SU755831A1 - Method of preparing additive to lubricating materials - Google Patents

Description

The invention relates to the production of additives, to lubricants.

A known method for producing an ashless dispersant additive for lubricating oils by the interaction of alkyl phenol, polyalkylene polyamine and aldehyde, for example, formaldehyde [ΐ].

A known method of producing additives for lubricants by the interaction of alkyl phenols, where C ₅₀ -C, _оо , formaldehyde and polyamines Η (ΝΗΑ) _χ ΗΗ ₂ , where A is alkylene C ^ -Cd, X = 1-10. The reaction is carried out at 5095 ° C [2]. fifteen

The resulting additive has only a dispersing effect, but has unsatisfactory antioxidant properties,

The purpose of the invention is the development of a method for producing an additive having improved detergent-dispersing and antioxidant properties.

This goal is achieved 25 by the fact that in the method of producing additives to lubricants by reacting a phenol derivative with polyamine and formaldehyde at elevated temperatures, polybutene-oxy-benzyl pol and an amine of the general formula are used as polyamine

HE

K - £ 0) ΌΗ -ΝΗ- ₂ AH, where A - _6D hydrocarbon radical -C _Lo A = (- CH ₂ -CH ₂ G-invariant) _{n, n} = 2-4, or -C-ΝΗ-) and as a phenol derivative, a compound of the general Formula is used

HE

where K ₂ , _KE , K ₄ is hydrogen or C С-C ₄ alkyl or an amino group or an oxy group, one of the radicals being hydrogen and a phenol derivative molecule contains 1-2 hydroxy groups and one amino group, and the process is carried out at a polybutene molar ratio -oxy-benzylpolyamine: phenol derivative: formaldehyde equal to 1: 1-4: 1-4.

The method is carried out as follows.

755831

To polybutene-hydroxybeneylpolyamine (1), which is a condensation product of polybutenphenol with a molecular weight of 800-2000 with polyamine and formdehyde, a phenol derivative (II) is added with stirring, in an amount of 1-4 mol per 1 mol of polybutenoxy-benzylpolyamine, raise the temperature to 85-120 ° C and maintain it for 0.5-1 h, then add formaldehyde in an amount of Ί-4 mol per 1 mol of polybutene-hydroxy-benzylpolyamcna and slowly raise the temperature to 145-170 ° C for 2 -3.5 h. '

Stirring is carried out for one hour at this temperature, after which the reaction mass is cooled and dissolved in benzene or toluene, centrifuged, then the solvent is distilled off at atmospheric pressure, then under vacuum, 5-15 mm Hg. the mixture is heated to 200-225 ° C.

The resulting compound is introduced in an amount of 0.1-5 wt.% In the lubricant. oil.

The method allows to obtain an additive to lubricating oils with improved detergent-dispersing and antioxidant properties. In addition, the resulting additive has a higher thermal stability than the original polybutene-hydroxybenzylpolyamine (high molecular weight Mannich base).

Example 1. K132 g (0.1 mol) of polybutec-hydroxybenzyltetraethylenephenamine obtained by Mannich’s condensation of polybutenphenol with tetraethyl npentamine and formaldehyde and having a molecular weight of 1330 and containing 4.7% nitrogen was added with stirring 80 g (0.4 mol)

-2,6-ditretbutylphenol, heated to 115 ° C and added 16 g (0.4 mol) of formaldehyde (paraform) and the mixture was kept at this temperature for 2 hours, then the temperature was slowly raised to 160 ° C and kept for 1 hour (in this time there is an intensive release of water).

The reaction mass is cooled, dissolved in benzene, centrifuged, then benzene is distilled off at atmospheric pressure, then under a vacuum of 515 mm Hg. the reaction mixture is heated to 200-230 ° C.

The resulting compound has the formula,.

where I is the hydrocarbon radical C ^ -C ^ and the molecular weight of 2100, contains 2.6% nitrogen.

Example 2. The treatment of 132 g (0.1 mol) of polybutene-hydroxy-tetraethylene pentamine is carried out with 60 g (0.3 mol} of 2,4-ditretbutylphenol and 12 g (0.3 mol) of formaldehyde as described in example 1.

The resulting compound has a molecular weight of 2000 and contains 3.4% nitrogen.

Example 3. To 132 g (0.1 mol) of polybutene-hydroxy-benzyltetraethylene pentamine, 16.7 g (0.1 mol) of 2-methyl-4-tert-butylphenol and 4 g (0.1 mol) of formaldehyde are added and the reaction is carried out as indicated in example 1 ..

The resulting compound has a molecular weight of 1600 and contains 4.1% nitrogen.

Example 4, Treatment of 132 g (0.1 mol) of polybutene-hydroxy-benzyltetraethylene pentamine is carried out with 22 g (0.2 mol) of resorcinol and formaldehyde (paraform) as described in example 1. The resulting product has a molecular weight of 1580 and contains 4.0% nitrogen.

Example 5. To 125 g (0.1 mol) of polybutene-hydroxybeneylthiourea based on polybutenphenol (molecular weight 1200), thiourea and paraform, 22 g (0.2 mol) of aminophenol and 40 g (0, 25 mol) of a 40% aqueous solution of formaldehyde (formalin), raise the temperature of the mixture to 95 ° C and hold for 3.5 hours, then the temperature is slowly raised to 150 ° C, hold for 1 hour, then the reaction mass is cooled, dissolved in benzene , centrifuged, distilled off the solvent.

The resulting product has the formula

where K is the hydrocarbon radical With _{8 °} -C _1st molecular weight of the product is 1500 g and contains 3.25% nitrogen.

Example 6. To 128 g (0.1 mol of polybutene-hydroxybeneyl-diethylenetriamine), add 6 0 g '(0.3 mol) -2,6 of ditretbutylphenol and 12 g (0.3 mol) of formaldehyde and the reaction is carried out as described in example 1.

The resulting compound has a molecular weight of 1860 and contains 2.3% nitrogen.

Data on the effectiveness of the additive obtained by the interaction of polybutene-hydroxy-benzylpolyamine. with phenol derivative and formaldehyde are given in the table.

Testing the washing potential is carried out according to GOST 10734-64, thermal oxides. Stability according to GOST 9352-60.

All additives are added to the oil MS-20 in an amount of 1.5 wt.%. .

As can be seen from the table, the obtained additives have good detergent-dispersing and antioxidant properties, while the known additives have thermal oxidative stability (TOC) at the oil level.

In addition, the additives obtained retain a high cleaning potential at elevated temperatures of 300. 35.y? .С ,. which makes it possible to use them when the engine is operating at elevated temperatures.

Additive Detergent potential at temperature ° s Thermooxidize linen stability min 250 300 350 Polybutenoxy-benzenetetraethylene pentamine (by a known method) 80 70 thirty 25 Following the example 1 95 85 65 90 2 90 80 60 75 3 90 90 fifty 60 4 90 80 90 60 Polybutenoxy-benzylthiourea (by a known method) ⁷⁰ 60 thirty 35 Following the example 5 95 90 70 75 6 85 80 60 80 Oil 'MS-20 10 0 0 22-24

Claims (1)

Claim A method for producing an additive to lubricants by reacting a phenol derivative with polyamine and formaldehyde at elevated temperature, characterized in that, in order to increase the detergent-dispersing and antioxidant properties of the additive, polybutene-hydroxybenzylpolyamine of the general formula is used HE Y0y-CH ₂ -MN-AN, where K is the hydrocarbon radical ^C 60 ~ ^C KM, X A = (- CH ₂ -CH ₂ -MH-) _P , n = 2-4. ”Or (-C-ΝH-) X = oxygen or sulfur, and as a phenol derivative, a compound of the general formula is used wherein & ₂ , K ₂ , K ₄ is hydrogen or alkyl _; C--C ₄ or an amino group or hydroxy group, one of the radicals being hydrogen and a phenol derivative molecule containing 1-2 oxy groups and one amino group, the process is carried out with a polybutene-hydroxy-benzyl polyamine molar ratio: derivative phenol: formaldehyde equal to 1: 1-4: 1-4.