RU2804800C1 - Method for making fatty grease - Google Patents

Abstract

FIELD: chemical technology.

SUBSTANCE: chemical technology for producing plastic grease lubricants. Method is disclosed for obtaining fatty grease by mixing 1/2 part of the mass of purified used motor oil heated to 50-70°C with unrefined sunflower vegetable oil and addition of lime milk comprising 0.2 mol/l sodium hydroxide solution comprising graphite with a plate thickness of less than 100 nm and a concentration in the range of 15-850 ppm by weight of grease, saponification at a temperature of 95-105°C for at least 1 hour, followed by the addition of the remaining 1/2 part of the purified used engine oil. At the same time, in the process of mixing heated purified used engine oil with unrefined vegetable oil, as an antiwear additive, α-form of copper phthalocyanine in the form of a suspension in an organic solvent in an amount based on the final content in the product from 0.05 to 5 wt.% is added.

EFFECT: reduction of wear of machine parts.

3 cl, 1 tbl, 2 ex

Description

The invention relates to chemical technology for producing plastic grease lubricants and solves the problem of reducing wear by 16.4%. The claimed result is achieved by introducing the α-form of copper phthalocyanine into a lubricant based on purified used motor oil, thickened with calcium soap of unsaturated fatty acids, modified with graphite nanoplates less than 100 nm thick. Layered particles of copper phthalocyanine are introduced at the initial stage of obtaining fatty grease - mixing heated purified waste motor oil and unrefined sunflower vegetable oil. The modifier is added in the form of a suspension in an organic solvent. Mixed petroleum solvent NEFRAS C2 80/120 is used as an organic solvent. In order to obtain stable suspensions of the α-form of copper phthalocyanine, its concentration in the organic solvent does not exceed 18% by weight of the suspension. Excess solvent is distilled off during the saponification process and reused in production. Used motor oil is used as base oil. The advantages of the proposed grease oil include a longer service life of machine parts due to low wear rates and a solution to the environmental problem of recycling used motor oils.

There is a known method for producing a grease containing a base oil and soap based on a calcium complex as a thickener, where the fatty acids in the soap based on the calcium complex are substituted or unsubstituted straight-chain higher fatty monoacid containing from 18 to 22 carbon atoms, an aromatic monoacid, containing a substituted or unsubstituted benzene ring, and a straight-chain saturated lower monoacid selected from acetic acid, propionic acid, butyric acid or combinations thereof, characterized by a high dropping point (RU No. 2637123).

The disadvantage of this method is the use of fatty acids, which require consistent and complex processing.

There is a known method for producing fatty grease containing calcium salts of higher fatty acids as thickeners. Mineral oils of various brands and raw glycerin, a waste product from biodiesel production containing glycerin, methyl esters of fatty acids and potassium salts of fatty acids, are used as feedstock for producing lubricants. The lubricant is obtained by treating a mixture of raw glycerin with mineral oil with calcium chloride in an anhydrous environment at a temperature of 60-100 °C for 4-6 hours and subsequent separation from the liquid glycerin layer of the resulting viscous-plastic mass, which is a plastic calcium lubricant (RU No. 2631112).

The disadvantages of this method is the use of calcium chloride, which, if not completely released from the lubricant, will lead to an increase in the hygroscopicity of the product.

There is a known method for producing a lubricant based on a calcium thickener by mixing fatty acids, calcium acetate, calcium hydroxide and mineral petroleum oil. A mixture of mineral oil and fatty acids is heated and a suspension of calcium acetate, calcium hydroxide in the remaining mineral oil is added. The resulting mixture is saponified at a temperature of 200-250°C, cooled and homogenized (GB No. 1399155).

The disadvantage of this method is the use of expensive calcium acetate and the existing need for fatty acids, as well as high energy costs during heat treatment and the need to use a homogenizer.

There is a known method for producing an anhydrous grease containing the following components by weight: 82-90% base oil, 1-4% calcium hydroxide, 6-15% fatty acid, 0.3-1% antioxygen, 0.5-1.5%. rust inhibitor and 0.5-3% extreme pressure anti-wear additive (CN #102757847B).

The main disadvantage of this method is the use of expensive raw materials – fatty acids.

There is a known method for producing a grease consisting of mineral oil and calcium salts of synthetic fatty acids. Synthetic fatty acids contain 20 or more carbon atoms in the chain. At the first stage, fatty acids are subjected to oxidation by atmospheric oxygen at a temperature of 100-160 °C. Oxidation time is 10-24 hours until the hydroxy acid content is 10-30 wt. %. Next, the oxidation product is mixed with mineral oil, the mixture is heated to a temperature of 80 °C, calcium hydroxide is added to it and kept with stirring for 3-4 hours at a temperature of 100-140 °C until saponification is completed (RU No. 2163628).

The disadvantages of this method are the use of expensive raw materials - synthetic fatty acids, as well as the high energy consumption of the process at the stage of long-term oxidation.

There is a known method for producing fatty grease, which has the following composition, wt.%: calcium hydroxide 2.0-3.0, water 0.3-2.5, products of distillation during deodorization of vegetable oil by distillation 9.0-18.0, petroleum oil - the rest. In this way, a lubricant is obtained that can be used in rolling and sliding friction units of machines and mechanisms operating at temperatures from minus 25 °C to plus 65 °C (RU No. 2271381).

The disadvantages of this method are the low maximum temperature for using the lubricant and low load-bearing capacity.

There is a known method for producing a greasy composition used for lubrication of heavily loaded open gears, steel ropes, tractor chassis and other sliding pairs of non-precision mechanisms. The composition contains, wt.%: synthetic molybdenum disulfide 1-3, graphite 7-10, fuel oil 2-5, grease up to 100 (RU No. 2200185).

The disadvantages of this method are the high consumption of graphite required to ensure good consumer properties, and the use of expensive equipment for introducing graphite into the lubricant.

The closest analogue to the claimed method for producing fatty grease by mixing 1/2 part of the mass of purified used motor oil heated to 50-70 °C with unrefined sunflower vegetable oil and adding lime milk containing 0.2 mol/l sodium hydroxide solution containing graphite with a thickness plates less than 100 nm and a concentration within 15-850 ppm of the solid oil mass, saponification at a temperature of 95-105 ° C for at least 1 hour, followed by the addition of the remaining 1/2 part of purified used motor oil. Graphite is produced in a sodium hydroxide solution by electrochemical exfoliation of thermally expanded graphite foil. (RU No. 2764085).

The disadvantage of this method is the inadequate protection against wear of the surfaces of machine parts. The technical objective of this invention is to reduce the wear of machine parts by modifying the fatty grease with layered particles of the α-form of copper phthalocyanine. By using used motor oils as base oil, an environmental problem is solved.

The technological problem is solved as follows:

1. A method for producing fatty grease by mixing 1/2 part of the mass of purified used motor oil heated to 50-70 °C with unrefined sunflower vegetable oil and adding lime milk containing 0.2 mol/l sodium hydroxide solution containing graphite with a plate thickness of less than 100 nm and a concentration in the range of 15-850 ppm from the mass of solid oil, saponification at a temperature of 95-105 ° C for at least 1 hour, followed by the addition of the remaining 1/2 part of purified used motor oil, characterized in that during the process of mixing heated purified waste motor oil with unrefined vegetable oil, the α-form of copper phthalocyanine is added as an anti-wear additive in the form of a suspension in an organic solvent in an amount based on the final content in the product from 0.05 to 5% wt.

2. The method for producing fatty grease according to claim 1, characterized in that NEFRAS C2 80/120 is used as an organic solvent.

3. The method for producing fatty grease according to claim 1, characterized in that the concentration of the α-form of copper phthalocyanine in the organic solvent is no more than 18% by weight.

Let's consider examples of the implementation of the method for producing solid oil.

Example 1

100 g of purified used motor oil and 80 g of sunflower vegetable oil were loaded into a 500 ml three-neck flask. The mixture was heated to 60 °C with constant stirring using an overhead paddle mixer. A 15% suspension of the α-form of copper phthalocyanine in an organic solvent was added to the flask at a final content of 0.01% in the product. The flask was filled with lime milk, which was prepared in advance in a glass beaker and contained 12 g of calcium hydroxide, a suspension of graphite in a solution of sodium hydroxide with a solid phase concentration of 2 g/l, added based on the final content of graphite in the product of 850 ppm. The concentration of sodium hydroxide is 0.2 mol/l. Next, the mixture was heated to 95-100°C and the saponification process was carried out for 2 hours. After the saponification time had passed, the heat was turned off and another 100 g of purified used motor oil was added. The mass was stirred for 15 minutes. Color of viscoplastic phase: light brown; consistency: homogeneous, viscous, with good adhesion to metal and glass.

For the resulting grease, the dropping point was determined according to GOST 6793, the proportion of free alkali in terms of NaOH and organic acids according to GOST 6707, the proportion of water according to GOST 2477 and the wear limit according to GOST 9490.

Physico-chemical indicators of grease in comparison with GOST indicators are given in Table 1.

Example 2

100 g of purified used motor oil and 80 g of sunflower vegetable oil were loaded into a 500 ml three-neck flask. The mixture was heated to 60 °C with constant stirring using an overhead paddle mixer. A 15% suspension of the α-form of copper phthalocyanine in an organic solvent was added to the flask at a final content of 0.01% in the product. The flask was filled with lime milk, which was prepared in advance in a glass beaker and contained 12 g of calcium hydroxide, a suspension of graphite in a solution of sodium hydroxide with a solid phase concentration of 2 g/l, added based on the final content of graphite in the product of 15 ppm. The concentration of sodium hydroxide is 0.2 mol/l. Next, the mixture was heated to 95-100°C and the saponification process was carried out for 2 hours. After the saponification time had passed, the heat was turned off and another 100 g of purified used motor oil was added. The mass was stirred for 15 minutes. Color of viscoplastic phase: light brown; consistency: homogeneous, viscous, with good adhesion to metal and glass.

For the resulting grease, the dropping point was determined according to GOST 6793, the proportion of free alkali in terms of NaOH and organic acids according to GOST 6707, the proportion of water according to GOST 2477 and the wear limit according to GOST 9490.

Physico-chemical indicators of grease in comparison with GOST indicators are given in Table 1.

Example 3

100 g of purified used motor oil and 80 g of sunflower vegetable oil were loaded into a 500 ml three-neck flask. The mixture was heated to 60 °C with constant stirring using an overhead paddle mixer. A 15% suspension of the α-form of copper phthalocyanine in an organic solvent was added to the flask at a final content of 0.05% in the product. Lime milk was poured into the flask, which was prepared in advance in a glass beaker and contains 12 g of calcium hydroxide, a suspension of graphite in a solution of sodium hydroxide with a solid phase concentration of 2 g/l, added based on the final content of graphite in the product of 150 ppm. The concentration of sodium hydroxide is 0.2 mol/l. Next, the mixture was heated to 95-100°C and the saponification process was carried out for 2 hours. After the saponification time had passed, the heat was turned off and another 100 g of purified used motor oil was added. The mass was stirred for 15 minutes. Color of viscoplastic phase: brown; consistency: homogeneous, viscous, with good adhesion to metal and glass.

For the resulting grease, the dropping point was determined according to GOST 6793, the proportion of free alkali in terms of NaOH and organic acids according to GOST 6707, the proportion of water according to GOST 2477 and the wear limit according to GOST 9490.

Physico-chemical indicators of grease in comparison with GOST indicators are given in Table 1.

Example 4

100 g of purified used motor oil and 80 g of sunflower vegetable oil were loaded into a 500 ml three-neck flask. The mixture was heated to 60 °C with constant stirring using an overhead paddle mixer. A 15% suspension of the α-form of copper phthalocyanine in an organic solvent was added to the flask at a final content of 0.05% in the product. The flask was filled with lime milk, which was prepared in advance in a glass beaker and contained 12 g of calcium hydroxide, a suspension of graphite in a solution of sodium hydroxide with a solid phase concentration of 2 g/l, added based on the final content of graphite in the product of 850 ppm. Next, the mixture was heated to 95-100°C and the saponification process was carried out for 2 hours. After the saponification time had passed, the heat was turned off and another 100 g of purified used motor oil was added. The mass was stirred for 15 minutes. Color of viscoplastic phase: light brown; consistency: homogeneous, viscous, with good adhesion to metal and glass.

For the resulting grease, the dropping point was determined according to GOST 6793, the proportion of free alkali in terms of NaOH and organic acids according to GOST 6707, the proportion of water according to GOST 2477 and the wear limit according to GOST 9490.

Physico-chemical indicators of grease in comparison with GOST indicators are given in Table 1.

Example 5

100 g of purified used motor oil and 80 g of sunflower vegetable oil were loaded into a 500 ml three-neck flask. The mixture was heated to 60 °C with constant stirring using an overhead paddle mixer. A 15% suspension of the α-form of copper phthalocyanine in an organic solvent was added to the flask at a final content of 0.05% in the product. The flask was filled with lime milk, which was prepared in advance in a glass beaker and contained 12 g of calcium hydroxide, a suspension of graphite in a solution of sodium hydroxide with a solid phase concentration of 2 g/l, added based on the final content of graphite in the product of 15 ppm. Next, the mixture was heated to 95-100°C and the saponification process was carried out for 2 hours. After the saponification time had passed, the heat was turned off and another 100 g of purified used motor oil was added. The mass was stirred for 15 minutes. Color of viscoplastic phase: brown; consistency: homogeneous, viscous, with good adhesion to metal and glass.

For the resulting grease, the dropping point was determined according to GOST 6793, the proportion of free alkali in terms of NaOH and organic acids according to GOST 6707, the proportion of water according to GOST 2477 and the wear limit according to GOST 9490.

Physico-chemical indicators of grease in comparison with GOST indicators are given in Table 1.

Table 1. Characteristics of grease samples

GOST requirements Serial sample Example 1 Example 2 Example 3 Example 4 Example 5 Dropping point, °C 78 89 89 86 93 83 91 Mass fraction of free alkali in terms of NaOH, % 0.20 0.15 0.14 0.15 0.18 0.16 0.18 Free organic acid content Absence Absence Absence Absence Absence Absence Absence Mass fraction of water, % 2.50 2.40 2.41 2.30 2.32 2.35 2.49 Wear limit value, mm 0.215 0.216 0.203 0.180 0.191 0.211

Claims (3)

1. Method for producing fatty grease by mixing 1/2 part of the mass of purified used motor oil heated to 50-70 °C with unrefined sunflower vegetable oil and adding lime milk containing 0.2 mol/l sodium hydroxide solution containing graphite with plate thickness less than 100 nm and a concentration within 15-850 ppm of the solid oil mass, saponification at a temperature of 95-105 ° C for at least 1 hour, followed by the addition of the remaining 1/2 part of purified used motor oil, characterized in that during the process of mixing heated purified used motor oil with unrefined vegetable oil, the α-form of copper phthalocyanine is added as an anti-wear additive in the form of a suspension in an organic solvent in an amount based on the final content in the product from 0.05 to 5% wt. 2. The method for producing fatty grease according to claim 1, characterized in that NEFRAS C2 80/120 is used as an organic solvent. 3. The method for producing fatty grease according to claim 1, characterized in that the concentration of the α-form of copper phthalocyanine in the organic solvent is no more than 18% by weight.