RU2278151C1 - Method for preparing additive for lubricant oils - Google Patents

Abstract

FIELD: petroleum chemistry, chemical technology.

SUBSTANCE: invention relates to synthesis of additives for lubricant oils. Method involves the condensation reaction of tributyl phosphite in carbon tetrachloride solution, vacuum distillation of the condensation products resulting to preparing the end product and light-boiling fraction, and additional treatment of light-boiling fraction with tributyl phosphite in the mole ratio = 1.0-2.5, respectively followed by vacuum distillation of the reaction products resulting to preparing the end product and butyl chloride. Vacuum distillation at both stages is carried out at temperature 30-60°C under pressure 4-40 mm of mercury column. The condensation reaction and treatment of light-boiling fraction with tributyl phosphite are carried out at the solvent boiling point. Invention provides enhancing yield and preparing the additive by the wasteless technology and with improved properties.

EFFECT: improved preparing method of additive.

1 ex

Description

The present invention relates to the field of petrochemistry, specifically to a method for producing additives for lubricating oils.

Active additives to lubricating oils that reduce wear during friction under heavy loads are organic compounds containing chlorine and phosphorus. Among them, the most effective are substances containing a trichloromethyl group, for example esters of chloroalkylphosphonic acids.

Dichutyl ether of trichloromethylphosphonic acid has found practical application as an antiwear additive to lubricating oils. (A.M. Kuliev "Chemistry and technology of additives to oils and fuels", Chemistry, 1985, p.121-122).

A known method of producing trichloromethylphosphonic acid dibutyl ester by reacting trichloromethylphosphonic acid dichloride and butyl alcohol in the presence of triethylamine ("Additives to oils and fuels", Moscow, 1961, p. 68).

However, this method has not found industrial application due to the complexity of obtaining one of the starting components - trichloromethylphosphonic acid dichloride.

Closest to the claimed one is a method of producing an additive for Chloref-40 oils, including the condensation reaction of tributyl phosphite in a solution of carbon tetrachloride at a boiling point of a solvent and subsequent vacuum distillation of the condensation products with separation of the target product from excess carbon tetrachloride and a by-product of butyl chloride ("Additives to butyl chloride oils and fuels ", Moscow, 1961, p.69).

The disadvantage of this method is that the additive obtained is not a sufficiently pure trichloromethylphosphonic acid dibutyl ester. The additive contains a significant amount of low-boiling fraction, which is a difficult to disperse and environmentally hazardous mixture of carbon tetrachloride and butyl chloride and partially dibutyl phosphite. The content of the additive in the composition of up to 30 wt.% This fraction significantly worsens its environmental properties, and also makes it substandard: it increases the acid number, and due to this, the corrosivity of the additive; reduces density and chlorine content. Since the low boiling fraction is ballast, the yield of the additive obtained in a known manner is low.

The objective of the present invention is to develop a method that allows to increase the yield of additives and improve its operational and environmental properties.

To solve this problem, we propose a method for producing additives for lubricating oils, including the condensation reaction of tributyl phosphite in a solution of carbon tetrachloride, vacuum distillation of condensation products to obtain the target product and low boiling fraction, additional processing of the low boiling fraction with tributyl phosphite in a molar ratio of 1.0-2.5, respectively vacuum distillation of the reaction products to obtain the target product and butyl chloride and the implementation of vacuum distillation in both stages at a temperature D 30-60 ° C and a pressure of 4-40 mm Hg

Moreover, the condensation reaction and processing of the boiling fraction with tributylphosphite is carried out at the boiling point of the solvent.

The proposed method differs from the known one in that it includes an additional stage — treatment of the low-boiling fraction with tributylphosphite at a given molar ratio of components with subsequent vacuum distillation of the reaction products. In this case, vacuum distillation at both stages is carried out under certain conditions.

These differences allow the separation of the mixture of butyl chloride-carbon tetrachloride, due to which the ballast content in the target product is reduced (no more than 6 wt.%) And the resulting additive is almost pure trichloromethylphosphonic acid dibutyl ether. The resulting additive due to a higher degree of purification has improved anti-wear, extreme pressure and environmental properties. In addition, when implementing the proposed method, along with the target product, butyl chloride is obtained containing not more than 5 wt.% Carbon tetrachloride, which can be used as a reagent for organic synthesis.

Thus, the proposed method, carried out by non-waste technology, allows to increase the yield of additives to lubricating oils with improved properties.

The following is an example implementation of the proposed method.

Example.

To 1.25 moles of boiling carbon tetrachloride, 1 mole of tributylphosphite is portionwise added dropwise, after completion of the dropping, the reaction is carried out for another 5 hours at a temperature of 50 ° C. After that, the condensation products are dispersed on a rotary-film evaporator at a temperature of 40 ° C and a pressure of 40 mm Hg. 1 mol of the additive and 1.2 mol of the low boiling fraction are obtained, which is treated with 1.25 mol of tributyl phosphite at the boiling point of carbon tetrachloride with constant stirring for 6 hours. After that, the reaction products are subjected to vacuum distillation on a rotary film evaporator at a temperature of 40 ° C and a pressure of 40 mm RT.article. Get 1 mol of additive and 1 mol of butyl chloride.

The resulting additive has the following characteristics

Indicators Received sample TU requirements Density d ²⁰ ₄ 1.1475 1.1050-1.220 Refractive Index, n ²⁰ _D 1,4508 1.4320-1.4600 Chlorine content thirty Not less than 26.0 Acid number, mg KOH / g 2.26 No more than 15 Copper plate corrosion Lack of Lack of

The data show that the additive obtained by the proposed method fully meets the requirements of the technical conditions, while the yield of the additive increases by 15 wt.%.

Anti-seize and anti-wear properties of the additive were evaluated using a four-ball friction machine (FWM). The tests showed that the introduction of 1.2-1.4 wt.% Additives obtained by the proposed method in transmission oils with a viscosity of not more than 15.5 cSt (T-14, MV-2F and others) containing additives of the type DF- 11, VNIINP-354, TsD-7, made it possible to improve the extreme pressure and antiwear properties of oils and to achieve indicators of a wear spot of 0.38-0.42 mm and a welding load of 425-450 MPa.

Claims (2)

1. The method of producing additives for lubricating oils, including the condensation reaction of tributyl phosphite in a solution of carbon tetrachloride, vacuum distillation of the condensation products to obtain the target product and low boiling fraction, characterized in that the low boiling fraction is further treated with tributyl phosphite in a molar ratio of 1.0: 2.5, respectively , the resulting reaction products are subjected to vacuum distillation with the release of the target product and butyl chloride, while the vacuum distillation of the reaction products at both stages suschestvlyayut at a temperature of 30-60 ° C and a pressure of 4-40 mm Hg 2. The method of producing the additive according to claim 1, characterized in that the condensation reaction and the treatment of the low-boiling fraction with tributylphosphite are carried out at the boiling point of the solvent.