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The method of obtaining serosoderjaschei additives

IPC classes for russian patent The method of obtaining serosoderjaschei additives (RU 2168536):
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(57) Abstract:

The invention relates to the field of synthesis of serosoderjaschei additives with enhanced extreme-pressure, anti-wear properties, high thermal and oxidative stability. The method consists in the interaction-olefin fraction WITH16-C28with sulfur at a temperature of 130-150°C for 3 h in the presence of 0.1-0.9 wt.% with respect to the olefin catalysts, which use mono-, or di-, or triethanolamine. The sulfur content in serosoderjaschei additives compared with the known method is increased by 9-12 wt.% and additives do not require additional purification from hydrogen sulfide, mercaptans, the used catalyst.

The present invention relates to the field of synthesis of serosoderjaschei additives with improved anti-wear properties, high thermal and oxidative stability.

These additives are used for the manufacture of lubricants, including applicable for operations in cold forming processes.

As additives used polysulfone olefins.

A method of obtaining polysulfonic olefins collaboration is nom, to obtain the adduct. Synthesized adduct is in contact simultaneously with halogenougljovodonika, a sulfur compound, for example, sulfide, hydrogen sulfide or polysulfide of an alkali metal and elemental sulfur in an aqueous or aqueous-alcoholic medium. The mixture is heated and after stratification separating the organic layer containing polysulfonyl olefin, which can be processed by the Foundation. The resulting olefins containing significant amounts of sulfur, have a sufficient viscosity and solubility in mineral and synthetic oils. They are used as high pressure additives in lubricating oils for gears and processing of metals [1. Application France N 2563231, class C 10 M 135/04, 1985] .

A significant disadvantage of this method is a multi-stage and the presence of significant amounts of sewage and industrial wastes.

A method of obtaining polysulfone compositions with high sulfur content and low content of chlorine [2. The application of EPO N 0293299, class C 10 M 135/04, 1988].

The specified composition obtained by reaction of mono - or sulfur dichloride with at least one C2-C12-monoolefins with the formation of the adduct, which is then con the SUB>4-aliphatic alcohol, with the possible addition of elemental sulfur and a halogenated hydrocarbon.

The mixture is heated, the alcohol is distilled with the addition of water and after decantation and separation of the aqueous layer are organic layer containing the main amount polysulfonamide olefins.

The main disadvantage of this method is the presence of large amounts of waste, sewage, and gas emissions.

A method of obtaining structuresa additive interaction-olefin fraction C16- C18with elemental sulfur and hydrogen sulfide at a ratio of initial components 1:1, 5:0.5 and a temperature of 171oC. Sulfurized - olefins contain 20.6 percent sulfur [3. International application PCT (WO) N 88/02771, class C 10 M 135/02, 141/08, 1987].

The disadvantages of this method are:
1. Use as a reagent and catalyst highly toxic hydrogen sulfide, which requires special conditions for safe conduct of the process.

2. Education in the presence of hydrogen sulphide mercaptans, giving received structuresa insertion tool hard to carry the scent.

3. The need for removal of hydrogen sulfide and mercaptans formed from the received seurusteleva amount of gas emissions, containing hydrogen sulfide and mercaptans.

The closest in technical essence and the obtained results is the way to obtain sulfonated ethylene hydrocarbons by the interaction of sulfur with olefins in solution aminoalcohols at elevated temperatures [4. EP 0714971 A1, 28.11.1994,, CL C 10 M 135/04].

In the interaction of low molecular weight olefin of isobutylene with sulfur in the solution aminoalcohols, for example, monoethanolamine, the sulfur content in the resulting insertion tool is from 43 to 65 wt.%. However, when the transition to more high molecular weight of the olefin - Dicyclopentadiene sulfur insertion tool does not exceed 19,3 wt.% (see example 10 prototype).

The disadvantages of this method are:
1. The use of large quantities of initiator, the reaction of mono-, diethanolamine or research: 1 mol of isobutylene supplied from 1,78 up 3,81 mol of amerosport.

2. The need for cleaning structuresa additives from an excess of initiator.

3. Education in the cleaning process large amounts of sewage and waste - waste aminoalcohols.

4. The low sulfur content in structuresa insertion tool based on more high molecular weight olefin-titilope is To do this in the way of getting structuresa additive interaction-olefin fraction C16-C28with S8at elevated temperatures the reaction is carried out without hydrogen sulfide, but in the presence of catalytic amounts of mono-, or di-or triethanolamine. Using as catalyst a mono-, or di-, or triethanolamine allows the reaction of interaction of sulfur with a-olefins at a lower temperature of 130 - 150oC without toxic hydrogen sulfide with getting serosoderjaschei additives with a sulfur content of 29 to 33 wt.%.

Synthesized sulfur-containing additives without any further processing and extraction of catalyst can be used to produce a variety of lubricants, including for cold massive forming of metals.

The method is as follows.

In temperature-controlled reactor, equipped with an efficient stirrer, a refrigerator and a thermometer, load-olefins fraction C16-C28, 0.1 to 0.9 wt.% in relation to-olefins catalyst, mono-, or di-, or triethanolamine, and the temperature was raised to 130oC. When the temperature reached 130oC in the reactor serves powdered, or liquid sulfur. Next, the temperature was raised to 140 - 150oC for 3 hours to carry out the synthesis zerocode what tion.

The method is illustrated by the following examples.

Example 1. In thermostated glass reactor, equipped with an efficient stirrer, thermometer, reflux condenser, download 700 g-olefin fraction C16-C18, 0.7 g of monoethanolamine and the temperature was raised to 130oC. for 1 hour in the reactor serves 300 g of powdered sulfur, then increase the temperature to 150oC for 3 hours to carry out the reaction of interaction of sulfur with a-olefins. The reaction mass is then cooled to 40oC and separated from neprevyshenie sulfur filtration. Received 998,5 g additives with a sulfur content of 29.8 wt.%.

Example 2. Charged to the reactor 650 g-olefin fraction C16-C18, 1.3 g of monoethanolamine and the temperature was raised to 130oC. for 1 hour in the reactor serves 350 g of sulfur, then the temperature was raised to 150oC for 3 hours to carry out the reaction of interaction of sulfur with a-olefins. After cooling the reaction mass to 40oC and filtering the resulting 980,2 g additives with a sulfur content of 32.9 wt.%.

Example 3 carried out analogously to example 1, but is used as raw material-olefins fraction C16-C28and as a catalyst of 0.5 wt.% diethanolamine on-olefins. Powe catalyst using a 0.3 wt.% triethanolamine on the source-olefins. Received 981 g additives with a sulfur content of 33 wt.%.

Example 5 is carried out analogously to example 3, but as the catalyst use is 0.7 wt.% triethanolamine taken on-olefins. Received 995 g additives with a sulfur content of 29.5 wt.%.

Example 6 is carried out as example 2, but as the catalyst used to 0.9 wt.% triethanolamine taken on-olefins. Received 985 additives with a sulfur content of 33 wt.%.

Thus the proposed method for structuresa additives compared with the prototype has the following advantages:
1. The reaction of interaction with the olefin fraction C16-C28carried out in the presence of catalytic amounts of mono-, di-, triethanolamine.

2. The sulfur content in structuresa insertion tool derived from high molecular weight olefins, more than 10 wt.% the prototype.

3. The method is distinguished by the single-stage process and the simplicity of the technology.

4. In the process do not generate waste water and waste products.

5. The obtained additive does not require additional purification from the used catalyst.

The method of obtaining serosoderjaschei additives through the interaction of a-olefins WITH16-C28with gray when tempto the catalyst is used in an amount of 0.1 - 0.9 wt.% with respect to the olefin.

 

 

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