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USEFUL ADDITIVES FOR PETROL AND OTHER MOTOR FUELS
INVENTION
Patent of the Russian Federation RU2262514

METHOD OF OBTAINING POLYMER ADDITIVES FOR DIESEL FUELS AND LUBRICATING OILS

METHOD OF OBTAINING POLYMER ADDITIVES TO DIESEL FUELS
AND LUBRICANT OILS

The name of the inventor: Martirosyan AG (RU); Musaev Kamran Musa oglu (AZ)
The name of the patent holder: Artur G. Martirosyan
Address for correspondence: 117279, Moscow, ul. Profsoyuznaya, 93, building 4, ap. 389, A.G. Martirosyanu
Date of commencement of the patent: 2003.12.30

The invention relates to the field of petrochemistry, in particular to a process for the preparation of polymer additives for diesel fuels and lubricating oils. Summary of the invention consists in that the raw material in the form of a crushed synthetic rubber containing a copolymer of ethylene with propylene is heated throughout the volume gradientlessly to a depolymerization temperature in a reactor containing a rotor apparatus. The resulting depolymerizate is withdrawn and maintained at a depolymerization temperature in an inert gas atmosphere, while the EPDM rubber or EPDM is used as the raw material, from which the raw material is first taken and the molecular weight composition and the optical density of the raw material are determined at a wavelength of 810, 1150 and 4310 cm- 1 , then the value of the ratio a / v · s is calculated, where a is the optical density of the feed at 810 cm -1 , c is the optical density of the feed at 1150 cm -1 , c is the optical density of the feed at 4310 cm -1, and a feedstock having The value of the ratio is not more than 1.5. The raw material is fed in an inert gas atmosphere. The temperature of the depolymerization is set by the number of revolutions of the rotor apparatus, depending on the molecular weight composition of the raw material and the type of additive obtained. The method makes it possible to obtain the desired product with the reproducibility of the physicochemical parameters and the qualitative characteristics required by the industry.

DESCRIPTION OF THE INVENTION

The invention relates to the field of petrochemistry and can be used for the preparation of polymeric additives of various functional purposes, in particular depressant additives for diesel fuels and viscous additives for motor lubricating oils.

A method is known for producing ethylene-propylene copolymers in a continuous mode by heating high-molecular rubber by dissociation of mechanical energy in rubber and its thermal destruction under conditions of shear strain in which intensive shear deformation is performed at shear rates of 2500-5000 s -1 (RF patent No. 2162473, 27.01.2001).

In carrying out the process, ethylene-propylene copolymers are produced over a wide range of molecular weights. As the starting rubber, both the serial rubber and the sub-standard rubber containing the crosslinked moieties can be used. In accordance with this method, three-zone treatment of the polymer material in the reactor is carried out. In the first zone rubber is heated by means of a compression screw, in the second one, direct destruction is carried out due to the shear rate established by means of the gap between the rotor and the stator, in the third, rubber is discharged through the adjustable spinneret. The molecular weight of the desired product is controlled by changing the shear rate and residence time in the destruction zone. However, the process does not concern the production of ethylene-propylene copolymers of a predetermined molecular weight range for a particular application, for example as depressant additives for fuels and oils, or as a viscous additive for motor lubricating oils.

It is known to produce low molecular weight polyolefins by thermal destruction of high molecular weight polyolefins at a depolymerization temperature of 320-370 ° C. in two stages in which the first stage of thermal degradation is carried out by heating as a high molecular weight polyolefin elastomer rubber EPDM ethylene copolymer with propylene and diene throughout Volume without gradient to the depolymerization temperature in a time of 1 to 6 minutes, the resulting depolymerization in the second stage is withdrawn and maintained at the depolymerization temperature for 15-30 minutes, both steps are carried out under an inert gas atmosphere, the final product being a depressant additive to diesel fuels with a mole .m. 800-3000 or viscous additive to lubricating oils with a mol. 8000-100000 (RF patent No. 2171816, published on August 10, 2001). Thermal decomposition is carried out in a reactor having a heating and depolymerization section and a depolymerization holding section. The heating and depolymerization section is equipped with a rotary device with a variable speed set inside the section.

It should be noted that when the final products are obtained by this method, the reproducibility of the physicochemical parameters of the final products is not achieved, but also the magnitude of the qualitative characteristics of these products, for example, the amount of depression required by industry.

The invention is based on the task of creating a method for producing polymeric additives for diesel fuels and lubricating oils that would allow the production of final products with the reproducibility of the physicochemical parameters and the quality characteristics required by the industry by using raw materials with a certain composition of components and specific molecular weights and molecularly Mass distribution (MMD) of the components in it.

The object is achieved in that in a process for the preparation of polymer additives, comprising feeding to a reactor containing a rotary apparatus for heating and thermal degradation of raw materials, ground synthetic rubber containing an ethylene-propylene copolymer in an inert gas atmosphere, heating the raw material to a depolymerization temperature, and withdrawing Followed by keeping the depolymerizer obtained at a depolymerization temperature in an inert gas atmosphere, the depolymerization temperature being realized by a rotor with a variable speed, the raw material being a EPDM rubber containing a copolymer of ethylene with propylene or a EPDM containing a copolymer of ethylene with propylene and a diene, Feeding the raw material portion, determining the molecular weight composition and the optical densities of the feed at a wavelength of 810, 1150 and 4310 cm -1 , then calculating the value of the ratio a / v · s, where a is the optical density of the feed at 810 cm -1 , The optical density of the feed at 1150 cm -1 , c is the optical density of the feedstock at 4310 cm -1 , and raw materials having a ratio of not more than 1.5 are used.

It is expedient to use as raw material a rubber containing a diene in an amount of not more than 1.6% by weight. Of the total mass of raw materials.

It is also advisable that vinylidenorbornene is included in the composition of the raw material as a diene.

Best Mode for Carrying Out the Invention

According to the invention, the process is carried out as follows. From a batch of raw materials, synthetic rubber containing a copolymer of ethylene with propylene and a diene, EPDM rubber (T), a batch is taken and the molecular weight composition is determined by a known method, for example, gel chromatography, and optical densities at a wavelength of 810, 1150 and 4310 Cm -1 , by a known method, for example, IR spectroscopy. For certain values, the value of the ratio a / c · s is calculated, where a is the optical density of the raw material at a wavelength of 810 cm -1 , c is the optical density of the raw material at a wavelength of 1150 cm -1 , c is the optical density of the raw material at a wavelength of 4310 cm- 1 , and the raw material is used, for which the calculated ratio is not more than 1.5. It can be used raw materials with a diene content of not more than 1.6, but also raw materials, in which the diene is vinylidene norbornene.

A known tubular reactor described in the above-mentioned RF patent No. 21171816, op. 10.08.2001. The reactor has a section for heating and depolymerization, inside which is installed a rotary apparatus with a variable speed. The depolymerization temperature is set by the number of revolutions of the rotor apparatus, which is determined from tables compiled on the basis of theoretical and experimental studies, depending on the molecular weight composition of the feed and the type of additive obtained, characterized by its own molecular weight.

Raw material is crushed on a mechanical crusher to obtain pellets 3-5 mm in size. The resulting granules are loaded into a feed hopper under a nitrogen atmosphere and from there are fed to the reactor under a nitrogen atmosphere. The granules delivered to the reactor due to the intensive shear deformation created by the rotational speed of the rotor apparatus, are heated to the depolymerization temperature gradientlessly and are destructured in all of its volume with the formation of depolymerizate. The resulting depolymerizate is removed and maintained at a depolymerization temperature until the molecular weight characteristics are stabilized.

Examples of a particular embodiment of the method.

Example 1 . From a batch of raw materials, a rubber of the TEP of a T-high molecular weight polyolefin elastomer containing a copolymer of ethylene with propylene and diene-vinylidene norbornene, a batch is taken and its molecular weight composition is determined by a known gel-chromatography method, and optical densities at a wavelength of 810, 1150 and 4310 cm- 1 , known method of IR spectroscopy, and the value of the ratio a / v · s is calculated from them. The molecular weight of the selected portion was 600,000, the content of vinylidene norbornene was 1.2% by weight. The value of the ratio a / b · s was 1.4, which indicates the suitability of raw materials for the production of high-quality polymer additives with narrow molecular weight distribution and reproducibility of properties. The vinylindenorbornene content of 1.2% increases the probability of obtaining polymer additives of high quality with a narrow molecular weight distribution and reproducibility of properties. According to a priori data, the rotational speed of the rotor is determined and set. To obtain from this raw material a viscous additive to lubricating oils, the rotor apparatus of the reactor is set to a speed of 3500 s -1 . Then the raw material is crushed on a mechanical crusher to obtain pellets of 3-5 mm in size. The resulting granules are charged into a feed hopper under a nitrogen atmosphere and fed thereto in a nitrogen stream to the reactor. The reactor is maintained at a nitrogen atmosphere with a residual pressure of 30 mm Hg. The pellets received at the inlet of the reactor due to the intensive shear deformation created by the speed of rotation of the rotor apparatus are heated to a depolymerization temperature of 380 ° C and destructurized throughout its volume with the formation of depolymerizate. The resulting depolymerizate is selected and maintained at a depolymerization temperature of 380 ° C until the molecular weight characteristics are stabilized.

The characteristics of the depolymerizate obtained were analyzed by gel chromatography.

The depolymerizate obtained has: thickening ability - 170%, viscosity index - 55, pour point - 16 ° C, mol. Weight 2000, MMP-2. Such characteristics confirm the production of a product suitable for its characteristics as a viscous additive to lubricating oils.

Example 2 . Example 2 was performed similarly to Example 1 on the same reactor and from the same feed. The number of revolutions of the rotor apparatus was changed, the required rotational speed was set to obtain a depressant additive for diesel fuels of 3000 s -1 . The characteristics of the depolymerizate obtained were analyzed by gel-chromatography.

The depolymerizate obtained has: thickening power - 170%, depression index - 55, pour point - 16 ° C, mol. Weight 7000, MMP - 1.8. Such characteristics confirm the production of a product suitable for its characteristics as a depressant additive to diesel fuels.

Example 3 . Example 3 is carried out analogously to Example 1 on the same reactor. As a raw material, rubber is used. The value of a / b · s was 0.08, which indicates the suitability of raw materials for the production of high-quality polymer additives with narrow molecular weight distribution and reproducibility of properties.

The depolymerizate obtained has: thickening power - 170%, viscosity index - 50, pour point - 16 ° C, mol. Weight 5000, MMP - 1.8. Such characteristics confirm the production of a product suitable for its characteristics as a viscous additive to lubricating oils.

In the case of a "double" ethylene-propylene rubber, i.e. Rubber, the value of a / in · s is close to 0, because Is close to 0 optical density at a wavelength of 810 cm -1 due to minimization of double bonds. The stability of the reproducibility of the properties of the additives obtained, the achievement of a narrow molecular weight distribution are improved by minimizing the values ​​of the a / b · s ratio in the declared range.

The process is possible in the atmosphere of any inert medium, including an inert gas. In industrial processes, the traditional inert medium is nitrogen.

CLAIM

A process for the preparation of polymer additives comprising feeding to the reactor a rotary apparatus for heating and thermal degradation of the raw material, ground synthetic rubber in an inert gas atmosphere, heating the raw material to a depolymerization temperature and withdrawing, followed by maintaining the depolymerization obtained at a depolymerization temperature in an inert gas atmosphere, The temperature of the depolymerization is realized by a rotor apparatus with a variable speed, characterized in that a EPDM rubber containing a copolymer of ethylene with propylene or a EPDM containing a copolymer of ethylene with propylene and a diene is used as the raw material, a portion of raw material is taken before feeding, The mass composition and the optical densities of the raw material at a wavelength of 810 cm -1 , 1150 cm -1 and 4310 cm -1 , then the value of the ratio a / v · s is calculated, where a is the optical density of the feed at 810 cm -1 , Raw materials at 1150 cm -1 , s - the optical density of the raw material at 4310 cm -1 , and use raw materials having a ratio value of not more than 1.5.

2. A method according to claim 1, characterized in that a rubber containing a diene in an amount of not more than 1.6% of the total weight of the raw material is used as the raw material.

3. A process according to claim 1 or 2, characterized in that the composition of the raw material as a diene is vinylidene norbornene.

print version
Date of publication 07.04.2007gg