SU887622A1 - Method of mineral oil deparaffinization - Google Patents

Description

(54) METHOD FOR DEPARAPHINIZATION OF MINERAL

12

The invention relates to the field of refining, in particular to the method of dewaxing mineral oils.

The increase in the production of low-hardening (winter and all-season) mineral oils and the share of paraffin oils involved in the processing led to the fact that the dewaxing process in the general scheme of the production of lubricating oils is steadily increasing.

The deparaffinization of the oils is carried out using various solvents 1.

One of the main parameters that determine the solvent dewaxing performance is the filtration rate, which depends on the size, shape and structure of the paraffin crystals formed when the dewaxed oil solution is cooled.

Small crystals very quickly clog the filter cloth, which requires frequent stopping and washing of the filters. Large crystals contribute to the formation of poorly washed mass with a high content of oil.

One way to increase the efficiency of the dewaxing process, which does not require large capital expenditures, is to use dewaxing additives that increase the speed of the oil filter.

and increase the oil yield due to changes in the size, shape and structure of paraffin crystals.

There are known methods for dewaxing oils with solvents using various dewaxing additives, which are condensation products of chlorine paraffin and naphthalene (paraflou), copolymers of ethylene, olefins, polymerethycrylates 2.

The closest to the described technical result and achieved results is the method of dewaxing mineral oils by mixing

15 raw materials with a solvent, followed by heat treatment, cooling the mixture and filtering, separating dewaxed oils and paraffins. The process is carried out using a mixture of oil-soluble polymer products A and B 3 as a dewaxing additive.

Product A is a copolymer of at least two olefins, or a mixture of a polymer and a copolymer with an average molecular weight of 2000-60000. Product A is obtained by polymerization or copolymerization of α-mo oolefins of Cu- € 24 - in the presence of Ziegler-Natta catalnzato / Zs in a hydrocarbon solvent in the atmosphere

30 nitrogen.

Product B is polymers or copolymers of n-alkyl methacrylates with an Cyu-C24 alkyl chain having an average molecular weight of 15,000-200,000.

Products A and B are introduced into the oil separately or as a concentrate with a content of 5-60 May. % of both products.

Introduction of 0.05-OD May. % of the mixture of A and B (50/50) in the residual oil improves the relative filtration rate by 2 times and increases the yield of dewaxed oil by 0.2-0.6 May. %

The disadvantages of this dewaxing method are not high enough filtration rate and a slight increase. Examination of the dewaxed oil output. In addition, the additive used in this method is obtained by a multistep and complex technology, and as a raw material, difficult-to-reach and expensive higher a-olefins are used, which are currently used in industry in small quantities, and in many important areas where they are an indispensable raw material.

The aim of the invention is to increase the filtration rate and oil yield.

The goal is achieved by the fact that in the method of dewaxing mineral oils by mixing the raw material with a solvent in the presence of a dewaxed, her additive with subsequent heat treatment, cooling the mixture and filtering to release dewaxed oils and paraffins, the product of thermal destruction of ethylene-propylene is used as a dewaxing additive. a copolymer (SKEP-R) having a molecular

mass 2000-7000, in the amount of 6.05-0.5 May. % The product of thermal degradation of the copolymer has the following composition, mol. %: propylene 36-50, ethylene 64-50.

The additive is obtained as follows. Ethylene is copolymerized with propylene ;; liquid propylene on Ziegler-Natta catalysts at temperatures from + 10 to -10 ° C, ethylene content in

the liquid phase 4-7 mol. % and the ratio of the components of the catalytic system AI / V 3: 1 -10: 1, the resulting copolymer with mol. mass from 100,000 to 1,000,000. Then, the high molecular weight copolymer is thermally degraded at 340-380 ° C and a residual pressure of 20-80 mm Hg. Art. within 5-30 minutes The result is a product with a molecular weight of 2009-- 7000, containing 36-50 mol. % propylene and 64-50 mol. % of ethylene, which is used as a dewaxing additive, is added to the oil in an amount of 0.05-0.5 May. %

Dewaxing is subjected to distillate and residual raffinate of paraffinic oils with characteristics (for comparison, the properties of the dewaxed oil of the prototype are attached) shown in Table. one.

Table 1

Indicators

Density, Viscosity at 100 ° C, eats Flash temperatures, ° C Pour point, ° C Paraffin content, May.

Deparates and oil raffinates are conducted as follows. The raffinate is mixed with a dewaxed additive with a solvent, then, after heat treatment, the mixture is cooled to filtration temperature and filtered under vacuum to obtain paraffins (on the filter) and a solution of de-aaraffinated oil, which is then separated from the solvent.

The distillation raffinate dewaxing is carried out in a mixture of selective solvents acetone: toluene 40: 60, taken in an amount of 350% relative to the raffinate at -25 ° C, and the residual solvent in a mixture of selective solvents acetone:

: toluene 30 70, taken in an amount of 400% at -25 ° C. These modes provide for the production of oils with a pour point of -15 ° C and high yield. The invention is illustrated by the following.

examples.

Example 1. The required amount of destructed copolymer of ethylene with propylene with a content of 42 mol. A 2000% molecular weight propylene was added at 60 ° C to the distillate raffinate, then after dilution with a solvent, heat treated and cooled to -25 ° C, filtered under vacuum. The concentration of degraded ethylene propyl: a new copolymer is 0.05; 0.15; 0.5 May. % of raw materials.

Example 2. The dewaxing was carried out analogously to example 1, but a degraded ethylene-propylene copolymer with MM 4300 was taken. The copolymer concentration was 0.05; 0.15; 0.5 May. % of raw materials.

Example 3. The dewaxing was carried out analogously to example 1, but a degraded ethylene-propylene copolymer with MM 6000 was taken. The concentration of the copolymer was 0.05; 0.1; 0.15; 0.20; 0.25; 0.30; 0.50 May. %

Example 4. Dbaraphenization proceeded analogously to example 1, but taking the co-Example 7. The required amount of a destructed copolymer of ethylene with propylene 1C O01 held “iOr lene 36 mol. % and MM 2000 are added at 60 ° C to the residual raffinate, then, after dilution with a solvent, thermally treated and cooled to -25 ° C, filtered under vacuum. The copolymer concentration is 0.05; 0.10; 0.15; 0.5 May. % of raw materials.

Example 8. The dewaxing is carried out analogously to example 7, but taking z; a structural copolymer with MM 4300. The copolymer concentration is 0.05; 0.10; 0.15; 0.5 May. % of raw materials.

Lime with MM 7000. Copolymer concentration 0.05; 0.15; 0.5 May. % of raw materials.

Example 5. The dewaxing is carried out analogously to example 1, but a degraded ethylene-propylene copolymer with MM 6000 and a propylene content of 36 mol. % The final concentration of the copolymer is 0.05; 0.15; 0.5 May. % of raw materials.

EXAMPLE 6: Dewaxing is carried out analogously to Example 1, but taking a degraded ethylene-propylene copolymer with 6000 mm containing 50 mol. % propylene. The copolymer concentration is 0.05; 0.15; 0.5 May. % of raw materials.

The results of distillation raffinate dewaxing according to examples 1-6 are presented in table. 2

table 2

Example 9. The dewaxing was carried out analogously to example 7, but a degraded copolymer with MM 6000 was taken. The co-grace of the copolymer was 0.05; 0.10;

0.15; 0.20; 0.25; 0.30; 0.50 May. % of raw materials.

Example 10. The dewaxing is carried out analogously to example 7, but a degraded copolymer with MM 7000 is taken.

about 1 ce of copolymer is 0.05;

0.10; 0.15, 0.5 May. % of sysh.

30 Example 11. The deparapisation procedure is carried out analogously to example 7, but a degraded ethylene-propylene copolymer with MM 6000, containing 42 mol. %

propylene The concentration of the CO copolymer is 0.05; 0,010; 0.15; 0.5 May. %

Example .12. The dewaxing is carried out analogously to example 7, but taking the degraded ethylene-propylene copolymer with MM 6000 and the content of the oil dewaxing method according to the invention allows, due to the additive used, to increase the relative filtration rate by 2.5-3.5 times (in the prototype 2 times), the yield the depot-araffined oil increases from 3.9 to 8.1 May. % (in the prototype 0.2 May.%).

one

The advantages of the dewaxing process according to the invention also lie in the fact that the depar used (ripylene 50 mol.%). The copolymer concentration is 0.05; 0.10; 0.15 and 0.5 wt.% Of the raw material.

The results of the dewaxing of the residual raffinate in examples 7-12 are given in table. 3

Table 3

The additive is obtained on the basis of cheap and readily available monomers using simple technology that makes it easy to adjust the process parameters.

The resulting additive is uniform in composition and dissolves well in oil.

Claims (3)

1. Goldberg D. O. et al. “Lubricating oils from the oils of the eastern fields. M., “Himi, 1972, p. 112-113. 2. "The study of polymer additives to increase the efficiency of the process of dewaxing oils," Chemistry and technology of fuels and oils, 1978, № 1, 21-24. 3. US patent No. 3806442, CL. 208-33, published. 1974 (prototype).