SU653290A1 - Method of obtaining additive to oil products - Google Patents

Description

This invention relates to a method for producing an additive that is a metal deactivator added to lubricating, insulating and hydraulic oils and hydrocarbon fuels to protect the surfaces of copper, its alloys and steel contaminated with oil or fuel, and passivation, from corrosion. surfaces of these metals and their oil-soluble compounds catalyzing the oxidation of oils and fuels. The corrosion of oils and fuels with respect to metals can be caused by the presence in oils and fuels of natural corrosive compounds, sulfur-containing additives or the formation of corrosive compounds during the oxidation of oils and fuels. Benzotriazole and its alkyl substitutes are known as effective deactivators of metals in aqueous and polar organic liquids. including in antifreezes 1 However, benzotriazole and its alkyl-substituted slightly soluble in hydrocarbon oils and fuels, especially at temperatures below and for this reason cannot be applied to in such oils and fuels. Known methods for the preparation of deactivators of metals based on benzotriazole, soluble in hydrocarbon oils and fuels, the interaction of (Cd-C alkl) - or (Cd-C-alkenyl) succinic anhydride with benzotriazole or methylbenzotriazole (21, the interaction of alkyl- or alkenyl succinic anhydride with benzotriazole or its alkyl-substituted and subsequent neutralization of the reaction product with alkanolamine 3J. A known method of obtaining an additive to petroleum products by benzotriazole or its alkyl-substituted with oil-soluble organic primary nitrogen-containing compound, for example, with di-2-ethylhexylamine, a mixture of primary (. -greg-alkyl) amines 4. However, the benzotriazole derivatives obtained by these methods are not stable enough in solutions of oils and fuels, especially at temperatures above 150 ° C and therefore, they are not sufficiently effective. The aim of the invention is to increase the thermal stability of the additive. The goal is achieved by the fact that in the process for the preparation of additives for oil products by the interaction of benzotriazole or its alkyl-substituted organic skim compound as an organic compound, a mixture of the aldehyde. with alkylphenol mol, c. 200-400 at the molar ratio of benzotriazole, aldehyde and alkylphenol, equal to 1:11, 4: 1-1.2. The optimum reaction temperature is 100-180 ° C. The reaction is carried out without a solvent or in a solvent selected from hydrocarbon oils, gasolines, benzene alkanes, xylene toluene, alcohols, dimethyl form amide, dimethyl sulfoxide, dioxane, and ch. Alkyl-substituted benzotriazole contains 1-2 alkyl in the benzene ring. During the interaction, the main reaction occurs according to the equation where R is alkyl; hydrogen or alkyl; R is hydrogen or alkyl. As a result of the reaction, a thermally stable d6 product of 250 ° C and higher is obtained. Example 1 A four-necked glass reactor equipped with a stirrer, an addition funnel, a reflux condenser, and a tube for the current of nitrogen are charged with a solution of 119 g {1 mol of benzotriazole in 200 g of isopropaial and a solution of 261 g (1 mol) of technical alkylphenol (mixture of hydrophenol obtained by alkylation of the phenyl fraction of propylene tetramers) in 200 g toluol. The reaction is carried out in a nitrogen atmosphere. 33 g (1 mol) napiaform (90%) and 2 g tetramethylene tetramine, which improves the color of the product, are added to the stirred mixture. The mixture is heated to boiling for 1 h, boiled for 1 h and filtered. Solvents, formed water, and Volatile components are distilled off from the filtrate when the mixture is heated to and under vacuum to No. Hg. 289 g of metal deactivator additive are obtained in the form of a transparent yellow viscous liquid, viscosity 178est (), nitrogen content: found 10.6%, calculated 10.7%, Example 2. In the same glass reactor as in example 1, load a solution of 147 g {1 mol) 5-ethylbenzotriazole in 200 g of a mixture of equal weight quantities of ethyl alcohol and dimethylformamide and a solution of 254 g (1 mol) (CdC alkyl) phenol with an average mol. at. 254 (obtained by alkylation of phenol with a mixture of propylene tetramers and diamylene) in 250 g of gasoline Galosh. 49 g (1.1 mol) of acetic aldehyde is added dropwise to the stirred mixture at 25 ° C over 0.5 h. The mixture is stirred at elevated temperature until boiling and boiled for 2 h, then filtered. From the filtrate, the solvents are distilled off and the water formed is initially at atmospheric pressure to the temperature of the liquid, and then under vacuum to the liquid temperature of mm Hg 421 g of the deactivator additive are obtained in the form of a transparent yellow viscous liquid, viscosity 138 eats (), nitrogen content: 9.9% found, 9.84% calculated. Example 3. In the same glass reactor as in Example 1, 133 g (1 mol) of 5-methylbenzotriazole and 280 g (1.1 mol) of (. -Alkyl) phenol with an average mol% were charged. 254 (obtained by alkylation of phenol with a mixture of propylene tetramers and diamylene). 86.5 g (1.2 mol) of oil aldehyde are added dropwise to the stirred mixture at 45 ° C over 1 hour, after which the temperature of the mixture rises to 3 hours and is kept for 2 hours under vacuum at mm Hg st., then the hot mixture is filtered. 456 g of the deactivator additive are obtained in the form of a transparent yellow viscous liquid, in SQ6ST, S 72 eats (100 ° C), nitrogen content: found 8.8%, calculated 8.99%. The test of the obtained deactivator additives in oils and fuels for corrosion in relation to copper is carried out according to GOST 2917-45, but for 3 hours and with an assessment of the color of the copper plate in points according to ASTM-D 130-68 (1A - surface without changes, 4C - the surface is black). 3% dibenzyl sulfide (anti-seize additive) is added to the base oils to give the oil corrosive properties with respect to copper. The test results are presented in table 1. The test results presented in Table 1 show that the metal deactivator obtained by the proposed method retains its effect after heating in an oil solution during and after storage in the fuel solution at 5 for 1 month, while the metal deactivator 4j is destroyed under the conditions of tests and loses its effectiveness

The test of oil AC-b {viscosity near b-hundred (), used as a base lubricant and hydraulic oil, with the addition of corrosion additives for steel and copper, is made according to GOST 9.044-75: after 500 ml of oil is blown off 30 l / h of humid air at an oil temperature for 12 hours in the presence of plates of steel, copper and lead. Test data are given in table 2.

The DS-11 base oil base test with corrosivity / additives for lead bronze mark Br. SZO (GOST 493-54), 70% of copper and 30% of lead used to make bearings for internal combustion engines, were produced according to GOST 13517-68 at 160 ° C for 25 hours in the presence of 0.02% copper naphthenate but with a lead plate on the platesTable

KU of bronze Br.SZO. Test data are given in table 3.

Transformer oil with a deactivator is tested for corrosion in relation to copper according to GOST 2917-45, but for 24 hours and with an assessment of the color of the copper plate in points according to ASTM-D 130-68. Test data are given in table 4.

The test results presented in Tables 1–4 show that the additive obtained by the method protects copper, its alloy and steel from corrosion, and also protects copper in case of P1 and is contained in oil with anti-contaminant sulfur-containing anti-corrosion from corrosion. cages.

The properties of this plant enable it to be widely used in lubricating, hydraulic and insulating oils and hydrocarbon fuels to reduce the corrosion of copper, its alloys and steel, which increases the durability of mechanisms and apparatus and reduces the costs of their weight.

Continued table. one

Transparent1B

Nef- No priodok cage

3% di1 babenzile disul4S

Same fida

1 ba3% dibeisile disulfide + 0.05% deactivator in example 11B 3% di-babenzyl disulfide + 0.05% deactivator from example 2

3% di 11 babenzyl disulfide + 0.05% deactivator from example 3

1B 3% di 11 babenzyl

2C

Turbid 3% diV

Transparent disulfide filter of walkie talkie

Muddy

4C

The same before filtration with an equimolar amount of smbsi for 1 h. primary (by the interaction of benzotrnazole, obtained tert-alkyl) with

No additive 0.3

0.1% deactivator from example 1 0.0

0.2% deactivator from Example 1 0.0

0.2% deactivator from example 3 0.0

Butter

Without additive 19,7

11 basic

0,.% Deactivagor from example 10.9 11 basic

0.2% deactivator from Example 2, 4 11 bas.

0.2% deactivator from example 30.1 11 baseline

Butter

0.02% deactivator from example 1

6.05% deactivator from example 1

table 2

0.4 2.8 5.2

0.05 .0.8 1.1

0.0 0.2 0.0

0.0 0.0 0.0

Ta lb and c and 3

Additive

Weight loss

bronze

g / m2

Table 4

Additive

Copper color

records

score

BEHIND

No additive

1B

(

1А 6 11 For {mMula iabbrete and 1.Spos about sex at 4ie neither at the moment with the oil nor to the oil stSHU th W by means of ТSH | eTe1111 | 5Sheola or; ёga g6 Гс ё1) gayy бbyym sёdinyonyom, ht and h and with the fact that, with tseijiiJb ysyyvShyyyi: fei: MH4eckoft stable T yy1dk; and alkyl enol, iSaiSBM 1: 1-1 4: 1-1.2. 2. Method rib p.1, about tl and h in h and with the fact that the interaction of benzoylbenyl and its alkyl-substituted with aldehyde and gkylphenol is carried out at 100-180 0. 3. method POPP.1I 2, o t l and the fact that the interaction of benzotriol or its alkyl-substituted with aldehyde and alkylphenol p {ovod t in a solvent from among hydrocarbon oils, gasolines, alkanes of benzene, toluene, xylenes, alcohols, dimethylformamide, dimethylsulfoxide, dioxane and their mixtures. Sources of information taken into account in the examination 1. Alshlbeeva A.I. Inhibitors of corrosion of metals, 1968, p. 27-28. 2. US patent No. 3788993, cl. 252-51.5A, 1974. 3. US Patent No. 3897351, cl. 2552-34. 4. Patent of Great Britain No. 1319246, cl. C 2 C, 1973.