KR101305080B1 - Manufacture method of complex aluminum grease for highest pressure and wear resistant - Google Patents

Abstract

The present invention relates to a method for producing a high extreme pressure wear resistant composite aluminum grease in which various fatty acids including benzoic acid, stearic acid and oleic acid and aluminum isopropoxide are reacted to improve various performances including extreme pressure resistance.
According to the present invention, stearic acid (Stearic acid) and oleic acid (Oleic acid) is added to the lubricating base oil by stirring at a predetermined temperature to dissolve; A second step of dissolving and stirring benzoic acid in alcohol, and adding aluminum isopropoxide to the mixture of the stirred alcohol and benzoic acid and heating it; A third step of mixing and heating the mixture dissolved in the first step with the mixture produced in the second step; A fourth step of cooling by adding water to the mixture produced in the third step; And a fifth step of adding a lubricating base oil to the mixture produced by cooling in the fourth step and heating the mixture to a predetermined temperature.

Description

MANUFACTURE METHOD OF COMPLEX ALUMINUM GREASE FOR HIGHEST PRESSURE AND WEAR RESISTANT

The present invention relates to a process for producing high extreme pressure wear resistant composite aluminum grease. More specifically, the present invention relates to a method for producing a high-polarization wear-resistant composite aluminum grease in which fatty acids benzoic acid, stearic acid and oleic acid are reacted with aluminum isopropoxide to improve various performances including extreme pressure resistance.

Generally, grease constituents are divided into three types: base oils, thickeners and additives. In the above, the base oil is roughly divided into general mineral oil, synthetic oil such as silicone oil, and ester oil, and the thickener is divided into soap-based such as barium, lithium, calcium, sodium, aluminum, and soap-based such as silica gel, benton, urea, and the like. In addition, various additives, such as antioxidants and extreme pressure agents, are added for various purposes according to their properties.

In the conventional grease production, grease is manufactured by using the thickener raw materials and additives as described above, and independently inputting them to a production line at a unique addition ratio of each company.

However, Korea's technological level in Greece is still in its infancy compared to developed countries such as the US and Japan. In addition, various types of greases have been researched and made according to the increasingly demanding performance according to the characteristics of various facilities.

In particular, the grease made of aluminum as a thickener is excellent in adhesion to metal surfaces and excellent in rust resistance compared to lithium grease or calcium grease, which is mainly manufactured. Since the stability is relatively poor, it is urgent to solve this problem.

In addition, as described above, lithium grease and calcium grease are mainly manufactured as lithium grease or calcium grease, and the thickener is made of lithium soap or calcium soap, which is very toxic and is actually harmful to the human body. However, the grease made of aluminum as a thickener has no toxicity at all, and is mainly used as a lubricant in the lubricating part of a machine or a food-only machine in a food manufacturing or processing plant.

Therefore, it is urgent to develop grease that can improve the performance such as extreme pressure resistance and heat resistance while maintaining the environmentally friendly characteristics of aluminum grease.

KR 10-2009-0025642 KR 10-2001-0029060

The present invention has been made to solve the above problems, by reacting the fatty acid benzoic acid, stearic acid and oleic acid with aluminum isopropoxide (Aluminum Isopropoxide) is more environmentally friendly than conventional grease, such as polar pressure resistance and heat resistance performance It is an object of the present invention to provide a method for producing high extreme pressure wear resistant composite aluminum grease that can be improved.

According to the present invention, stearic acid (Stearic acid) and oleic acid (Oleic acid) is added to the lubricating base oil by stirring at a predetermined temperature to dissolve; A second step of dissolving and stirring benzoic acid in alcohol, and adding aluminum isopropoxide to the mixture of the stirred alcohol and benzoic acid and heating it; A third step of mixing and heating the mixture dissolved in the first step with the mixture produced in the second step; A fourth step of cooling by adding water to the mixture produced in the third step; And a fifth step of adding a lubricating base oil to the mixture produced by cooling in the fourth step and heating the mixture to a predetermined temperature.

On the other hand, after the fifth step by adding and stirring the additive containing the extreme pressure additive, a sixth step of manufacturing a composite aluminum grease through milling; characterized in that it further comprises.

On the other hand, the lubricating base oil of the first step is characterized in that the base oil is a mixture of ester base oils having different kinematic viscosity.

On the other hand, the benzoic acid is 1 to 3% by weight of the total amount of grease, the stearic acid is 3 to 5% by weight of the total amount of grease, the oleic acid is 0.1 to 0.3% by weight of the total amount of grease, the aluminum isopropoxide (Aluminum Isopropoxide ) Is characterized in that it contains 2 to 4% by weight of the total amount of grease.

On the other hand, the extreme pressure additive is characterized in that the sulfur and antimony-based (antimony dialkyl dithiocarmate) extreme pressure additive or fluorine-based (PTFE: Poly tetrafluoroethylene) extreme pressure additive.

The high-polarization wear-resistant composite aluminum grease according to the present invention has an effect of improving various performances including polar pressure resistance by reacting fatty acid benzoic acid, stearic acid and oleic acid with aluminum isopropoxide.

In addition, the present invention was able to produce a composite aluminum grease having excellent polar pressure resistance and the like by adding an extreme pressure additive.

In addition, the present invention is the mechanical shear stability, heat resistance, oxidative stability, rust resistance, evaporation result of the evaluation of the physical properties through the compounding experiment using a synthetic base oil of excellent synthetic oil to compensate for the various disadvantages of general mineral oil system It showed excellent effects in all performances including water resistance, oil resistance and so on.

1 is a graph showing the biodegradability of the lubricant base oil (synthetic oil ester) and mineral oil used in the method for producing a high-polarization wear-resistant composite aluminum grease according to an embodiment of the present invention.

Hereinafter, preferred embodiments of the present invention will be described in detail. In the following description of the present invention, a detailed description of known functions and configurations incorporated herein will be omitted when it may make the subject matter of the present invention rather unclear.

Method for producing a high-polarization wear-resistant composite aluminum grease according to an embodiment of the present invention is as follows.

In the first step, stearic acid and oleic acid are added to the lubricating base oil to dissolve by stirring at a predetermined temperature. The lubricating base oil of the first step is a synthetic oil, and is preferably a base oil obtained by mixing ester base oils having different kinematic viscosities. Referring to FIG. 1, the biodegradability of mineral oil (right) and synthetic oil (left) is compared with the FT-IR test before and after the test to show the results of evaluating biodegradability by comparing 2930 cm ^-1 absorbance. The biodegradability of the right figure is 37.2%, whereas the biodegradability of the ester base oil (left diagram), which is a synthetic oil, is 89.6%. Therefore, using synthetic oils other than mineral oils will have the effect of producing environmentally friendly greases that can fundamentally block the source of environmental pollution compared to conventional greases.

On the other hand, the stearic acid is added to 3 to 5% by weight of the total amount of grease, the oleic acid is preferably added to 0.1 to 0.3% by weight of the total amount of grease. The embodiment will be described below.

The second step is a step in which benzoic acid is dissolved in alcohol and stirred, and aluminum isopropoxide is added to the mixture of the stirred alcohol and benzoic acid and heated.

On the other hand, the benzoic acid is added to 1 to 3% by weight of the total amount of grease, the aluminum isopropoxide (Aluminum Isopropoxide) is preferably added to 2 to 4% by weight of the total amount of grease, the embodiment Will be explained below. Aluminum isopropoxide may also be referred to as aluminum isopropylate.

The third step is a step in which the mixture dissolved in the first step and the mixture produced in the second step are mixed with each other and heated.

The fourth step is a step of cooling by adding water to the mixture produced in the third step.

The fifth step is a step of adding a lubricating base oil to the mixture produced by cooling in the fourth step and heating to a constant temperature.

In a sixth step, after the fifth step, an additive including an extreme pressure additive is added and stirred to prepare a composite aluminum grease through milling.

The reaction mechanism of the composite aluminum grease prepared in the first to sixth steps is as follows.

The composite aluminum grease prepared in the first to sixth steps as described above is more effective than the conventional grease in terms of pole pressure resistance, abrasion resistance, and other performance, which will be shown through the following examples.

On the other hand, the benzoic acid is 1 to 3% by weight of the total amount of grease, the stearic acid is 3 to 5% by weight of the total amount of grease, the oleic acid is 0.1 to 0.3% by weight of the total amount of grease, the aluminum isopropoxide (Aluminum Isopropoxide ) Is preferably 2 to 4% by weight of the total amount of grease. This will be explained through the following examples.

On the other hand, the extreme pressure additive is a sulfur and antimony-based (antimony dialkyl dithiocarmate) extreme pressure additive or a fluorine-based (PTFE: Poly tetrafluoroethylene) extreme pressure additive.

The present invention is described in more detail with reference to the following Examples, but the present invention is not limited to these Examples.

[Example]

i) Mix two Polyol Ester base oils with a kinematic viscosity of about 50 and 400 cSt at an appropriate ratio to adjust the kinematic viscosity to about 120 cSt, and then add stearic acid and oleic acid at about two thirds of them, at 60 ° C for 30 minutes. Mix well to dissolve. ii) In a separate container, benzoic acid dissolved in methanol was added to mix well. After confirming that the solution was sufficiently dissolved, aluminum isopropoxide was added while gradually raising the temperature, and heated at about 104 ° C. until a clear solution appeared. Methanol, which was used as a reaction catalyst in this process, evaporated and generated a lot of foam, but continued stirring for about 30 minutes to completely extinguish the foam.

iii) The solution of acid mixed in i) was added to the solution of aluminum isopropoxide produced in ii) and dark grease formed with the release of isopropanol. The reaction was heated to 150 ° C. for 40 minutes after the alcohol had been removed. The reaction was then cooled to about 93 ° C. and a small amount of water added to neutralize unreacted isopropoxide. The release of more alcohol results in this result and a dark gel is formed. The mixture was heated to about 143 ° C. again, and the remaining 1/3 of Ester base oil was added to the mixture, and the mixture was heated to about 204 ° C. while stirring for about 3.5 hours to terminate the reaction. Thereafter, after cooling to about 90 ° C. naturally, additives other than the extreme pressure additive and the solid powder were added, and the product was finished by milling.

In the above [Example], the process for the preparation of the high-polarization wear-resistant composite aluminum grease was described. In Table 1 below, the blending ratio of benzoic acid, stearic acid, oleic acid, and aluminum isopropoxide (aluminum isopropoxide) was shown. According to the case of Examples 1 to 9. In Table 1, aluminum isopropoxide is briefly referred to as AIP.

In each case of Examples 1 to 9, the degree of gelation along with the soap formation process was confirmed through the lead test method of KS M 2037 and the titration test method of KS M ISO 2176, and the results are shown in [Table 2]. .

As can be seen from the above [Table 2], it can be seen that the formation of soap is different depending on the blending ratio, and as the blending amount is increased, the formation of soap is better and the gelation proceeds faster. And with the formation of a stable soap, the lead is lowered (hardened), and at the same time the dropping point is improved.

And the confirmatory test whether the reaction to the product according to Examples 1 to 9 was properly performed in the case of greases do not react in the reaction of fatty acids and AIP through the test method of free acid and free alkali of KS M 2038 The remaining free acid and free alkali could be confirmed, and the results are shown in [Table 3].

As can be seen from [Table 3], free alkali was not detected, and in the case of free acid, the higher the acid content, the higher the value. However, the presence of a large amount of unreacted free acid due to the high acid content does not mean that the soap is not formed. Rather, when the content of the free acid is low, soap was not formed well. This suggests that the reaction mechanism is not necessarily theoretically consistent.

In Example 1 to Example 9 of Table 1, the two reaction products having the best reaction state were added to other additives including extreme pressure additives and finally showed excellent quality (compound-1, Formulation-2) was tested for various performances compared to conventional grease (aluminum grease, lithium grease), and the results are shown in Table 4 below.

In Table 4, the results of the dropping test were shown by the evaluation of the stability of the heat of the grease. It is noted that the test method was KS M 2276. Looking at the dropping point test results through [Table 4], it can be seen that the composite aluminum grease of the formulation-1 and formulation-2 has a significant improvement in the dropping point than the general aluminum grease or lithium grease.

In addition, in Table 4, it can be seen that the mixing induction of the formulation-1 and the formulation-2 satisfies the development target value.

In addition, in Table 4, the degree of separation between the solid thickener and the liquid base oil was evaluated. The test method was based on KS M 2050, and the sample was filled in a 250 μm conical metal mesh and the amount of oil separated from the grease under the specified conditions was investigated. The results are shown in [Table 4]. Table 4 also shows the results of the test results, synthetic oil-based greases of the formulation-1 and formulation-2 are prepared with paraffinic mineral oil, which is generally used a lot better oil separation than grease prepared with naphthenic mineral oil. Oil separation was much better than grease.

In addition, the copper plate corrosion test, which is a test for evaluating the corrosiveness of the grease plate in [Table 4], was carried out by the test method KS M 2088. After leaving under the condition of discoloration of copper plate was investigated and the results are shown in [Table 4]. Looking at the results, all showed a pass state without discoloration.

In addition, the evaporation test was performed through the test method of KS M 2037 in Table 4, and the results showed that the greases of the compound-1 and the compound-2 using the synthetic oil were much better than those of the aluminum grease and the lithium grease.

In addition, in [Table 4], the water resistance, or flush water resistance test of grease is conducted by KS M 2087, which is filled with samples in rolling bearings and sprayed with water under prescribed conditions to investigate the amount of grease washed out. Table 4]. Looking at the results, it can be seen that Formulation-1 and Formulation-2 have better water resistance than other greases.

In addition, in Table 4, the miscibility test, which is a test for checking the mechanical stability and shear force of grease, was conducted by KS M 2137. The results of the miscibility test showed that the grease produced was significantly better.

In addition, the Timken method, which is an extreme pressure resistance test, was performed in [Table 4]. Among them, the test was performed by the Timken method of KS M 2026 according to the type and dosage of the extreme pressure additive, and the results are shown in [Table 5] below. In addition, the Timken test results according to the amount of the additive used when mixed with the additives are shown in [Table 6].

As can be seen from the above [Table 5], the effect on the polar pressure resistance of the fluorine-based extreme pressure additive was the greatest, and it was found that the extreme pressure was increased according to the amount added. And as can be seen from Table 6, when used in combination with a sulfur and antimony-based extreme pressure additive and a fluorine-based extreme pressure additive was found that the effect is improved than when used alone. In particular, the results obtained in [Table 6] are mentioned in the Timken load carrying capacity performance of [Table 4].

In addition, in Table 4, the rust resistance test, that is, the wet test, was conducted by KS M 2130, and the results showed that the results of Formulation-1 and Formula-2 were much better than those of other greases.

In addition, the oxidative stability test was carried out by KS M 2049 in [Table 4], and the results showed that the results of Formulation-1 and Formula-2 were much better than those of other greases.

Therefore, on the basis of these results, the composite aluminum grease according to the present invention has excellent shear stability and fluidity, hardly leaves residue when decomposed at high temperatures, and has a higher dropping point than general bearing greases, so that it can be used at relatively high temperatures. It also has excellent merit that it can be used at low temperature and high temperature. Therefore, it has good fluidity even at low temperatures, and thus has a very excellent effect on pumping performance than other greases, and thus can be advantageously used in intensive oil supply equipment.

In addition, it is excellent in water resistance and can be used in equipment that can penetrate moisture such as cooling water. It also has extreme pressure resistance, so it can be used in places where shocks, loads and loads are high and vibrations are severe.

Therefore, the composite aluminum grease produced by the manufacturing method of the present invention has an effect that can be used for general industrial purposes in addition to steelmaking facilities or cement manufacturing facilities, which have poor environmental conditions.

While the present invention has been described with reference to exemplary embodiments, it is to be understood that the invention is not limited to the disclosed exemplary embodiments. Therefore, the embodiments disclosed in the present specification are intended to illustrate rather than limit the present invention, and the scope and spirit of the present invention are not limited by these embodiments. The scope of the present invention should be construed according to the following claims, and all the techniques within the scope of the present invention should be construed as being included in the scope of the present invention.

Claims (5)

Stearic acid (Stearic acid) and oleic acid (Oleic acid) is added to the lubricating base oil by stirring at a predetermined temperature to dissolve;
A second step of dissolving and stirring benzoic acid in alcohol, and adding aluminum isopropoxide to the mixture of the stirred alcohol and benzoic acid and heating it;
A third step of mixing and heating the mixture dissolved in the first step with the mixture produced in the second step;
A fourth step of cooling by adding water to the mixture produced in the third step; And
And a fifth step of adding the lubricating base oil to the mixture produced by cooling in the fourth step and heating the mixture to a predetermined temperature.
The method of claim 1,
A sixth step of preparing a composite aluminum grease through milling after adding and stirring the additive including the extreme pressure additive after the fifth step; and a method of manufacturing a high extreme pressure wear-resistant composite aluminum grease further comprising .
3. The method according to claim 1 or 2,
The first step of the lubricating base oil is a method for producing a high extreme pressure wear-resistant composite aluminum grease, characterized in that the base oil is a mixture of ester base oils having different kinematic viscosity.
The method of claim 1,
The benzoic acid is 1 to 3% by weight of the total amount of grease, the stearic acid is 3 to 5% by weight of the total amount of grease, the oleic acid is 0.1 to 0.3% by weight of the total amount of grease, the aluminum isopropoxide (Aluminum Isopropoxide) is A method for producing a high extreme pressure wear resistant composite aluminum grease, characterized by containing 2 to 4% by weight of the total amount of grease.
The method of claim 2,
The extreme pressure additive is a sulfur and antimony-based (antimony dialkyl dithiocarmate) extreme pressure additive or a fluorine-based (PTFE: poly tetrafluoroethylene) extreme pressure additive, characterized in that the manufacturing method of high extreme pressure wear-resistant composite aluminum grease.

Images