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The method of obtaining serosoderjaschei additives

The method of obtaining serosoderjaschei additives
IPC classes for russian patent The method of obtaining serosoderjaschei additives (RU 2181137):
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(57) Abstract:

The invention relates to the synthesis of serosoderjaschei additives with enhanced extreme-pressure, anti-wear properties, high thermal and oxidative stability. The method consists in the interaction of olefins fraction16-C26or Dicyclopentadiene with grey at 130-150oC for 6 h in the presence of 0.5-5 wt.% in relation to the raw material of the catalyst, which is used as dialkyldithiophosphate zinc formula I, where R is ISO-C3H7or ISO-C4H9; R' - n-C12H25or ISO-C9H19. The sulfur content in serosoderjaschei additives compared with the known method is increased by 10-11 wt.%, and received the additives do not require additional cleaning of the used catalyst.

The invention relates to the field of additive synthesis with enhanced extreme-pressure, anti-wear properties, high thermal and oxidative stability.

These additives are used for the manufacture of lubricants used in metal processing, and transmission oils.

A method of obtaining polysulfonic about the room, typically, isobutylene, to obtain the adduct. Synthesized adduct is in contact simultaneously with halogenougljovodonika, a sulfur compound, such as 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 metal processing. /Application France 2563231, CL 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 structuresa additive interaction-olefin fraction WITH16-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% sulfur /international application PCT (WO) 88/02771, CL 10 M 135/02, 141/08, 1987/.

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 structuresa additives in order to give the latter the desired organoleptic properties.

4. The presence of significant quantities of gaseous emissions containing hydrogen sulfide and mercaptans.

Closest to the claimed invention is a method for xerostomia additive interaction of the ethylene hydrocarbons such as isobutylene with elemental sulfur in the presence of aminoalcohols or research at an elevated pressure and a temperature of 130oC /EP 0714971, 05.06.96,, CL 10 M 135/04/.

At 1,285 mol of isobutylene serves 2,3-4.9 mol of monoethanolamine, 2-7 mol of sulfur. The sulfur content in the ready insertion tool is 40-65 wt.%. In the case of use as a feedstock heavier Dicyclopentadiene content of sulfur in the resulting reaction product does not exceed 19,3 wt.% (example 10).

The disadvantages of this method are:
1. The use of large isback is esperta.

2. The need for cleaning structuresa additives from the initiator. The obtained additive extracted from the reaction mixture with n-heptane, the extract solution is washed with 10% soda and water. At the final stage n-heptane is separated from additives by distillation under vacuum.

All these operations complicate the process and lead to the formation of significant amounts of sewage and waste - waste aminoalcohols.

3. Sulfated isobutylene with high sulfur content due to the low flash point of less than 100oWith can't be used for cold forming processes by which the metal surface is achieved, the temperature of 500-550oWith, and the sulfurized isobutylene will evaporate and contaminate the environment. In addition, they have an unpleasant odor, which is also unacceptable for additive technology lubricants. Therefore, to obtain serosoderjaschei additive technology grease as feedstock use fractions of olefinic hydrocarbons above C12H24.

The problem to which the alleged invention is directed, is to simplify the process technology.

To solve pointed to by the about dicyclopentane with sulfur at elevated temperature 130-150oWith carried out in the presence of catalytic amounts (0.5 to 5 wt.% for raw materials) dialkyldithiophosphate zinc formula
< / BR>
where R is ISO-C3H7or ISO-C4H9; R' - n-C12H25or ISO-C9H19.

The content of sulfur in the insertion tool is 30-35 wt.%. Synthesized sulfur-containing additives without any further processing and extraction of catalyst can be used to produce a variety of lubricants and gear oils.

The method is as follows.

In temperature-controlled reactor, equipped with an efficient stirrer, a refrigerator, a thermometer, download olefins fraction16-C26or Dicyclopentadiene and 0.5-5 wt. % relative to the initial raw material, the catalyst - dialkyldithiophosphate zinc formula
< / BR>
where R is ISO-C3H7or ISO-C4H9;
R' - n-C12H25or ISO-C9H19.

The temperature was raised to 140 to 150oWith and within 6 hours carry out the synthesis structuresa additives. The reaction mass is then cooled to 40oWith and separate neprevyshenie sulfur filtering.

The method is illustrated by the following examples.16-C18and 0.5 wt.% (2.5 g) dialkyldithiophosphate zinc as a catalyst having the formula
< / BR>
The temperature in the reactor was raised to 130oWith and serves 220 g of powdered sulfur for 1 h Then the temperature was raised to 150oC for 6 h carry out the reaction of interaction of sulfur with olefins. The reaction mass is then cooled to 40oWith and separated from neprevyshenie sulfur filtration. Received 711 g of additive containing to 30.1 wt.% sulphur.

Example 2 carried out analogously to example 1, but the catalyst serves to 1 wt.% of raw materials; the quantity of sulfur is 240 was Obtained 719,8 g additives with a sulfur content of 32.1 wt.%.

Example 3 carried out analogously to example 1, but the catalyst serves 2 wt.% of raw materials; the quantity of sulfur is 250 was Obtained 721,4 g additives with a sulfur content of 33 wt.%.

Example 4 is carried out analogously to example 1, but the catalyst serves 4 wt.% of raw materials; the quantity of sulfur is 260, the Received 729,8 g additives with a sulfur content is 34.9 wt.%.

Example 5 is carried out analogously to example 4, but the catalyst serves 5 wt.% for raw materials. Received 730,1 g additives with a sulfur content of 35.1 wt.%.

Example 6 the BR>
in the amount of 4 wt.% of raw materials; the quantity of sulfur 260, Received 730,2 g additives with a sulfur content of 34.7 wt.%.

Example 7 is carried out analogously to example 4, but is used as raw material Dicyclopentadiene and the reaction is carried out at a pressure of 7 ATA. Received 728,7 g additives with a sulfur content of 30.4 wt.%.

Example 8 is carried out analogously to example 6, but used as raw material Dicyclopentadiene and the reaction is carried out at a pressure of 7 ATA. Received 731,1 g additives with a sulfur content to 30.1 wt.%.

Example 9 is carried out analogously to example 6, but is used as raw material olefin fraction WITH16-C26. Received 731,1 g additives with a sulfur content to 30.1 wt.%.

Thus, the proposed method for structuresa additives compared with the prototype has the following advantages:
1. The reaction of interaction of olefins WITH16-C26, Dicyclopentadiene is carried out in the presence of catalytic amounts of 0.5-5 wt.% dialkyldithiophosphate zinc formula
< / BR>
where R is ISO-C3H7or ISO-C4H9;
R' - n-C12H25or ISO-C9H19,
instead of aminoalcohols or research, the supply of which is up to 200% on selected referatories 19,3% (example 10).

3. The process is not formed wastewater and waste.

4. The obtained additive does not require additional purification from the used catalyst, which generally simplifies the process of its receipt.

The invention can find application in the production of serosoderjaschei additives for industrial lubricants used in metal processing, as well as for the manufacture of transmission oils.

The method of obtaining serosoderjaschei additives by reacting olefins WITH16-C26or Dicyclopentadiene with grey at 130-150oIn the presence of a catalyst, wherein the catalyst used dialkyldithiophosphate zinc formula
< / BR>
where R is ISO-C3H7or ISO-C4H9;
R' - n-C12H25or ISO-C9H19,
in the amount of 0.5-5 wt.% for raw materials.

 

 

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