A method of obtaining a linear medium-density polyethylene

 

(57) Abstract:

The invention can be used in the production of plastics. Linear medium-density polyethylene produced by polymerization of ethylene in the gas phase in the presence of a catalyst and alyuminiiorganicheskikh of socializaton. The catalyst is a deposited on an inorganic carrier, titanium tetrachloride by magnesium dichloride and Zirconia-alyuminiiorganicheskikh connection - product of the interaction of zirconium tetrachloride with the diene and triisobutylaluminum. The catalyst further includes fixed on an inorganic carrier, the product of the interaction of Nickel dichloride with a diene, triisobutylaluminum and acceptor additive or without it. This additional component allows you to adjust the melt flow index and alter other properties of the polyethylene without reducing the yield of product per unit of catalyst. table 2.

The invention relates to the production of plastics.

A method of obtaining linear medium-density polyethylene (LPAS) polymerization of ethylene in the environment of a solvent in the presence of a catalyst based on titanium tetrachloride and tetraethoxysilane on the media and triisobutyl what I complicates the process. The yield does not exceed 3 kg PASP per 1 g of titanium.

Closest to the invention to the technical essence and the achieved result is a method of obtaining PASP polymerization of ethylene in gaseous form in the presence of hydrogen, alyuminiiorganicheskikh of socializaton and a catalyst comprising a deposited on an inorganic carrier, titanium tetrachloride, fixed on the magnesium dichloride, zirconium-alyuminiiorganicheskikh connection (Caos), obtained by the interaction of 1 mol. hours of zirconium tetrachloride with 3 to 6 mol. hours of diene selected from the group comprising butadiene, isoprene and Allen, and 3 to 6 mol. H. CHIBA (SU, patent 2001042, class C 08 F 110/02, 1993).

The technical problem of the invention is the development of highly efficient single-stage (without the introduction of co monomer) of the process of obtaining LPAS with adjustable melt flow index (MFR5) when the possibility of introducing hydrogen to 30% vol. without reducing the yield of product per unit of catalyst, and ensuring the variation of other properties LPAS that can be achieved by changing the ratio between oligomerization and polimerizuet components of the catalyst.

This technical result is achieved by the fact that str is the catalyst and catalyst, representing deposited on an inorganic carrier, titanium tetrachloride, fixed on the magnesium dichloride, and CEOS obtained by the interaction with 3 - 6 mol. H. CHIBA, using a catalyst, optionally including the application of inorganic carrier, Nickel-alyuminiiorganicheskikh connection (NAOS), obtained by the interaction of 1 mol. including dichloride Nickel with 4 mol. hours of diene and 3 - 6 mol. H. CHIBA or 1 mol. including dichloride Nickel with 4 mol. hours of diene, 3 - 6 mol. H. CHIBA and 3 to 8 mol. h acceptor additives selected from the group comprising titanium tetrachloride, sesquiterpenoid and complex trichloride aluminum with an aromatic hydrocarbon, when used as diene, butadiene, isoprene or Allen, and the resulting atomic relations Zirconia:titanium 0,2 - 3,0, titanium, magnesium 0,01 - 0,10, titanium, Nickel and 0.2 to 3.0, the concentration of titanium on inorganic media 0.1 - 2.0 wt.% on 100 wt.% media, and the process is carried out at an atomic ratio of aluminum in socializaton:titanium 50 - 500.

The essence of the invention consists in that the catalyst consists of polymersomes titanium-zirconium bearing component and oligomerizes Nickel component.

As the inorganic carrier is used, napora - alyuminiiorganicheskikh connection, for example, diethylaluminium (DEHA).

The NAOS is produced by interaction of Nickel dichloride with diene and CHIBA in the environment of the solvent. For example, in the solution with a stirrer download 0.65 g of dehydrated Nickel dichloride (0,005 mol), 48 ml 32 ml hexane mixture (isopentane-isoprene mixture with the concentration of isoprene of 0.95 mol/l) containing 0.03 mol of isoprene, and 20 ml CHIBA in hexane (0.015 mol). After stirring at 30oC for 4 h are the solution of the SPLA in the form oligoaniline Nickel-aluminum complex with a concentration of 0.05 mol NAOS/L.

CEOS get patent SU 2001042. For example, in a reactor with a stirrer load of 1.5 g of zirconium tetrachloride (0,0064 mol), 61,6 ml of hexane, 40,4 ml of a mixture having the above composition and containing of 0.038 mol of isoprene, and 26 ml CHIBA in hexane (0,0192 mol). Get the solution Caos as oligoaniline zirconium-aluminum complex with a concentration of 0.05 mole Caos/L.

The titanium tetrachloride attached to the magnesium chloride receive, for example, the interaction of titanium tetrachloride with freshly prepared magnesium dichloride. Charged to the reactor 9.6 g of metallic magnesium, 100 ml of heptane, 0.1 g of iodine and 130 ml of butyl chloride. After paramapoonya heptane, add 7 ml of titanium tetrachloride and stirred at 70oC for one hour. The concentration of titanium in suspension 0,046 g/L. the Atomic ratio of titanium, magnesium 0,1.

Polimerizuet component of catalyst prepared as in patent SU 2001042. For example, a suspension of SiO2(0,58 g) in hexane is mixed with a suspension (1.31 ml) of titanium tetrachloride (610-5mol), attached to the magnesium chloride in hexane. The concentration of titanium in suspension 0,046 g-a/l Add cos (310-5mol). The atomic ratio of zirconium:titanium 0,5.

Oligomerize component of the catalyst receive, for example, by mixing a suspension of SiO2(1,15 g) in hexane with 3.6 ml NAOS (1,810-4mol).

Oligomerize component of the catalyst was prepared with the use of acceptor additives, for example, a suspension of SiO2(1,46 g) in hexane is treated with a solution of 4.1 ml) NAOS (2,010-4mol). In the resulting suspension is added 2.5 ml (1,010-3mol) of titanium tetrachloride. The molar ratio of the NAOS:acceptor additive 1:5.

The process of preparation of the catalyst involves the stages of mixing and drying of components to obtain a homogeneous free flowing powder.

The polymerization is carried out in the reactor for gas polymerizatio in the reactor support through the contact of monometr, associated with the solenoid valve. The reactor is pre-rinsed pure ethylene.

The invention is illustrated by examples 1 to 13, in examples 3, 5, 6, 12 as acceptor additives used set of toluene with trichloride aluminum, for example 4 - sesquiterpenoid, in examples 7 to 11 - titanium tetrachloride. The conditions of polymerization and properties LPAS are shown in tables 1 and 2, where C5- isoprene, C4- butadiene and C3- Allen. The density of the resulting polyethylene is within 0,940 - 0,945.

A method of obtaining a linear medium-density polyethylene by polymerization of ethylene in the gas phase in the presence of hydrogen, alyuminiiorganicheskikh of socializaton and a catalyst comprising a deposited on an inorganic carrier, titanium tetrachloride, fixed on the magnesium dichloride, zirconium-alyuminiiorganicheskikh compound obtained by the interaction of 1 mol.h. of zirconium tetrachloride with 3 to 6 mol.h. the diene selected from the group comprising butadiene, isoprene and Allen, and from 3 to 6 mol.h. triisobutylaluminum, wherein the used catalyst, optionally including deposited on an inorganic carrier, Nickel-alyuminiiorganicheskikh connection, polucheniya Nickel with 4 mol.h. diene, 3 - 6 mol. hours of triisobutylaluminum and 3 to 8 mol.h. acceptor additives selected from the group comprising titanium tetrachloride, sesquiterpenoid and complex trichloride aluminum with an aromatic hydrocarbon, when used as diene, butadiene, isoprene or Allen, and the resulting atomic relations Zirconia : titanium 0,2 - 3,0, titanium, magnesium 0,01 - 0,10, titanium, Nickel and 0.2 to 3.0, the concentration of titanium on inorganic media 0.1 - 2.0 wt.% on 100 wt. % of the medium and the process is carried out at an atomic ratio of aluminum in socializaton : titanium 50 - 500.

 

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