The method of preparation of the catalyst and the method for the agent reducing the hydrodynamic resistance on the basis of polyacene obtained using this catalyst

 

The invention relates to methods for macromolecular higher poly-alpha-olefins, in particular polyacene, and catalysts for carrying out the method. High molecular weight higher poly-alpha-olefins are used in various fields, in particular as agents of reducing the hydrodynamic resistance during movement of hydrocarbon liquids, for example, pumping of oil by pipeline. The invention solves the problem of simplification of the method of preparation of the catalyst and increase the activity of the catalyst, and the problem of increasing molecular weight poly alpha olefin obtained at elevated temperature polymerization. The proposed method includes a step for magnesium-containing media, followed by the interaction of the carrier with titanium tetrachloride and alkylaromatic ether, with a magnesium-containing carrier get in two stages, where in the first stage interact metal magnesium with an aromatic halide in the presence of a simple ester with formation of a suspension containing solution magyarkanizsa connection and a solid phase, and the second stage carry out the sequential interaction of the resulting suspension with alkoxide licencie esters. The polymerization of 1-hexene is carried out at a temperature from 0 to 50S. 2 S. and 2 C.p. f-crystals, 2 tab.

The invention relates to methods for macromolecular higher poly-alpha-olefins, in particular polyacene, and catalysts for this process. High molecular weight higher poly-alpha-olefins are used in various fields, in particular, as agents of reducing the hydrodynamic resistance during movement of hydrocarbon liquids, for example, during transfer of oil through the pipeline.

A method of obtaining agents of reducing the hydrodynamic resistance (SDS) of hydrocarbon liquids by polymerization of higher alphaolefins using aluminothermic catalyst il31/3ll3and alyuminiiorganicheskikh of socializaton of diethylacetanilide (GEAH) for 31 hours (U.S. Patent No. 3692676, C 08 F 6/12, 1972). The yield of the target product is 88%, decreased hydrodynamic resistance of oil - 12% when the concentration of the agent 5 ppm (parts per million). The disadvantages of this method are the low value of reducing the hydrodynamic resistance, long curing times and low activity is imerissia higher alphaolefins with the number of carbon atoms from 6 to 10 in the environment of the hydrocarbon solvent in the presence of a catalyst, obtained by reduction of titanium tetrachloride alyuminiiorganicheskikh connection, and alyuminiiorganicheskikh of socializaton (RF Patent No. 2075485, C 08 F 10/14, 1997). This catalyst has a higher activity compared with aluminothermic catalyst and allows at a temperature of from -30 to 20With (mostly when 0C) for 5 h to achieve the conversion of 1-hexene 58-70%. In this way we obtain a high molecular weight polymers with a characteristic viscosity []=1.2 to 1.7 m3/kg, which reduce SDS heptane at 30-58% at a polymer concentration of 2 ppm. The disadvantages of this method are the low activity of the catalyst, the necessity of using low temperatures (0(C) during polymerization and relatively low molecular weight of the obtained polymer.

A method of obtaining higher poly-alpha-olefins using a catalyst system consisting of applied titanomagnievoe catalyst containing titanium tetrachloride on the media - magnesium chloride and stereoregular donor additive (e.g., dibutyl phthalate) and socializaton, representing a mixture of trialkylsilyl activity compared to catalysts based on il3and is widely used to obtain polypropylene and copolymers of propylene with alphaolefins. A number of cooking methods applied titanomagnievyj catalysts are described, for example, in the book by E. P. Moore (Jr.), Polypropylene Handbook. Hansen Publishers, 1996.

The closest in technical essence and the achieved result is a method using a catalyst obtained in three stages (RF Patent No. 2152404, C 08 F 4/64, 10.07.2000).

Stage (a). The contacting metallic magnesium with an aromatic halide RX, in which R is an aromatic group containing from 6 to 20 carbon atoms, X is a halogen atom. The result is a suspension that contains the solution magyarkanizsa compounds and solid by-product consisting mainly of magnesium chloride. The solution magyarkanizsa connection is separated from the solid by-product and used in the next stage (b).

Stage (b). Introduction silicon compound containing alkoxygroup or alloctype, the solution magyarkanizsa compounds at a temperature of from -20 to 20With the formation of a solid product, which is used in the subsequent stage (s) in contact with the titanium tetrachloride and alkylaromatics especial getting polypropylene powder with a small amount of fine fraction, that is a major advantage when obtaining polypropylene in modern industrial processes in the liquid monomer in the gas phase. The catalyst provides a much higher output at higher polymerization of olefins as compared with a catalyst based on il3. The disadvantage of this method of preparation of the catalyst is the presence of significant amounts of solid waste in the first stage of preparation of the catalyst. The need to separate these wastes complicates the technology of preparation of the catalyst.

The invention solves the problem of simplification of the method of preparation of the catalyst and increase the activity of the catalyst, and the problem of increasing the molecular weight of polyacene obtained at elevated temperature curing.

The problem is solved through the use of a catalyst, which is prepared in three stages as follows.

Stage (a). The contacting metallic magnesium with an aromatic halide RX similar to the method described in the prototype (Patent RF №2152404, C 08 F 4/64, 10.07.2000). You get a suspension (product (I) containing solution magyarkanizsa connection and a solid phase, and then use this suspension without separation R is Oh in stage (a) and containing a solution of magyarkanizsa connection and a solid phase, add first connection of the silicon-containing alkoxygroup, and then further electron-donating organic compound (alcohol, cyclic, or a simple ester) with the formation of the magnesium-containing solid carrier product II.

The interaction of magnesium-containing product II with titanium tetrachloride and alkylaromatic ether to obtain the final catalyst [stage (C)] performed similarly well-known solution.

In addition to simplifying the technology of preparation of the catalyst and reduce the amount of waste at the stage of (a) a further advantage of the catalyst compared to the prototype is a higher activity, which is achieved through the use of electron-donating compounds in the second stage of the synthesis of magnesium-containing solid product II.

Stage (a) in the process of preparation of the catalyst according to the invention is carried out by contacting metallic magnesium with an aromatic halide, which is used as chlorobenzene, bramasol and iadanza, preferably chlorobenzene. You can also use a combination of two or more of aromatic halides. Magnesium and aromatic halide is brought into contact with each other in the presence of inertness or aromatic solvents, containing 4-10 carbon atoms. Examples of ethers are diethyl ether, diisopropyl ether, disutility ether, dietarily ether, dellroy ether, tetrahydrofuran (THF) and anisole.

The reaction temperature in stage (a) is usually from 20 to 150With, mainly from 90 to 110; Time of interaction ranges from 2 to 20 hours, mostly 4-8 PM

After the completion of stage (a) receive a suspension (product II), consisting of sediment, representing mainly of magnesium dichloride, and the solution magyarkanizsa connection structure of Mg3PhnClm(n=3.5 to 4.5; m=1.5 to 2.5). This product is used for the subsequent stage (b).

At the stage (b) the suspension obtained in stage (a) is brought into contact with alkoxysilanes compound of silicon and electron-donating compound. This is carried out by adding to a suspension of the product I first silicon compound containing alkoxygroup or alloctype at a temperature of from -20 to 20With, and then subsequent addition of electron-donor compound at a temperature of from 0 to 20C, extracts of the reaction medium at a temperature of from 20 to 70EDINENIE silicon, contains alkoxygroup or alloctype, is used as a compound of General formula R1nSi(OR2)4-nwhere R1and R2is a hydrocarbon group containing from 1 to 6 carbon atoms, n=0-2. Preferably using tetraethoxysilane.

As the electron-donating compound at the stage (b) use alcohols ROH, where R is a hydrocarbon group containing from 2 to 8 carbon atoms, and cyclic ethers. Examples of cyclic ethers include: a furan, tetrahydrofuran and derivatives thereof. Mostly use tetrahydrofuran.

The molar ratio between silicon and magnesium in stage (b) can vary from 0.2 to 20, preferably from 0.2 to 1. The molar ratio between the electron-donating compound and magnesium at the stage (b) can vary from 0.5 to 5, preferably from 1 to 3.

Formed in stage (b) the product II is then used for the preparation of the catalyst in stage (C). The preparation of the catalyst is conducted by contacting stage (s) of product II obtained in stage (b) with titanium tetrachloride and alkylaromatic ether.

High-molecular-weight polyhexes possessing properties agent reducing the hydrodynamic resistance, get the of telesfora. As socializaton use trialkyl aluminum, for example triethylaluminium or triisobutylaluminum. The polymerization process is carried out at a temperature from 0 to 50C, preferably at 10-30C.

In the polymerization of olefins in the reaction medium usually impose additional electron-donating compound, which increases stereoregular the ability of the catalyst. As such compounds may be used alkoxy(alkyl)containing the silicon compound of the structure R1nSi(OR2)4-nwhere R1and R2is a hydrocarbon group containing from 1 to 6 carbon atoms, n=1-2.

Prepared according to the proposed method, the catalyst suitable for the polymerization of olefins such as ethylene, propylene, butylene, hexene, octene, the mission dodecen. This catalyst is particularly suitable for the polymerization of 1-hexene.

The polymerization is carried out mainly in the liquid phase in the presence of a hydrocarbon solvent such as hexane, heptane, octane, cyclohexane. benzene, toluene or xylene. The polymerization temperature is 0 to 50C. Important technological advantage of the catalyst is in what anoniem high molecular weight polymer.

Using the proposed method provides the high yield of high-molecular polyctena in the temperature range from 10 to 30C. While the resulting polymers have characteristic viscosity [] 1.7 to 0.7 m3/kg and have properties agent reducing the hydrodynamic resistance (SDS) when the movement of hydrocarbons. In particular, it ensures the reduction of SDS on 50-20% at a polymer concentration of 2 ppm.

Hydrodynamic testing of agents on the capillary turboramjet in a solution of n-heptane. Capillary length and inner diameter equal to 0.8 m and 1.110-3m respectively. The concentration of the agent SDS in each of the tests is 2 ppm. Reducing SDS is determined by the formula:

where0- the expiration time of the pure solvent, C;

- the expiration time of the polymer solution, C.

The present invention will be further explained using examples that do not limit the invention.

Example 1

Preparation of catalyst

Stage (a). In a three-neck flask equipped with a reverse howat 1 h at 80And then add a mixture of 173 ml dibutylamino ether and 80 ml of chlorobenzene. Then the reaction mixture was added 0.03 g of iodine and 3 ml of chloride n-butane. After the disappearance of the iodine staining raise the temperature of the mixture up to 97With and slowly add 250 ml of chlorobenzene for 2.5 hours the reaction mixture is intensively stirred for 8 h at 97C. the result is a suspension (product (I) containing solution magyarkanizsa connection (MOS) structure MD3RH4CL2and a solid phase containing MgCl2in the ratio of Mg3Ph4Cl2/MgCl2=2:l.

Stage (b). The suspension obtained in stage (a), (100 ml, 0.25 mol Mg), loaded into the reactor. The reactor is cooled to 0C and for 2 h add a mixture of 22 ml of tetraethoxysilane (TES) and 38 ml of heptane under stirring.

Then the reaction mixture was kept at 0With another 0.5 h under vigorous stirring dosed for 1 h in a mixture of 14.6 ml of ethanol (0.25 mol) and 45.4 ml of heptane. Then increase the temperature of the reaction mixture to 70C and maintained at this temperature for 2 hours then paramasivam. The solid is washed with heptane (4 x 250 ml). Get 25,2 g magnesium-containing solid product (II), suspended in 100 ml of heptane.

Stage (C). The reactor is rinsed with nitrogen and load it consistently mixture of 150 ml of titanium tetrachloride and 150 ml of chlorobenzene and 12 g of product (III) in 48 ml of heptane. The reaction mixture is heated with stirring to 115With, give it a 7.2 ml of dibutyl phthalate and maintained at 115C for 1 h After mixing is stopped and the solid product is allowed to settle.

The liquid above the precipitate is removed by decantation, and then add a mixture of 150 ml of titanium tetrachloride and 150 ml of chlorobenzene. The reaction mixture is again heated to 115C and stirred for 30 min, then the solid product is allowed to settle for 30 minutes This last cycle was repeated once more. The obtained solid is washed 5 times using 300 ml of heptane at 60C. Get the catalyst, suspended in heptane. The titanium content in the catalyst of 1.9 wt.%.

Polymerization

In the reactor of 1 l load at a temperature of 20With 150 ml of heptane and 5 ml of a solution of threesoms) and 62 ml (0.5 mol) of 1-hexene, which corresponds to the concentration of 1-hexene in the reactor of 2.5 mol/l and 0,0144 g of catalyst. The polymerization is carried out at a temperature of 20C for 1 h, the Polymer is discharged, add 20 ml of isopropanol and 20 ml of stabilizer ANOX in acetone with a concentration of 1 g/l Polymer is dried to constant weight. The output polyacene is 1.0 kg/g cat.; conversion of 1-hexene is 46%. The characteristic viscosity of the polymer [] dened in gasoline at 20With, is 1.3 m3/kg, the effect of reducing the hydrodynamic resistance (DR) is 39%.

Example 2

The catalyst was prepared as described in example 1 except that in stage (b) use of 21.9 ml of ethanol (0,375 mol, the molar ratio of ethanol : Mg=1.5) and 38,1 ml of heptane.

Polymerization of 1-hexene carried out analogously to example 1, but using 0,0121 g of catalyst. The output polyacene is 1.1 kg/g cat.; conversion of hexene-1 - 46%. Characteristic viscosity of polyacene is 1.6 m3/kg, and the value of DR=50%.

Example 3

The catalyst was prepared as described in example 1 except that in stage (b) use 43,8 ml of ethanol (0.75 mol, the molar ratio of ethanol:Mg=3) and 16.2 ml of heptane is polyhexes the characteristic viscosity of 1.41 m3/kg, and the value of DR=46%.

Example A (comparative)

Preparation of catalyst

Stage (a). In a three-neck flask, equipped with reflux condenser and addition funnel, load 26 g of magnesium powder (1.07 mol). The flask is rinsed with nitrogen. Magnesium is heated 1 h at 80And then add a mixture of 173 ml dibutylamino ether and 80 ml of chlorobenzene. Then the reaction mixture was added 0.03 g of iodine and 3 ml of chloride n-butane. After the disappearance of the iodine staining raise the temperature of the mixture up to 97With and slowly add 250 ml of chlorobenzene for 2.5 hours the reaction mixture is intensively stirred for 8 h at 97C. Then, the stirring and heating is stopped and the solid material give be deposited within 48 hours After desantirovaniya solution above the precipitate isolated solution (MOS) having a concentration of 1 g-al Mg/L. This solution is used for carrying out stage (b).

Stage (b). The solution of reaction product 1 (100 ml, 1 mol/l) are metered into the reactor. The reactor is cooled to 0C and for 2 h add a mixture of 11.2 ml of tetraethoxysilane (TES) and 38 ml dibutylamino ether with stirring.

After �https://img.russianpatents.com/chr/176.gif">C. Then the reaction mixture was kept at 60C for 1 h, then stirring and heating stopped and the solid product is allowed to settle for 30 minutes, the Liquid above the precipitate is removed by decantation. The solid is washed 4 times using 150 ml of heptane. Obtain 13.5 g of light yellow solid, suspended in 40 ml of heptane.

Stage (C) preparation of the catalyst carried out analogously to example 1. Polymerization of 1-hexene carried out analogously to example 1, but using 0.015 g of catalyst. Get 7.5 g of polyacene. The output is 0.50 kg/g cat., the characteristic viscosity of the polymer 1,25 kg/m3the value of DR=37%.

The example In (comparative)

Stage (a) is carried out analogously to example 1. Stage (b) is conducted as described in example 1, except that at this stage do not use ethanol and after the addition of tetraethoxysilane and exposure at 0°C for 0.5 h hold temperature rise to 70With further preparation carried out analogously to example 1.

Stage (C) and polymerization of 1-hexene carried out analogously to example 1. The output polyctena 0,55 kg/g cat; characteristic viscosity of polyacene 1.2 m3/kg, the values of the deposits (1 mol), 169, 5mm ml dibutylamino ether (1 mol) and 370 ml of chlorobenzene. The result is a suspension containing solution MOS composition of Mg3Ph4Cl2and a solid phase containing MgCl2.

Stage (b). The suspension obtained in stage (a) (100 ml, 0.2 mol Mg), loaded into the reactor and added under stirring to 40 ml of heptane. The reactor is cooled to -15C and for 1 h add a mixture of 17.9 ml of tetraethoxysilane (TES, of 0.08 mol) and 42.4 ml of heptane under stirring. Then the reaction mixture was kept at -15With another 0.5 h and then for 1 h to increase the temperature to 60C. Then the reaction mixture was kept at 60C for 1 h, cooled to a temperature of 20C and at this temperature with vigorous stirring dosed for 1 h in a mixture of 3.7 ml of etilbenzene (0,026 mol) and 26.3 ml of heptane. Then aged 0.5 h and dosed for 2 h in a mixture of 5.8 ml of ethanol (0.1 mol) and 54,2 ml of heptane. Then increase the temperature within 1 h to 70C and maintained at 70C for 2 hours After mixing and heating stopped and the solid product is allowed to settle. Liquid on sieges is containing a series of product (II), suspended in 100 ml of heptane.

Stage (C) and the polymerization of 1-hexene carried out analogously to example 1. The output polyacene is 0.65 kg/g cat. Characteristic viscosity of polyacene 1.3 m3/kg, the value of DR=34%

Example 5

Stage (a) is conducted as described in example 4.

Stage (b) is conducted as described in example 4, except that after cooling the reaction mixture to 20Since it is dosed with vigorous stirring for 3 h the mixture of 7.8 ml of 2-ethylhexanol (2-EH, 0.05 m), and 8.8 ml of ethanol (0,15 mol) and 73.4 ml of heptane. Then increase the temperature within 1 h to 70C and maintained at 70C for 2 hours After mixing and heating stopped and the solid product is allowed to settle. The liquid above the precipitate is removed by decantation. The solid is washed 4 times using 250 ml of heptane. Get the magnesium-containing product II, suspended in 100 ml of heptane.

Stage (C) and the polymerization of 1-hexene carried out analogously to example 1. The output polyacene is 0.72 kg/g cat. Characteristic viscosity of polyacene 1.4 m3/kg, the value of DR=49%.

Example 6

Stage (a) and phase (b) is conducted as described in example 5 for the l of heptane.

Stage (C) and polymerization of 1-hexene carried out analogously to example 1. The output polyacene is 1.0 kg/g cat. Characteristic viscosity of polyacene 1,24 m3/kg, the value of DR=34%.

Example 7

Stage (a) is conducted as described in example 4.

Stage (b) is conducted as described in example 4, except that after cooling the reaction mixture to 20Since it is dosed with vigorous stirring for 1 h the mixture of 5.8 ml of ethanol (0,1 mole) and 24.2 ml of heptane, allowed to stand for 1 h and then further dosed for 1 h in a mixture of 8.1 ml of tetrahydrofuran (0,1 mole) and 21.9 ml of heptane. Then raise the temperature within 1 h to 60C and maintained under stirring for 2 hours After mixing and heating stopped and the solid product is allowed to settle. The liquid above the precipitate is removed by decantation. The solid is washed 4 times using 250 ml of heptane. Get the magnesium-containing product (II), suspended in 100 ml of heptane.

Stage (C) is conducted as described in example 1. Polymerization of 1-hexene carried out analogously to example 1. The output polyacene is 0.74 kg/g cat. Characteristic viscosity of polyacene 1.30 m3/kg, the value of DR=39%.

Example 8

In example 1, except that instead of propyltrimethoxysilane as part of socializaton use propyltrichlorosilane. The output polyacene is 0.9 kg/g cat. Characteristic viscosity of polyacene 1,62 m3/kg, the value of DR=48%.

Example 9

The preparation of the catalyst were carried out as described in example 2. Polymerization of 1-hexene is carried out in the conditions of example 2, except that the polymerization time is 2 hours Output polyacene is 1.4 kg/g cat, conversion of hexene - 1-53%. Characteristic viscosity of polyacene []=1,41 m3/kg; value of d=46%.

Example 10

Using the catalyst prepared according to example 1. Polymerization of 1-hexene is carried out in the conditions of example 9, but as socializaton use triethylaluminium (tea). The output polyctena in these conditions is 1.1 kg/g cat.: conversion of 1-hexene reaches 30%. The characteristic viscosity of the polymer of 0.95 m3/kg, the value of DR=27%.

Example 11

Using the catalyst prepared according to example 1. Polymerization of 1-hexene is carried out in the conditions of example 10, but at the temperature of polymerization 30With and hanging catalyst 0,0086, the polymer Yield is 3.1 kg/g cat., the type field is p>Using the catalyst prepared according to example 1. Polymerization of 1-hexene is carried out in the conditions of example 10, but at the temperature of polymerization 11C. the polymer Yield is 0.9 kg/g cat. Received polyhexes has a characteristic viscosity of 0.97 m3/kg, the value of DR=26%.

As seen from the above examples and tables 1, 2, the present invention can simplify the method of preparation of the catalyst, thus obtained catalyst has higher compared with the known catalysts activity. The use of the catalyst according to the proposed method in the process of polymerization of hexene-1 leads to increased molecular weight received polyctena and increasing the temperature of polymerization. We then obtain polyhexes provides reducing hydrodynamic resistance to 50-20% at a concentration of 2 ppm polymer in comparison with the known agents.

Claims

1. The method of preparation of a catalyst to obtain high-molecular polyctena possessing properties agent reducing the hydrodynamic resistance, comprising a step for magnesium-containing carrier, the subsequent interaction but the spruce receive in two stages, where in the first stage interact metal magnesium with an aromatic halide in the presence of a simple ester with formation of a suspension containing solution magyarkanizsa connection and a solid phase, and the second stage carry out the sequential interaction of the resulting suspension with alkoxysilanes silicon and then electron-donating compound, which is used as alcohols, simple and cyclic ethers.

2. The method according to p. 1, characterized in that as the electron-donating compound in the second stage using the alcohol ROH, where R is a hydrocarbon group containing 2-8 carbon atoms, and cyclic ethers.

3. The method according to any of paragraphs.1 and 2, characterized in that the molar ratio between the electron-donating compound and the magnesium is 1-3.

4. A method of obtaining a high-molecular polyctena possessing properties agent reducing the hydrodynamic resistance, by the polymerization of 1-hexene in the presence of a catalytic system comprising a solid component containing titanium tetrachloride, magnesium-containing carrier and electron-donating compound and socialization consisting of trialkylamine and electrondonating trichosis fact, the polymerization process is carried out at a temperature of 0-50C.

 

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