JP4627415B2 - Lubricant for metal processing, method for forming solid lubricant film for metal processing - Google Patents

Description

  The present invention relates to a lubricant for metal processing and a method for forming a solid lubricant film for metal processing. More specifically, the present invention is a novel type one-part treatment type metalworking lubricant having a simple composition that a base liquid (water) contains a polybasic acid of a dibasic acid or higher and a higher alcohol, The present invention relates to a method for forming a good solid lubricating film for metal working equivalent to the chemical conversion coating film by a simple process.

  Conventionally, in metal processing such as metal plastic processing, the surface of the workpiece is reduced in order to reduce the frictional resistance between the metal that is the workpiece and the mold for processing, or to prevent seizure between the two. A lubricating film is formed. Such lubricating films for metal working can be broadly classified into chemical conversion film types and oily types from the properties and formation processes.

  Generally speaking, the chemical conversion film type provides a solid solid film, so it is suitable for severe metal processing with strong impact and high pressure, such as cold forging and my press processing. On the other hand, there is a demerit that the film forming process is complicated, and the work efficiency in the metal working field is lowered or the work cost is raised. On the other hand, the mechanical strength of the lubricating film cannot be expected with the oil-based mold, but the work efficiency is good because it is only necessary to apply the oil-based base agent to the metal surface.

  These prior arts will be described in more detail below. The typical technology of the chemical conversion film type is as follows. That is, the workpiece is immersed in a primary zinc phosphate bath to allow the free phosphoric acid to react with the metal surface and to precipitate tertiary zinc phosphate on the surface. In this method, the metal soap film layer is formed by immersion in a reactive soap solution such as acid soda. By such treatment, it is possible to form a good solid film excellent in processing performance such as prevention of seizure between the processing mold and the workpiece.

  On the other hand, many types of oil-based lubricants have been used, and for example, one-component processing type metal processing lubricants as shown in Patent Document 1 and Patent Document 2 below have been proposed. It was.

In the invention of the acidic lubricant for cold working disclosed in Patent Document 1 above, phosphoric acid and a certain higher alcohol are heated and reacted in advance, and the reaction product obtained there In contrast, mineral oil (paraffinic or naphthenic crude products or derivatives thereof), saturated fatty acids having 12 to 22 carbon atoms, and one or more oily substances selected from paraffin, wax, resins, etc. The pH is adjusted with alkali.

In the invention of the lubricating oil composition for metalworking disclosed in JP-A-63-264698 and the method for producing the same, a mineral oil, a synthetic oil, or a mixed oil thereof, a phosphate ester and an orthophosphoric acid are disclosed. A lubricating oil composition for metalworking is disclosed that contains an aggregate of In addition, as a production method thereof, the above-mentioned mineral oil, synthetic oil or mixed oil thereof is mixed with a phosphate ester and regular phosphoric acid at a predetermined concentration, and heated to 80 ° C. or more to form the above-mentioned aggregate. Is described.

  However, the chemical conversion film treatment method described above includes a number of steps such as a step of immersing an iron material in a first zinc phosphate solution and fixing a third zinc phosphate, and a step of forming a metal soap film thereon. Therefore, the process is complicated, and there are various other problems in terms of management complexity and poor workability.

  On the other hand, the oil film forming technique is a one-liquid processing type, and only applies a lubricant to the metal surface, so that the process is remarkably simplified. However, as described above, the mechanical strength of the lubricating film cannot be expected so much, so it cannot withstand severe processing. There were also problems such as smoke from the base oil.

  Further, in the inventions disclosed in Patent Document 1 and Patent Document 2 described above, phosphoric acid and higher alcohol are heat-treated in advance, pH is adjusted with an alkali, or an association of phosphate ester and normal phosphoric acid is formed. It is said that the lubricating performance could be improved by the inclusion.

However, phosphoric acid and higher alcohols that have been heat-treated in advance and whose pH has been adjusted with alkali, and aggregates of phosphoric acid esters and normal phosphoric acid are dispersed and dissolved in the base mineral oil and synthetic oil. However, the effect of improving the lubrication performance is limited. And since it is the same as a conventional oil-type lubricant in that it is based on mineral oil, synthetic oil or the like, the formed lubricating film is basically an oil film. Accordingly, it is much inferior to the chemical conversion film in terms of mechanical strength as a lubricating film, heat resistance, metal adhesion, and the like, so that it is difficult to use for severe processing.

  In addition, an extra step called a heat treatment step is required for the production of phosphoric acid and a higher alcohol that have been heat-treated in advance and adjusting the pH with an alkali, and for the formation of an association between a phosphoric ester and normal phosphoric acid. It is added. There may be a problem of fuming such as mineral oil or synthetic oil as a base oil.

  Therefore, the present invention is a water-based one-component treatment type lubricant that has a simple film formation process, and is not an oil film but a solid film excellent in metal adhesion and not inferior to the above-mentioned chemical conversion treatment film. It is an object to be solved to provide a metal working lubricant capable of forming a metal working material and a method for easily forming a solid lubricating film for metal working using the metal working lubricant.

(Configuration of the first invention)
The structure of the first invention of the present application for solving the above-described problem is that a dibasic acid or higher polybasic acid and an alcohol having a carbon chain of 10 or more carbon atoms are contained in water as an evaporable base liquid. It is a lubricant for metal processing.

(Configuration of the second invention)
The configuration of the second invention of the present application for solving the above problem is a metalworking lubricant obtained by further adding a fatty acid amide to the base liquid according to the first invention.

(Configuration of the third invention)
The structure of the third invention of the present application for solving the above-mentioned problem is that the polybasic acid and alcohol according to the first invention or the second invention, or further the fatty acid amide is dispersed in the base solution using a surfactant or A metalworking lubricant that has been dissolved.

(Configuration of the fourth invention)
The constitution of the fourth invention of the present application for solving the above problems is that the concentration of polybasic acid of dibasic acid or higher in the metal processing lubricant according to any of the first to third inventions is 0.5 to The lubricant for metalworking is in the range of 30% by weight and the alcohol concentration is in the range of 1 to 20% by weight.

(Structure of the fifth invention)
The configuration of the fifth invention of the present application for solving the above problem is that the polybasic acid of the dibasic acid or more according to any one of the first to fourth inventions is any one or more of phosphoric acid or dicarboxylic acid. A lubricant for metal processing (Structure of the sixth invention)
The structure of the sixth invention of the present application for solving the above-described problem is that the alcohol according to any one of the first to fifth inventions has a saturated carbon chain, or a carbon chain containing 2 or less unsaturated bonds. It has a metal processing lubricant.

(Structure of the seventh invention)
In order to solve the above-mentioned problem, the seventh aspect of the present invention is configured such that the metal processing lubricant according to any one of the first to sixth aspects of the invention is applied to the surface of a metal as a workpiece, and the base liquid is evaporated. This is a method for forming a solid lubricating film for metal working that allows the following effects (1) to (3) to be exhibited.
(1) A salt formation reaction between a polybasic acid of dibasic acid or more and a metal is caused on the metal surface, and micro unevenness is formed on the metal surface.
(2) Based on an increase in the concentration of polybasic acid of dibasic acid or higher and alcohol, an aggregate that does not reach an ester bond is formed between them.
(3) A highly adhesive solid lubricating film containing the aggregate is completed by sufficient evaporation of the base liquid.

(Configuration of the eighth invention)
The structure of the eighth invention of the present application for solving the above-mentioned problems is that the base liquid of the metal processing lubricant according to the seventh invention is applied to the surface of the metal, and then within the range of 40 ° C to 150 ° C. This is a method for forming a solid lubricating film for metal working that promotes the evaporation of the base liquid by heating at the above.

(Effect of the first invention)
The lubricant for metal processing of the first invention is a one-component processing type lubricant comprising water as an evaporable base liquid, a polybasic acid of dibasic acid or more, and an alcohol having a carbon chain of 10 or more carbon atoms. The film forming process is simple because it is only necessary to evaporate the base liquid by applying to the metal surface.

  Moreover, the metalworking lubricant of the first invention has the following actions and effects described with reference to FIG. That is, as shown in FIG. 1 (a), the metalworking lubricant 1 in a state before use is a dibasic acid or higher polybasic acid 3 at a concentration not so high in the evaporable base liquid 2. It contains alcohol 4 having a carbon chain with 10 or more carbon atoms.

  When the metal processing lubricant 1 is applied to the surface of the metal 5 as the workpiece as shown in FIG. 1B and the base liquid 2 is evaporated, in the process, the polybasic acid 3 and the alcohol 4 Was found to be significantly enriched to form certain aggregates (or something similar to aggregates).

  In metal processing lubricants containing water as a base solution, it is considered that phosphoric acid is trapped in water, so that no association with alcohol is formed. However, it is considered that in the process of applying a metal processing lubricant to the surface of the metal and evaporating the water as the base liquid, the contact with the alcohol is gradually facilitated and the above-mentioned aggregate is formed.

  Although detailed data presentation is refrained, in the process of studying the mechanism of action of phosphoric acid (polybasic acid) and alcohol by the inventor of the present application, while the infrared absorption analysis shows a peak similar to that of phosphate ester, In H-NMR, it was found that protons attributed to the —OH group of phosphoric acid shifted to the low magnetic field side, and protons attributed to the alcohol —OH group shifted to the high magnetic field side. Furthermore, although it was presumed to be this aggregate, it showed the same acid value as phosphoric acid in the strong acid value measurement.

  From the above points, it is suggested that phosphoric acid and alcohol do not reach ester formation, but have an affinity binding state, that is, an aggregate state presumed as “Chemical Formula 1” below. Is done. This aggregate is different from the aggregate of phosphate ester and orthophosphoric acid disclosed in Patent Document 2 described above.

そして図１（ｃ）に示すように、ベース液２は最終的に全て蒸発し、固形皮膜６が形成される。この固形皮膜６は、上記の会合体を形成している多塩基酸３とアルコール４からなり、過酷な金属加工に耐える強固な固形皮膜であって、油膜ではない。従って当然ながら、ベース油の発煙等の問題も起こらないし、いわゆる油膜ハジキの問題も起こらない。

And as shown in FIG.1 (c), all the base liquid 2 finally evaporates and the solid membrane | film | coat 6 is formed. The solid film 6 is composed of the polybasic acid 3 and the alcohol 4 forming the above-mentioned aggregate, and is a solid solid film that can withstand severe metal processing, and is not an oil film. Therefore, as a matter of course, problems such as smoke generation of the base oil do not occur, and so-called oil film repellency does not occur.

  Furthermore, the metalworking lubricant of the first invention uses a polybasic acid of dibasic acid or higher as the acid. For this reason, while the polybasic acid is involved in the formation of the above-mentioned aggregate, it reacts with the surface of the metal as the workpiece, and as shown in FIG. 7, 7, ... are formed (micropool action). As a result, since the solid film 6 is formed in a state of being bitten by the micro irregularities 7, 7,..., The adhesion of the solid film 6 to the metal surface is excellent.

  When an alcohol having a carbon chain with less than 10 carbon atoms is used as the alcohol, the solid film becomes somewhat soft and its strength may be insufficient.

  Since the water that is the base liquid of the metal processing lubricant is not flammable, the metal processing lubricant is applied to the surface of the metal that is the workpiece, and then heated to promote the evaporation of the water. Can be made more efficient.

(Effect of the second invention)
By adding a fatty acid amide to the base solution of the metal processing lubricant, the liquid dispersibility of the higher alcohol by the surfactant is improved, and the metal and the polybasic acid react to form a salt of the polybasic acid. Prevent free fall off. In addition, it is possible to obtain an effect of suppressing reaction unevenness on the metal surface and improving the finished skin after processing.

(Effect of the third invention)
Polybasic acids, alcohols, or even fatty acid amides contained in the base liquid of metal processing lubricants can be dispersed or dissolved in the base liquid using a surfactant to stabilize their content and to process metals. It is more preferable in stabilizing the properties of the lubricant for use.

(Effect of the fourth invention)
Since the polybasic acid and alcohol contained in the metal processing lubricant are sufficiently concentrated before film formation as described above, the concentration may be low in the base solution. The content concentration of these components in the lubricant for metal working can be in the range as defined in the fifth invention. Within such a range, the fluidity of the metalworking lubricant is maintained at a level suitable for application, and the problem of excessive time required for evaporation of the base liquid can be avoided.

(Effect of the fifth invention)
The type of polybasic acid of dibasic acid or higher contained in the base solution is not particularly limited, but for reasons of corrosion resistance, metal surface fixability, affinity with higher alcohols, etc., for example, either phosphoric acid or dicarboxylic acid One or more types are particularly desirable. As particularly preferred dicarboxylic acid, oxalic acid can be exemplified.

(Effect of the sixth invention)
Among alcohols having a carbon chain having 10 or more carbon atoms, alcohols having a carbon chain containing 2 or less unsaturated bonds are preferable, and alcohols having a saturated carbon chain are particularly preferable. If an alcohol that does not meet such conditions is used, it is difficult to solidify at room temperature, and a good film may not be formed.

(Effect of the seventh invention)
According to the method for forming a solid lubricating film for metal working of the fifth invention, since any one of the metal working lubricants is applied to the metal surface and the base liquid is evaporated, (1) polybasic acid on the metal surface and Micro unevenness can be formed by reaction with metal, and then (2) based on the increase in concentration of polybasic acid and alcohol, an aggregate that does not reach an ester bond between them is formed. And (3) by sufficiently evaporating the base liquid, a highly adhesive solid lubricating film containing the aggregate can be completed.

  As a result, the film formation process becomes simple, the base liquid evaporates and the formation of aggregates forms a solid solid film instead of an oil film, avoids problems such as fuming of the base oil, and forms micro unevenness on the metal surface. Thus, sufficient adhesion of the solid film to the metal surface can be secured.

In addition,
(Effect of the eighth invention)
Water, which is the base liquid for metalworking lubricants, can be accelerated by heating, but the temperature range of this heating prevents the problem of the evaporation rate of water and the increase in coating amount due to the increase in liquid viscosity. For the purpose, it is preferably 50 ° C. or higher, and from the viewpoint of maintaining the dispersion stability of the components and maintaining stable liquid properties, it is preferably 150 ° C. or lower.

  Next, modes for carrying out the first to eighth inventions of the present application will be described including the best mode. In the following, the term “present invention” refers to each invention of the present application collectively.

[Metal processing lubricant]
The metal processing lubricant according to the present invention contains water as an evaporable base liquid containing at least a polybasic acid having a dibasic acid or more and an alcohol having 10 or more carbon atoms. Preferably, it further contains a fatty acid amide. These can be stably dissolved or dispersed using a surfactant.

  Note that the total content of the polybasic acid, alcohol and fatty acid amide in the lubricant for metal processing is 50% by weight or less from the viewpoint that it is desired to be a fluid at room temperature from the viewpoint of applicability. preferable.

  In addition to the above components, the metal working lubricant can contain various known corrosion inhibitors and antioxidants for the purpose of suppressing excessive corrosion and deterioration of the metal. In addition, various components that may be contained in this type of lubricant, for example, pour point depressants for the purpose of stabilizing liquid properties, detergent dispersants, etc., as long as the effects of the present invention are not impaired. Can be made. In addition, waxes (paraffin wax, oxidized paraffin wax, beeswax, paraffin wax, wood wax, carnauba wax, etc.), animal and vegetable oils or derivatives thereof, and various rust preventive additives for improving rust prevention and film properties. Etc. can be contained.

[Polybasic acid]
The polybasic acid used in the present invention is not particularly limited as long as it is a dibasic acid or higher. Examples of particularly preferred polybasic acids include phosphoric acid, dicarboxylic acid and tricarboxylic acid, and among these, phosphoric acid and succinic acid are particularly preferred. Examples of phosphoric acid include diphosphorus pentoxide, orthophosphoric acid, polyphosphoric acid, and metaphosphoric acid.

  The concentration of the polybasic acid contained in the metal processing lubricant is not limited, but generally it is preferably in the range of 0.5 to 30% by weight, particularly preferably in the range of 1 to 20% by weight. When the polybasic acid is phosphoric acid, its concentration in the metal working lubricant is preferably in the range of 0.5 to 15% by weight, particularly preferably in the range of 1 to 10% by weight.

If the concentration of polybasic acid (or phosphoric acid) deviates from the lower limit of the above numerical range, the reactivity will decrease due to the lack of absolute amount, the compatibility of polybasic acid and higher alcohol will decrease, There is concern about a decrease in adsorptivity. When the concentration of polybasic acid (or phosphoric acid) deviates from the upper limit of the above numerical range, the effect is saturated, and at the same time, the solubility and the liquid property of the lubricant are not necessarily good. There is also concern about the deterioration of the metal surface skin based on the concentration variation.

  In addition, when using phosphoric acid, combined use with another polybasic acid, especially oxalic acid contributes to the improvement of rust prevention. The reason is considered to be due to the difference in water affinity of the metal salt produced and the adsorptive action of the carboxyl group.

〔alcohol〕
The alcohol used in the present invention is not particularly limited as long as it is an alcohol having 10 or more carbon atoms. Alcohols having less than 10 carbon atoms are insufficient in terms of carryability into the plastic working mold and lubrication performance. From this aspect, alcohol having 12 or more carbon atoms is particularly preferable.

  In addition, alcohols having a high degree of saturation, that is, those having a saturated carbon skeleton are particularly preferred, but those having a carbon skeleton containing two or less unsaturated bonds are also preferred. Such a carbon skeleton is not necessarily linear, and may be branched. Those having an alicyclic or aromatic cyclic carbon skeleton have a low melting point for those having a small number of carbon atoms, and are unsatisfactory in terms of solubility and film formability for those having a large number of carbon atoms.

  Specific examples of preferred alcohols include lauryl alcohol, cetyl alcohol, stearyl alcohol, oleyl alcohol, behenyl alcohol, ceryl alcohol, myricyl alcohol, lanolin alcohol and the like from the viewpoint of lubricity.

  The concentration of the alcohol contained in the lubricant for metal working is not limited, but generally it is preferably in the range of 1 to 20% by weight, particularly preferably in the range of 5 to 10% by weight. If the alcohol concentration deviates from the lower limit of the above numerical range, there is a possibility that a satisfactory solid film cannot be formed due to an insufficient absolute amount. Even if the alcohol concentration deviates from the upper limit of the above numerical range, the effect may be saturated and useless, and at the same time, the viscosity and melting point of the metal working lubricant may not be optimal.

[Fatty acid amide]
The type of fatty acid amide to be contained in the lubricant for metal processing is not limited, but examples include oleic acid amide, stearic acid amide, stearic acid bisamide, and preferably one or more of these are preferably used. Can do.

  The content concentration of the fatty acid amide in the lubricant for metal processing is not limited, but generally it is preferably in the range of 0.1 to 5% by weight, particularly preferably in the range of 0.5 to 2% by weight. When the fatty acid amide content concentration deviates from the lower limit of the above numerical range, there are concerns about several dissatisfaction points, such as unevenness in film formation due to insufficient absolute amount. Concentration of fatty acid amide Even if the concentration deviates from the upper limit of the above numerical range, there is a concern that the effect may be saturated and useless, and there is a concern that higher alcohol may float and separate as an oil component.

[Method of forming solid lubricating film for metal processing]
A method for forming a solid lubricating film for metal processing according to the present invention comprises applying one of the above-mentioned lubricants for metal processing to the surface of a metal that is a workpiece, evaporating the base liquid, and (1) micro-processing on the metal surface. Each of the following functions is formed: (2) formation of an association between a polybasic acid and an alcohol, and (3) formation of a highly adhesive solid lubricating film containing the association. When the base liquid is evaporated by applying a metal processing lubricant to the surface of the metal, it is preferable to promote evaporation of the water as the base liquid by heating within a range of 40 ° C to 150 ° C.

  The method of applying the metal processing lubricant to the surface of the metal is not limited. For example, a method of immersing the metal (work material) in the metal processing lubricant, spraying the metal processing lubricant on the metal, brushing, etc. Can be arbitrarily adopted. As a method of heating to evaporate the base liquid, any heating method such as a method of heating a metal as a workpiece, a method of pickling as a pretreatment or washing with hot water in a degreasing process is adopted. can do.

  The target metal and the type of metal processing are not particularly limited, but examples of the metal include carbon steel, iron-based alloy steel, and stainless steel. As the type of metal processing, plastic processing such as press processing and cold forging processing is typical, but other examples include drawing processing, sizing processing, swaging processing, butted processing, and the like.

(Example A)
In the column of “Table 1” in the following “Table 1”, metal working lubricants having the compositions shown in the sections of “Sample A” and “Sample B” were prepared. Sample A is an example of the present invention, and sample B is a comparative example. In the column of “Table-1”, “stearyl” means stearyl alcohol, and “cetyl” means cetyl alcohol. Moreover, the numerical value which shows the composition ratio of each composition is a weight% unit.

次に、被加工材であるＳ−２５Ｃの鉄材（直径１８．７ｍｍ、長さ４２０ｍｍ、引抜加工材）をアルカリ脱脂液にて脱脂し、次いで水洗、湯洗した。そして、上記のサンプルＡに１分間浸漬した後、８０°Ｃの加熱条件下で水を蒸発させることにより、乾燥させた。

Next, S-25C iron material (diameter: 18.7 mm, length: 420 mm, drawn material) as a workpiece was degreased with an alkaline degreasing solution, and then washed with water and hot water. And after immersing in said sample A for 1 minute, it was made to dry by evaporating water on 80 degreeC heating conditions.

Meanwhile, degreasing another S-25C of iron two like the each of the above, washed with water, washed with hot water, 30% orthophosphoric acid aqueous solution of 60 ° C, one is 1 minute, the other one is 5 Each was immersed for a minute. Subsequently, after drying these, the sample B was apply | coated to the said two S-25C iron materials, and it was dried again.

  Using the above S-25C iron material as a test piece, each was pressed with a hydraulic press, and the following evaluation was performed. The evaluation method is that the test piece is processed at a processing speed of 141.2 cm / min. In this process, the length is reduced to 195 mm to an oval shape (reduction area: 12.6%). The evaluation items are visual observation of the applied load (ton unit) and the surface state of the processed part.

  The evaluation results are shown in the column of “Table-2” in Table 1. In the S-25C iron material according to the comparative example, the surface of the iron material is iron phosphated in advance, and the higher alcohol is coated thereon. With the S-25C iron material according to the example, the film is formed by the method of the present invention. A film is formed. From the results shown in the column of “Table-2”, it can be seen that the film of the example shows higher lubricating performance than the film of the comparative example.

(Example B)
Next, regarding the S-25C iron material dipped in sample A and dried as described above, (a) the film-formed surface before the above-described open drawing process, and (b) after the open-drawing process of the film-formed surface And (c) X-ray fluorescence analysis was performed on the surface after further washing with normal hexane to completely remove the solid film. X-ray fluorescence analysis is a measurement method that converts the intensity of a fluorescent X-ray spectrum generated by X-ray irradiation into a concentration. Therefore, it can be said that the phosphorus content is a value indicating the intensity of the fluorescent X-ray spectrum.

The measurement results were as follows: (A) processed part area = 100.073 cm ² , processed part coating amount = 0.100 g, phosphorus content = 7.66 wt%, (B) phosphorus content = 6.69 wt%. It was. Further, the phosphorus content in (c) was 4.66 wt%. Considering that the amount of coating after processing = the amount of cleaning membrane, the average value of 10 test samples was 0.012 g. From these values, the amount of the detached film at the time of processing is 0.088 g from “the amount of film before processing−the amount of film after processing”. On the other hand, the phosphorus content is 0.97 wt% in the release film from “Phosphorus before processing−Phosphorus after processing”, and 2% in the film after processing from “Phosphorus after processing−Phosphorus after washing”. 0.03 wt%, and the iron surface after cleaning is calculated to have a phosphorus content of 4.66 wt%.

Considering these values from the viewpoint of the coating amount and the phosphorus content, the ratio of the phosphorus content to the amount of the detached film during processing is 0.97 ÷ 0.088 = 1.02 wt% / g, based on the coating amount dissolved by cleaning. The ratio of phosphorus content is 2.03 ÷ 0.012 = 169.17 wt% / g. This indicates that the phosphorus concentration in the film after processing is extremely high, and it is considered that the affinity between the higher alcohol and phosphoric acid shown by 1 H- NMR contributes to the lubricity of processing. .

(Example C)
In the following “Table 2”, “Example 1” to “Example 5” are prepared, and metal working lubricants having the compositions shown in the respective columns are prepared, respectively, in the same manner as in Example A above, 50 × 300 × t 0.8 mm SPCD (JIS G 3141 cold-rolled steel plate and steel strip for drawing) was applied to a test piece, and water was evaporated to form a solid film on the surface of the test piece.

一方、比較例１〜比較例４をそれぞれ次のように行って、同上の試験片の表面に潤滑膜を形成させた。

On the other hand, Comparative Example 1 to Comparative Example 4 were performed as follows, and a lubricating film was formed on the surface of the test piece.

  Comparative Example 1: A general-purpose lubricant conversion coating treatment comprising a zinc phosphate conversion coating treatment and a sodium stearate salt coating was used. After immersing the test piece in the first zinc phosphate solution and creating a zinc phosphate conversion coating on the surface, the sample is immersed in a metal stearate soap solution to form a zinc phosphate conversion coating and a sodium stearate coating. Formed.

  Comparative Example 2: A water-based film-type lubricant having a surfactant dispersion of calcium stearate as a lubricating component and a water-based acrylic resin and polyvinyl alcohol as a binder was used.

  Comparative Example 3: A reactive lubricating oil in which an acidic phosphoric acid ester composed of monooleate phosphate and dioleate phosphate is used as a lubricating component and dissolved in mineral oil is used. By applying to a test piece, a lubricating oil film was formed on the surface together with a reaction film made of an acidic phosphate ester.

  Comparative Example 4: A lubricating oil comprising a sulfur compound, zinc dialkyldithiophosphate, calcium sulfonate, and a fat wear reducing agent is used. A lubricating oil film was formed on the test piece.

(Example D)
In order to evaluate the adhesion of the lubricating films formed on the surfaces of the test pieces according to Examples 1 to 5 and Comparative Examples 1 to 4, the test was repeated 10 times using a sliding tester. The sliding test was conducted, and the friction coefficient was measured.

  2, the test piece 8 is sandwiched between a pair of molds 9 in the vertical direction, and a predetermined portion of the test piece 8 is placed in the same direction (left side in FIG. 2), speed, It was based on a method of repeatedly sliding 10 times with surface pressure. Then, the sliding resistance was calculated as a friction coefficient. The implementation conditions of the sliding test are shown in “Table 3” below.

（実施例Ｅ）
前記の「表２」における「実施例１」〜「実施例５」の欄にそれぞれ示す組成の金属加工用潤滑剤を調製し、これらをそれぞれ、前記の実施例Ａの場合と同じ方法で、前記Ｓ−２５Ｃの鉄材に塗布し、水を蒸発させて試験片の表面に固形皮膜を形成させた。一方、前記比較例１〜比較例４をそれぞれ同上のＳ−２５Ｃの鉄材に対して実施し、その表面に潤滑膜を形成させた。

(Example E)
The metal working lubricants having the compositions shown in the columns of “Example 1” to “Example 5” in the above “Table 2” were prepared, respectively, in the same manner as in Example A above, It apply | coated to the said S-25C iron material, water was evaporated, and the solid film was formed on the surface of the test piece. On the other hand, each of Comparative Examples 1 to 4 was carried out on the same S-25C iron material, and a lubricating film was formed on the surface thereof.

  In order to evaluate the press performance of the lubricating films formed on the surface of the S-25C iron material according to Examples 1 to 5 and Comparative Examples 1 to 4, a molding test was performed using a press machine. The molding load was measured and the state of the processed surface was observed.

  In this test method, as shown in FIG. 3, an S-25C iron material 10 is pushed into a mold under the predetermined conditions shown in the following “Table 4”, and the iron material 10 is changed into the shape of the iron material 11 shown in FIG. Then, the measurement of the molding load at that time and the observation of the state of the processed surface 12 were performed.

（実施例Ｆ）
上記の実施例Ｃにおける実施例１〜実施例５、及び比較例１〜比較例４に係る摩擦係数の測定結果を下記の「表５」に示す。比較例４については、第２回目の摺動試験の際に試験片が破断し、それ以後の摺動試験を実施できなかった。

(Example F)
The measurement results of the friction coefficients according to Examples 1 to 5 and Comparative Examples 1 to 4 in Example C are shown in “Table 5” below. For Comparative Example 4, the test piece broke during the second sliding test, and the subsequent sliding test could not be performed.

表５の結果から、次のことが言える。即ち、多段加工において、油性型潤滑剤の使用では加工の都度に潤滑剤の供給を必要とする。このことは、摺動試験結果の比較例４が１回の摺動にて潤滑膜が大きく欠損した事実と一致する。一方、従来の化成皮膜では、一度の処理にて多段加工を完了させることができる。これは比較例１の繰り返しの摺動試験にも皮膜破損が少なく、常に安定した低摩擦係数を維持していることでも理解される。比較例２〜３では比較例４よりも繰り返し性が高いが、いずれも３回〜４回程度の摺動にて潤滑膜が大きく欠落し、初期の摩擦係数は維持できなかった。

From the results in Table 5, the following can be said. That is, in multistage processing, the use of an oil-based lubricant requires the supply of a lubricant every time processing is performed. This is in agreement with the fact that the lubricating film was largely lost in Comparative Example 4 of the sliding test result by one sliding. On the other hand, in the conventional chemical conversion film, multi-stage processing can be completed by a single treatment. This can also be understood from the fact that the repeated sliding test of Comparative Example 1 has little film damage and always maintains a stable low coefficient of friction. Although high repeatability than Comparative Examples 2-3 In Comparative Example 4, both the lubricating film is missing greatly Te to about 3 times to 4 times the sliding, the initial coefficient of friction could not be maintained.

  In contrast, the metalworking lubricant according to the example (metalworking lubricant according to the present invention) exhibits an initial coefficient of friction that is greater than that of each comparative example and follows a repeated sliding to a normal chemical film. The value is comparable.

(Example G)
The measurement of the molding load according to Examples 1 to 5 and Comparative Examples 1 to 4 in Example D and the observation results of the state of the processed surface 12 are shown in “Table 6” below.

表６の結果から、次のことが言える。即ち、実施例Ａと同様に比較例１の通常の化成皮膜処理は低成形荷重であり、良好な加工面となったが、比較例２〜４ではいずれも成形荷重は高く、しかも、加工面には潤滑膜の破断によるかじりが発生した。

From the results in Table 6, the following can be said. That is, examples usual chemical conversion coating process A as well as Comparative Example 1 is a low molding load heavy, but a good machined surface, both Comparative Examples 2 to 4 shaped load weight is high, moreover, On the processed surface, galling due to breakage of the lubricating film occurred.

In contrast, in the metal working lubricants according to the example (metalworking lubricant according to the present invention), good at comparable Comparative Example 1 is a conventional conversion coating process or less of the molding load heavy machining It is possible to conclude that the film has a surface and is a coating agent that can follow severe processing.

  According to the present invention, a water-based one-component processing type metal processing lubricant capable of forming a solid lubricating film that is easy to process and has good lubrication performance in the field of metal processing, particularly metal composition processing, and the use of this lubricant. A method for easily forming a good solid lubricating film for metal working equivalent to a chemical conversion coating is provided.

It is a figure which visualizes and demonstrates the operation of the present invention.

Is a diagram briefly illustrating the sliding Do試 test in Examples.

It is a figure which illustrates the press work test in an Example simply.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Lubricant for metal processing 2 Base liquid 3 Polybasic acid 4 Alcohol 5 Metal 6 Solid film 7 Concavity and convexity 8 Test piece 9 Mold 10 Iron material 11 Iron material 12 Work surface

Claims (7)

A metal processing lubricant characterized by being a one-component processing type lubricant comprising water as an evaporable base solution, a polybasic acid of dibasic acid or more contained in the water, and an alcohol (A) below. .
(A) An alcohol selected from lauryl alcohol, cetyl alcohol, stearyl alcohol, oleyl alcohol, behenyl alcohol, ceryl alcohol, myristyl alcohol, and lanolin alcohol. It is a one-component treatment type lubricant composed of water as an evaporable base solution, a polybasic acid of dibasic acid or more contained in the water, an alcohol of the following (A), and a fatty acid amide. Lubricant for metal processing.
(A) An alcohol selected from lauryl alcohol, cetyl alcohol, stearyl alcohol, oleyl alcohol, behenyl alcohol, ceryl alcohol, myristyl alcohol, and lanolin alcohol. Water which is an evaporable base solution, a polybasic acid of dibasic acid or more contained in the water, an alcohol (A) below, a fatty acid amide, and these polybasic acid, alcohol and fatty acid amide A metal processing lubricant characterized by being a one-component processing type lubricant comprising a surfactant dispersed or dissolved in a liquid.
(A) An alcohol selected from lauryl alcohol, cetyl alcohol, stearyl alcohol, oleyl alcohol, behenyl alcohol, ceryl alcohol, myristyl alcohol, and lanolin alcohol. The content concentration of polybasic acid of dibasic acid or higher in the metal processing lubricant is in the range of 0.5 to 30% by weight, and the content concentration of alcohol is in the range of 1 to 20% by weight. The metal working lubricant according to any one of claims 1 to 3. The metalworking lubricant according to any one of claims 1 to 4, wherein the dibasic acid or higher polybasic acid is at least one of phosphoric acid and dicarboxylic acid. The following effects (1) to (3) are obtained by applying the metal processing lubricant according to any one of claims 1 to 5 to a surface of a metal as a workpiece and evaporating the base liquid. A method for forming a solid lubricating film for metalworking, characterized in that
(1) A salt formation reaction between a polybasic acid of dibasic acid or more and a metal is caused on the metal surface, and micro unevenness is formed on the metal surface.
(2) Based on an increase in the concentration of polybasic acid of dibasic acid or higher and alcohol, an aggregate that does not reach an ester bond is formed between them.
(3) A highly adhesive solid lubricating film containing the aggregate is completed by sufficient evaporation of the base liquid. The metal processing according to claim 6, wherein after the metal processing lubricant is applied to the surface of the metal, heating is performed within a range of 40 ° C. to 150 ° C. to promote evaporation of the base liquid. Of forming a solid lubricating film for use.

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