.

Repels with boric acid or boric anhydride; examples of the alkanolamines obtained include monoethanolamine,
Monoisoglobanolamine, N, N Dimethylethanolamine, N, N, di, L-Tanolamine, N, N Diisopropylethanolamine, N, N
cyphytylethanolaminenolamine, N-butylethanolamine, N-butylethanolamine, N-butylethanolamine, N-butylethanolamine. N-y methyl isobutyl
: 1 panolamine, N,N-dimethylbutanolamine/, neopentanolamine, butanolamine, dimethylneopentanolamine, N,N-dimethylhexanolamine, 2aminopropanol, 2aminobutanol-1 , jetanolamine, diisopropanolamine, methyldiethanolamine, butyljetanolamine, N,N di(2-human 1koxyedyl)aniline, phenyldiethanolamine, triethanolamine, triisopropanolamine, etc. Examples of the dihydric or higher polyhydric alcohols used in the present invention include ethylene glycol, propylene glycol, 1.3-butanediol, 1.4-butanediol, neopentyl glycol, trimethylolpropane, and pentaerythritol. , glycerin, sorbitol,
Examples include mannitol.

In the present invention, the reaction between boric acid or boric anhydride and an alkanolamine is usually carried out by a conventional method. That is, boric acid or boric anhydride and 1 to 6 equivalents of alkanolamine are placed in a reaction vessel equipped with a thermometer, a stirrer, and a countercurrent cooling tube, mixed, and heated to 100 to 180°C under normal pressure or reduced pressure.
A dehydration reaction is performed to obtain a boric acid ester.

The reaction with dihydric or higher alcohols is also usually carried out by the following method. That is, boric acid or boric anhydride and 1 to 3
An equivalent amount of dihydric or higher alcohol is placed in a reaction vessel equipped with a thermometer, a stirrer, and a backflow condenser, mixed, and dehydrated at 100 to 250°C under normal pressure or reduced pressure to obtain a boric acid ester.

The boric acid ester thus obtained is used by dispersing it in water, and in this case, the ester is dispersed in an amount of 5 to 70% by weight, preferably 10 to 50% by weight. This boric acid ester alone exhibits the above-mentioned excellent effect.

However, another excellent effect of this boric acid ester is that when used in combination with conventionally used lubricity imparting ingredients, the amount used can be reduced without reducing the lubricity. As the lubricity-imparting component used in this case, any conventionally used component can be used within a wide range, and the following components can be exemplified as representative examples.

<Graphite> As the graphite, any of earth graphite, phosphorous graphite, and artificial graphite can be used.

<Metal Soap> Examples include fatty acid metal soaps such as aluminum stearate, zinc stearate, and calcium stearate.

<Organic powder> Melamine resin, polyolefins such as polyethylene and polypropylene, fluororesins such as trifluoroethylene and tetrafluoroethylene, polycarbonate, polyacecool,
Examples include polyimide such as nylon 66.

<Inorganic powder> Boric acid, boric anhydride, meboric acid, sodium metaborate, sodium borate, sodium carbonate, calcium carbonate, monobasic sodium phosphate, dibasic potassium phosphate, sodium metaphosphate, potassium titanate, zinc pyrophosphate, Sodium silicate, calcium pyrophosphate, calcium fluoride,
Examples include molybdenum disulfide.

These powders are used when greater lubricity is required, but the amount used is usually 50% by weight or less, preferably 30% by weight or less, compared to 20 to 80% by weight.

When these donor components are used, a water-soluble polymer compound may be used as a dispersion aid in order to improve their dispersibility. Examples of the polymer compound at this time include block polymers of ethylene oxide and propylene oxide (molecular weight 3.000 to 100,000), carboxymethyl cellulose, hydroxymethyl cellulose,
An example is one in which propylene oxide or ethylene oxide is added as a block to propylene glycol.

If the boric acid ester which is the compound of the present invention is less than 5%, the effect is poor, and if it is more than 70%, it is economically disadvantageous. Further, in the present invention, it can be used in combination with other known additives, such as fatty acids, animal and vegetable oils, synthetic esters, extreme pressure additives, antioxidants, and celluloses.

〔Example〕

In order to make it easier to understand the present invention, reference examples as synthesis examples are shown below, and examples using the synthesized products are shown below, but the following reference examples and examples are not intended to limit the present invention in the same way.

Reference example 1 i'+'W hair 18-1, l, +1:1'fT 11k
, j)))nj! ! , i, l:i', l li
=-x 1. t ts: )-v response'g device c,
': ;l; gunoic acid (i I, 8 units (1,
0T a) Convert, Noi/Bjjl, Be, Norami/' 225fX(3,0:t,n,,
), 130' (: T”J 5 hours J\):
, IH'-, 9), the reaction water 4 of 5-core H (3,0:+L) comes out, t!゛(, 11th color transparent viscosity U, Rinahopa 7th alcohol], Sue) -λI f4%ノ,・.

Nooimatsu 12 Warm nail;) 1. Stirring ↑iP machine, reverse? 7th floor, W-eyebrow... :i
i) Boric acid (11,8IN (i
, (') 'l, le) and di, 1゛even, noramine 1
05, 2 (1,0 [ru) Mi J, N Mi 5.1 Del 81-ta 7 Nor 7゛ Min 1171'! (+, 0 dry) (,,,,
, 'i' was added, and the reaction was heated at 130-150° for 8 hours. +i9
+rv.

＠Oimatsu 3 Temperature tl'-, stirring plate, backflow Reitake (・) In a reaction vessel, add 61.8 g (1,0'E) of diboric acid and 1
Add 49 g (1,, o T-ru) of ethanol,
0-1 nyl) reaction water outflow 2\U'ζ, colorless and transparent.
A viscous phosphoric acid (I:, l')-luk was obtained.

4 Example 4 1KA degree d1, a stirrer and an oil cooling pipe attached to the counter L1. ．．
]'+', Container (, Nihog) acid G1. h(1,0:l-
104g (1
,0dril),":N,IN-f;;chill 1 "tsubu[lbe? 11. ．． ．． 1
The reaction was carried out at 30...150'C for 5 h (3
, Q chill), the water flow rate is 1J, and the water is 5. Obtained a yellow and viscous substance.

Actual h (11, Examples 1 to 14 and Comparative Example 1...4
Table C) The components shown in Table 1 are combined in a predetermined amount 1′1 self-combined j2°, ・
'Water-soluble hot lubricant, AI 1.7, various physical properties,
Measure ノζ. In the same table (, 11, the small amount % is reduced.

Thermal stability I/4: When the test hot lubricant is applied to a high xlA tool/mold, etc., most of the water and organic matter disappears due to transpiration, combustion, etc. In such a high temperature range, inorganic solid lubricants are often used for lubrication.
(In step 1, the evaporation loss curve of the hot lubricant was measured using a thermal balance, and the residual amount of the solid lubricant, which is essential for lubrication in high temperature ranges, was measured. Metal-to-metal contact resistance in moderately hot conditions, prevention of wear and tear on molds, etc.
7. It can be said that there are many silk products.

Measurement strip ('1 test) Rice: 10 - 15 mg Heating rate: 5°C/min Temperature range: RT (room temperature) -900°C 5900°C held for 6oN, gas N: 100 mN/min Measurement result 1st Table 2 shows the remaining state at 900°C (50 minutes hold).

- High temperature adhesion test steel plate test piece (SI'CC-5D) (100
x 100 x 10mm) to 100'c, 20
Heat to 0℃ and 300℃7, add 5% by weight of lubricant Hanashaku water? Dilute the liquid to 2 kg/
Apply by spraying with ct for 2 seconds and observe the adhesion condition. The results are shown in Tables 1 and 2. (-8L, 0 indicates that a continuous film is formed (7, × indicates J that there is a part that does not adhere).

Heating Test J1 (Ring) Using a hot ring compression tester, a 5% aqueous solution of lubricant was applied to a die heated to 200°C. Measure the coefficient of friction when compressed -L, and the results are shown in Table 12.
(Quality: S, 4.5C, 5tlS, -304 Ring shape = 20φXiO# X 7mm Ring heating temperature nail:
], 1100°CX 2 min cart: 1.
00 kg pressure 41? i rate = 40-50% (11fi L, commercial products in Tables 1 and 2 are as follows.

Commercially available product (Comparative Example 1) A water-soluble hot lubricant containing a total of 30% by market weight of a basic acid and a salt formed with it]' alkali metal hydroxide and an organic thickening agent.

Commercial product (Comparative Example 2) A water-soluble hot lubricant containing 30% by weight of a phosphate, a water-soluble polymer dispersant, and a water-soluble polymer dispersant.

Commercial product (Comparative Example 4) An alkali metal hydroxide containing 30% by weight of glasoite and forming a dibasic acid and a salt therewith, and an organic thickener;
A water-soluble hot lubricant containing a total of 8125% by weight of a disinfectant and a dispersant.

(J=, ) -YoJ-゛-Next city iF,? ＋ (Method) Heisei 1), July 2411 Patent Office 1i-Officer Satoshi Uematsu 1, Table of Case 1': Sei 241 Patent Side May 2, 2009 6372 Name of Invention Water-soluble hot lubrication side composition Item 3: Relationship with the supplementary IF case Patent applicant address
Osaka Shoshin, Ume HJ 1'Y L72-2 1400
Name and name Jindo Kagaku - Toso Co., Ltd. Representative Kuro J 4, Agent 1-1-2E, Minamimorimachi, Shoka-ku, Osaka, 530〒6,
Column 7 for the detailed description of the invention in the text description of the Japanese book. June 26, 2016) Contents of amendment 1, details, 4) Item 2 from right below inner box 1 i] [(Industrial use!llf:), r J:, as follows:
1 Correct.

[3. Detailed description of the invention [Industrial application field] 1 (below)

Claims (4)

[Claims] (1) Water-soluble, characterized in that it contains as an essential component a boric acid ester obtained by reacting boric acid or boric anhydride with at least one of an alkanolamine and a polyhydric alcohol of dihydric or higher valence. Hot lubricant composition. (2) The water-soluble hot lubricant composition according to claim (1), wherein the boric acid ester is contained in water in an amount of 5 to 70% by weight. (3) The water-soluble hot lubricant composition according to claim (1) or (2), further comprising a lubricity-imparting component dispersed therein. (4) Lubricity imparting component is graphite, metal soap,
Claim (1) wherein the powder is molybdenum disulfide or other lubricating powder.
), (2) or (3).