Method for preparing higher trialkyl aluminum

FIELD: chemistry of metalloorganic compounds, chemical technology.

SUBSTANCE: invention relates to the improved method for preparing higher organoaluminum compounds, namely, to trialkyl aluminum. Method is carried out by interaction of aluminum preliminary subjected for activation with triethyl aluminum, hydrogen and olefin or olefin hydrocarbons at increased temperature and pressure. Activation of aluminum is carried out by interaction of aluminum, triethyl aluminum and part of olefin or olefin hydrocarbon and kept at temperature 40-50°C followed by feeding hydrogen and by increasing temperature to 125-135°C, kept at this temperature for 0.5-2 h, the remained amount of olefin or olefin hydrocarbon is fed and kept the formed reaction mass at temperature 135-155°C for 5-10 h. method provides enhancing conversion of olefins in the process for synthesis of trialkyls aluminum that are used broadly in different branches of industry, in particular, in production of polyolefins, higher saturated alcohols and others.

EFFECT: improved preparing method.

2 cl, 5 ex

 

The invention relates to the production of higher alumoorganic compounds, specifically higher aluminization, which find wide application in various industries, in particular in the production of polyolefins, higher fatty alcohols, etc.

The highest aluminiumrail can be obtained in various ways, for example through haloalkyl (U.S. Patent No. 2848472, publ. 19.08.58; 2863894, publ. 09.12.58; 2957897, publ. 28.10.68 of Ministry, 2957898, publ. 25.10.68). This method has not found industrial application due to the high cost and difficulties of the process.

A method of obtaining hydrocarbon aluminum compounds by interaction ethylamine, α-olefin having at least three carbon molecules and final group H2C=CH-, and a catalyst selected from the group consisting of salts and oxides of metals of group VIII of the Periodic table and manganese, titanium, and copper (U.S. Patent No. 2962513, publ. 29.11.60). The molar ratio of catalyst: ethylaluminum withstand equal to 0.005 to 0.1:1. For full replacement of the ethylene from ethylaluminum and substitute it with alkylation, relevant α-olefin, the reaction mixture is heated to a temperature of 50-200°C. as the catalyst use Nickel sulfate, cobalt chloride, manganese chloride, iron oxide (III), Nickel oxide, and as a α-olefin-propylene, n-butene-1, n-penten-1, 3,3-dimethylpentan-1, 3,3-dimethylbutene-1, 4-methylpentene-1, 3,4-dimethylpentan-1, octene-1, 7-methyloctane-1, mission-1, nonen-1, dodecene-1, branched derivatives of these alkenes and other α-olefins obtained by cracking of paraffins having 16-18 carbon atoms.

The disadvantage of this method is the complexity of the technological process is associated with the need for preparation of the catalyst.

The most common in industry the process of obtaining alkylamine (U.S. Patent No. 5233103, IPC5C 07 C 27/00, publ. 3.08.93, France application No. 1251038, IPC C 08 F 10/00, publ. 15.01.61) reaction of escalating chain of triethylaluminum ethylene with obtaining compounds trialkylamine with the distribution of the lengths of the alkyl chains on the Poisson, for example, from 2 to 20 carbon atoms, with a maximum of approximately C8. The obtained intermediate alkylamine then reacts with the mixture α-olefins with higher average carbon number with the purpose of substitution of alkyl groups and receive alkylamine with a higher average length of alkyl chains. Typical thermal substitution reaction requires temperatures of about 340-375°and hold it in a closed system, so replaced with more light olefins remain in the system.

Since the substitution is an equilibrium reaction, the conversion of intermediate alkylamine in the SPS with a higher length of the alkyl chains is limited (˜ 80% mol.). When the excess olefin (350%) received alkylamine contains a significant number of alkyl groups With2and C4that is a shortcoming of the process.

The known process of obtaining trialkylamine method displacement (U.S. Patent No. 5278330 MPC C 07 F 5/06, publ. 11.01.94), including the interaction of (1) alkylamino raw material containing one or more alkylamine represented by the formula, R3Al, in which R represents premiani alkylation2-C20and R may be the same or different, with the average length of the chains, at least about C8and (2) raw materials linear α-olefins containing one or more linear α-olefins having a chain of at least 2 carbon atom more than alkerdeel alkylamino raw materials. The displacement reaction of olefins corresponding to R alkylamino raw materials, and replacing them with alkylsalicylate derived linear α-olefinic feedstock flows in the presence of a cobalt catalyst at a temperature of 50-150°and a pressure below atmospheric (5-100 mm Hg). Formed trialkylamine has a higher average length of alkyl chains than the original alkylamino raw materials. Substituted olefins are removed from the reaction mixture.

The disadvantage of this method is the necessity of cooking rolled atora, what complicates the technological process.

A method of obtaining organoaluminium connection interaction triisobutylaluminum, trioctylamine or product accession of ethylene to trialkylaluminium or olefin and powdered aluminum and hydrogen at a temperature of 80-200°and the pressure 60-350 ATM. The reaction product is diethyl - or dialkylaminomethyl (UK Patent No. 939824, IPC With 22 21/00, 07 F 5/06, publ. 16.10.63).

In the process of implementation of the described method are hydrides that you want to select and send to the next stage of the synthesis trialkylamine.

Known direct synthesis of aluminization activated alkaline or alkaline-earth metal aluminium, hydrogen and olefin at temperatures of 100-240V°and the pressure 35-240 ATM (U.S. Patent No. 3100786, publ. 13.08.63).

The method is intended primarily for triisobutylaluminum and diisobutylaluminum.

There is a method to simultaneously obtain trialkylamine and hydrides alkylamine by the interaction of aluminum with olefins and hydrogen in the presence of monofunctional dialkylamide. Pre-exercise activation of aluminium by trialkylaluminium when the ratio trialkylaluminium: aluminum, equal to 10:1 (Germany Application No. 1031792, IPC 07 F 5/06, publ. 12.06.58).

The disadvantage of which is the need for additional phase synthesis of monofunctional dialkylamide.

In the described synthesis process trialkylamine using aluminum metal there is a General problem is de-activated aluminum, which offers a variety of ways, for example, including the stage of processing of aluminum powder activating agents containing halogen (U.S. Patent 3000919, publ. 19.09.61), or the use of special alloys of aluminum with other metals (Patents France No. 1153017, IPC 07 F 5/06, publ. 28.02.58; 1155598, IPC 07 F 5/06, publ. 06.05.58; 1247893, IPC 07 F 5/06, publ. 02.12.60).

To improve the activity of the aluminum used in the direct synthesis of aluminization proposed mechanical grinding on fibromalgia, granulation of molten aluminum in a stream of inert gas or the activated powdered aluminum small additions of metals of group IV and V ("Chemical industry", №9, 645, 1962; №3, 178, 1963; №1, 24, 1962; №2, 97, 1963).

The known method of connection alkylamine produced by the interaction of a component selected from the group consisting of aluminium and aluminium-containing alloys, with a component consisting of a mixture of alkylamine and hydrogen or a mixture alkylamine, hydrogen and olefin (U.S. Patent No. 3402190, publ. 17.09.68). Alkylamine has the General formula RR'AlR"', where R and R', respectively, which are selected from alterationof with 2-20 carbon atoms, R"' the choice is up from the group, composed of alterationof with 2-20 carbon atoms and hydrogen atoms. The reaction is carried out in the presence of an activator having the General formula RnMY, where R" is selected from the group consisting of alkoxy, araxi, Alcoxy, helcaraxe, alkylaryl, aralkyl and alkaryl radicals; Y is selected from the group consisting of alkoxy, araxi, Alcoxy, helcaraxe radicals; M is a metal selected from the group consisting of sodium, lithium, potassium, magnesium, and n is 0 when M is sodium, potassium or lithium, and is 1 if M is magnesium.

The disadvantage of the process is the use of additional chemical compounds - activator, including oxyradical, which requires special care.

Closest to the present invention is a method of obtaining alkylamine compounds (Patent USSR No. 404263, IPC 08 F 5/06, publ. 26.10.73). The described method is that the alloy of aluminum with silicon is subjected to interaction with alkylamine compound and hydrogen or with hydrogen, alkylamine compound and the olefin when heated to 50-200°under pressure, mainly 10-300 kg/cm2. Applied olefins contain from 2 to 20 carbon atoms. Pre-carry out mechanical or chemical activating the source of aluminium alloy. As the activating metal compound m which can be used aluminum hydride, sodium hydride, chloride diethylamine, chloride diisobutylaluminum, triethylaluminium, triisobutylaluminum etc. Alkylamino connection, which may be, for example, triethylamine, hydrogen and olefin served in the lower or middle part of the reactor filled with the alloy. Metal residue can be squeezed out through the sieve from the top of the reactor feed alkylamino compounds and hydrogen, then it is separated from alyuminiiorganicheskikh connection. The target product is formed due to the interaction of aluminum, olefin and hydrogen in the presence of triethylamine, which is the starting material in this reaction.

The disadvantage of this method is that for synthesis use the original trialkylaluminium and an olefin having the same number of carbon atoms in the chain. For higher trialkylamine, for example, with the number of carbon atoms C5-C20, it is first necessary to synthesize the original higher trialkylaluminium that requires greater consumption of the starting components.

Object of the invention is the simplification of the method of obtaining the highest aluminization to increase the conversion of olefinic hydrocarbons in the process of obtaining the target product.

The problem is solved by providing a method of obtaining highest aluminization by the interaction of Aktivera the data aluminium-containing reagent, triethylaluminum, hydrogen and olefin or olefin hydrocarbons at elevated temperature and pressure, thus activating expose the aluminum in the process of interaction of aluminum, triethylaluminum and part of the olefin or olefin hydrocarbons and maintained at a temperature of 40-50°C for 5-30 minutes, then begin to apply hydrogen, increasing the temperature up to 125-135 mA°C, kept at this temperature for 0.5-2 hours, then serve the remaining amount of olefin or olefin hydrocarbons formed and maintained the reaction mass at a temperature of 135-155°C for 5-10 hours.

On activating the aluminum serves 2,5-7,0% of the mass. olefin or olefin hydrocarbons of the stoichiometric amount.

The difference of the invention from the closest is that the activation of aluminum is carried out by interaction of aluminum, triethylaluminum and 2,5-7,0% of the mass. olefin or olefin hydrocarbons of the stoichiometric amount and is maintained at a temperature of 40-50°C for 5-30 minutes, then begin to apply hydrogen, increasing the temperature up to 125-135 mA°C, kept at this temperature for 0.5-2 hours, then served the rest of the stoichiometric amount of olefin or olefin hydrocarbons and stand formed of reactions is nnow mass at a temperature of 135-155° C for 5-10 hours.

The activation of aluminium by the proposed method eliminates the possibility of decontamination, in addition, eliminating the need for separate additional stage activated aluminum and achieve a high conversion of the initial olefin or olefin hydrocarbons in the target trialkylaluminium.

In the process of obtaining the highest aluminization can be used, for example, aluminum powder, corresponding to the requirements of normative-technical documentation THE 1791-99-019-98 or THE 48-5-230-82.

As olefinic hydrocarbons may be used any of olefinic hydrocarbons With6-C20for example, the fraction of 1-hexene (TU 2411-059-05766801-96), the fraction of alpha-olefins of C8C10C8-C10(THE 2411-057-05766801-96), the fraction of alpha-olefins With12-C14(THE 2411-058-05766801-96), the fraction of alpha-olefins of C16-C18(THE 2411-067-05766801-96), the fraction of alpha-olefins With18-C20with different alpha-olefins With18and C20and others.

The method of obtaining the highest aluminization is as follows.

In the batch reactor, the, equipped with a mixing device and a device for supplying coolant serves aluminium, triethylaluminium and 2,5-7,0% of the mass. of the stoichiometric amount of olefin or olefin hydrocarbons With 6-C20, maintained at a temperature of 40-50°C for 5-30 min with constant stirring, after which start the flow of hydrogen into the reactor until a pressure of 25-35 kg/cm2while increasing the temperature up to 125-135 mA°C. the Reaction mass is kept in these conditions for 0.5-2 hours.

Then, the reactor serves the remainder of the stoichiometric amount of olefin or olefin hydrocarbons With6-C20increase the pressure up to 35-55 kg/cm2and maintain the reaction mass at a temperature of 135-155°C for 5-10 hours.

After this time the reaction mass is then cooled, reducing the pressure, and incubated for 2-5 hours. Received the highest aluminiumrail unloaded from the reactor.

Implementation of the proposed method to obtain the highest aluminization illustrate the examples below.

Example 1

The highest aluminiumrail get in a laboratory setup in a batch reactor, the equipped with a magnetic stirrer and an outer jacket coolant. Before loading the reagents into the reactor creates an inert atmosphere.

Charged to the reactor to 18.7 g of triethylaluminum, 8,9 g of aluminum and 9.3 g of the fraction of olefins, C18-C20containing 98.4% of the mass. C18olefins and 1.6% of the mass. With20olefins that faced the t of 2.5% of the mass. from its stoichiometric amount. Used fraction contains 96,03% of the mass. alpha-olefins, 1,96% of the mass. olefins with internal double bonds, 1,41% of the mass. vinylidene and 0.6% of the mass. paraffin hydrocarbons.

The mixture was kept at a temperature of 50°C for 30 min with constant stirring, and then begin feeding hydrogen to a pressure of 35 kgf/cm2while increasing the temperature to 135°C. In such conditions, the reaction mass was kept for 2 hours.

Then, the reactor serves the remainder of the stoichiometric quantity (363,8 g) fraction of olefins, C18-C20. The temperature was raised to 155°C, pressure up to 48 kgf/cm2and maintain the reaction mass in these conditions for 10 hours.

Upon completion of the reaction, reduce the temperature to 100°C, pressure up to 2 kgf/cm2can withstand 3 hours and unload the reaction mass from the reactor.

The resulting product contains 89,1% of the mass. trioctadecyl and 1.4% of the mass. triacetyluridine. Conversion of olefins is 93,8%.

Example 2

The highest aluminiumrail get in an industrial unit in a batch reactor, the equipped with a stirrer and an internal coil coolant. Before loading the reagents into the reactor creates an inert atmosphere.

Charged to the reactor 980 kg Treaty is aluminum, 464 kg of aluminum and 464 kg fraction of 1-hexene (TU 2411-059-05766801-96)containing 95.6% of the mass. hexene-1, 0.3% of the mass. hexane, 2.8% by mass. vinylidene and 1.3% of the mass. hydrocarbons with an internal double bond which is 6.75% of the mass. from its stoichiometric amount.

The mixture was kept at a temperature of 40°C for 5 min with constant stirring, and then begin feeding hydrogen to a pressure of 25 kgf/cm2while raising the temperature to 125°C. In such conditions actionnow to withstand the weight for 0.5 hours.

Then, the reactor serves the remainder of the stoichiometric quantity (6407 kg) fraction of 1-hexene. The temperature was raised to 130°C, pressure up to 30 kgf/cm2and maintain the reaction mass in such conditions for a period of 7.5 hours.

Upon completion of the reaction, reduce the temperature to 70°C, pressure up to 1 kgf/cm2can withstand 2 hours and unload the reaction mass from the reactor. The resulting product contains 86,9% of the mass. tridecylamine. Conversion of olefins is a 94.6%.

Example 3

The highest aluminiumrail get the same as described in example 2. In the reactor load 750 kg of triethylaluminum, 356 kg of aluminum and 356 kg faction mission-1 (TU 2411-057-05766801-96)containing 96.7% of the mass. the mission-1, 0.4% of the mass. paraffin, 1.8% by mass. vinylidene and 1.1% of the mass. hydrocarbons with an internal double bond, representing 4.3% of the mass. about the its stoichiometric amount, maintained at a temperature of 50°C for 15 minutes and Then the temperature was raised to 135°C, pressure up to 32 kgf/cm2by feeding into the reactor with hydrogen. The reaction mass is kept in these conditions for 2 hours.

Then, the reactor serves 7954 kg faction mission-1. The temperature was raised to 148°C, pressure up to 55 kgf/cm2and maintain the reaction mass in these conditions for 5 hours.

Upon completion of the reaction, reduce the temperature to 85°C, pressure up to 1.5 kgf/cm2can withstand 2 hours and unload the reaction mass from the reactor.

The resulting product contains 85.9% of the mass. tridecylamine. Conversion of olefins is of 91.3%.

Example 4

The highest aluminiumrail get in the same way as described in example 1.

Charged to the reactor 13,52 g triethylaluminum, to 6.43 g of aluminum and 7 g of fraction olefins C16-C18containing 61.7% of mass. C16olefins and 38.3% of the mass. C18olefins, which is 2.6% of the mass. of the stoichiometric amount. Used fraction contains 92,8% of the mass. alpha-olefins, of 2.5% of the mass. olefins with internal double bonds, 3,6% of the mass. vinylidene and 1.1% of the mass. paraffin hydrocarbons.

The mixture was kept at a temperature of 50°C for 20 min with constant stirring, and then begin feeding hydrogen to a pressure of 32 kg/cm2while increasing temperature the market to 130° C. under such conditions, the reaction mass was kept for 2 hours.

Then, the reactor serves the remainder of the stoichiometric quantity (261 g) fraction of olefins, C16-C18. The temperature was raised to 150°C, pressure up to 45 kgf/cm2and maintain the reaction mass in these conditions for 8 hours.

Upon completion of the reaction, reduce the temperature to 100°C, pressure up to 2 kgf/cm2can withstand 3 hours and unload the reaction mass from the reactor.

The resulting product contains 55.4% of the mass. trihexyphenidylum and 34.3% of the mass. trioctadecyl. Conversion of olefins accounts for 93.4%.

Example 5

The highest aluminiumrail get the same as described in example 2. Charged to the reactor 469 kg of triethylaluminum, 222 kg of aluminum and 222 g of the fraction of olefins With12-C14(THE 2411-058-05766801)containing 89.2% of mass. alpha-olefins, 0.5% mass. paraffin, 5.1% of the mass. vinylidene and 5.2% of the mass. hydrocarbons with an internal double bond which is 3.4% of the mass. of the stoichiometric amount. The mixture was kept at a temperature of 45°C for 25 min, then increase the temperature to 135°C, pressure up to 30 kgf/cm2feed to the reactor of hydrogen. In such conditions, the reaction mass was kept for 2 hours.

Then, the reactor serves 6297 kg fraction of olefins With12-C14. The temperature was raised to 152°S, is a t - up to 52 kg/cm2and maintain the reaction mass in these conditions for 10 hours.

Upon completion of the reaction, reduce the temperature to 80°C, pressure up to 1.5 kgf/cm2can withstand 2 hours and unload the reaction mass from the reactor.

The resulting product contains 55,75% of the mass. tridodetsilamin and 26,05% of the mass. trimethylenediamine. Conversion of olefins is 85.9%.

As seen from the above examples, the proposed method for obtaining the highest aluminization enhances the conversion of olefinic hydrocarbons in the process of obtaining the target product.

1. The method of obtaining the highest aluminization by the interaction of activated aluminium-containing reagent, triethylaluminum, hydrogen and olefin or olefin hydrocarbons at elevated temperature and pressure, characterized in that the activating expose the aluminum in the process of interaction of aluminum, triethylaluminum and part of the olefin or olefin hydrocarbons and maintained at a temperature of 40-50°C for 5-30 minutes, then begin to apply hydrogen, increasing the temperature up to 125-135 mA°C, kept at this temperature for 0.5-2 h, and then serve the remaining amount of olefin or olefin hydrocarbons formed and maintained the reaction mass at a temperature of 135-155°C for 5-10 hours

2. SPO is about getting the highest aluminization according to claim 1, characterized in that the activation of aluminum serves 2.5 to 7.0 wt.% olefin or olefin hydrocarbons of the stoichiometric amount.



 

Same patents:

FIELD: chemical technology.

SUBSTANCE: invention relates to a method for treatment of aluminum alcoholates. Method involves passing aluminum alcoholates through a column filled with extrudates of aluminum oxide in γ-form with pore volume from 0.4 to 0.8 cm3/g prepared by preliminary hydrolysis of aluminum alcoholates, molding the prepared aluminum oxide to extrudates with diameter from 1.6 to 3 mm and length 3-4 mm and their following purification by calcinations at temperature 400-500°C. As a rule, the treatment of alcoholates is carried out at temperature 20-150°C in column for 1-5 h. Method provides the development of simple and available technology for treatment of aluminum alcoholates with hydrocarbon chain length from C3 to C6 and above from impurities up to the level 10-3-10-4 wt.-%.

EFFECT: improved treatment method.

2 cl, 5 ex

FIELD: chemistry of metalloorganic compounds, chemical technology.

SUBSTANCE: invention relates to the improved method for preparing polyalkoxyalumoxanes of the general formula: RO{[-Al(OR)-O-]x[-Al(OR*)-O-]y}zH wherein z = 3-100; x + y = 1; R*/Al = 0.05-0.95; R means CnH2n+1; n = 1-4; R* means -C(CH3)=CHC(O)CnH2n+1; -C(CH3)=CHC(O)OCnH2n+1, and preparing a silica-free binding agent based on thereof for producing refractory corundum ceramics for precise casting by melting out models. Method is carried out by interaction of organoaluminum compound with alcohol and chelating agent in an organic solvent medium wherein compound of the general formula: AlL3 is used as organoaluminum compound wherein L means CnH2n+1, CnH2n+1O, (CnH2n+1)2AlO[(CnH2n+1)AlO]t wherein n = 1-4 and t = 2-10 that is subjected for interaction with water, alcohol and chelating agent at temperature 0-250°C wherein compound of the formula R*OH is used as a chelating agent wherein R* means -C(CH3)=CHC(O)CnH2n+1; -C(CH3)=CHC(O)CnH2n+1 in the mole ratio H2O : ROH : R*OH = p : x : y wherein p = 0.001-1; x = 0.05-0.95; y = 0.05-0.95, and x + y = 1. Also, invention describes a silica-free binding agent based on chelated polyalkoxyalumoxanes in the following ratio of components, wt.-%: chelated polyalkoxyalumoxane, 5-90, and aliphatic alcohol, the balance, up to 100. Invention provides preparing air-stable polyalkoxyalumoxanes and a silica-free binding agent based on thereof, simplifying technology in preparing the corundum composition suspension and fitness period of suspension is prolonged.

EFFECT: improved preparing method, improved and valuable properties of compounds.

3 cl, 3 tbl, 2 ex

FIELD: chemistry of metalloorganic compounds, chemical technology.

SUBSTANCE: invention relates to a method for preparing aluminum-organic compounds of the general formula (I) wherein R means ethyl (Et), n-propyl (n-Pr), n-butyl (n-Bu). Method involves interaction of di-substituted acetylenes with ethylaluminum dichloride (EtAlCl2) in the presence of metallic Mg and a catalyst in argon atmosphere under atmosphere pressure and room temperature for 8 h followed by addition of maleic anhydride at temperature -5°C and stirring the reaction mass at room temperature for 8 h. The yield of the end product is 56-78%. Proposed compounds can be used in fine organic and metalloorganic synthesis and as co-catalysts in processes of oligo- and polymerization of olefins and coupled dienes.

EFFECT: improved preparing method.

2 cl, 1 tbl, 1 ex

The invention relates to a method of obtaining new alyuminiiorganicheskikh compounds which may find application as components of catalytic systems in the processes of oligomerization and polymerization of olefin and diene hydrocarbons, and fine organic and ORGANOMETALLIC syntheses

The invention relates to a method of obtaining a new alyuminiiorganicheskikh connection, which can be applied in thin organic synthesis, and as acetalization in oligo - and polymerization of Alifanov and conjugated dienes

The invention relates to a method of obtaining new alyuminiiorganicheskikh compounds of General formula

< / BR>
where R is CH3or n-C3H7; R1-n-C6H13or n-C8H17that may find application in thin organic and ORGANOMETALLIC synthesis, as well as socialization in the processes of oligo - and polymerization of olefins and conjugated dienes

The invention relates to methods of producing new aluminum-organic compounds, which can find application in organic and ORGANOMETALLIC synthesis

The invention relates to methods of producing new aluminum-organic compounds, which can find application in organic and ORGANOMETALLIC synthesis

The invention relates to a method of obtaining a new alyuminiiorganicheskikh connection, which can be applied in thin organic and ORGANOMETALLIC synthesis

The invention relates to a method of obtaining a new alyuminiiorganicheskikh connection, which can be applied in thin organic synthesis, and as acetalization in oligo - and polymerization of olefins and conjugated dienes

FIELD: chemistry of metalloorganic compounds, chemical technology.

SUBSTANCE: invention relates to a method for preparing aluminum-organic compounds of the general formula (I) wherein R means ethyl (Et), n-propyl (n-Pr), n-butyl (n-Bu). Method involves interaction of di-substituted acetylenes with ethylaluminum dichloride (EtAlCl2) in the presence of metallic Mg and a catalyst in argon atmosphere under atmosphere pressure and room temperature for 8 h followed by addition of maleic anhydride at temperature -5°C and stirring the reaction mass at room temperature for 8 h. The yield of the end product is 56-78%. Proposed compounds can be used in fine organic and metalloorganic synthesis and as co-catalysts in processes of oligo- and polymerization of olefins and coupled dienes.

EFFECT: improved preparing method.

2 cl, 1 tbl, 1 ex

FIELD: chemistry of metalloorganic compounds, chemical technology.

SUBSTANCE: invention relates to the improved method for preparing polyalkoxyalumoxanes of the general formula: RO{[-Al(OR)-O-]x[-Al(OR*)-O-]y}zH wherein z = 3-100; x + y = 1; R*/Al = 0.05-0.95; R means CnH2n+1; n = 1-4; R* means -C(CH3)=CHC(O)CnH2n+1; -C(CH3)=CHC(O)OCnH2n+1, and preparing a silica-free binding agent based on thereof for producing refractory corundum ceramics for precise casting by melting out models. Method is carried out by interaction of organoaluminum compound with alcohol and chelating agent in an organic solvent medium wherein compound of the general formula: AlL3 is used as organoaluminum compound wherein L means CnH2n+1, CnH2n+1O, (CnH2n+1)2AlO[(CnH2n+1)AlO]t wherein n = 1-4 and t = 2-10 that is subjected for interaction with water, alcohol and chelating agent at temperature 0-250°C wherein compound of the formula R*OH is used as a chelating agent wherein R* means -C(CH3)=CHC(O)CnH2n+1; -C(CH3)=CHC(O)CnH2n+1 in the mole ratio H2O : ROH : R*OH = p : x : y wherein p = 0.001-1; x = 0.05-0.95; y = 0.05-0.95, and x + y = 1. Also, invention describes a silica-free binding agent based on chelated polyalkoxyalumoxanes in the following ratio of components, wt.-%: chelated polyalkoxyalumoxane, 5-90, and aliphatic alcohol, the balance, up to 100. Invention provides preparing air-stable polyalkoxyalumoxanes and a silica-free binding agent based on thereof, simplifying technology in preparing the corundum composition suspension and fitness period of suspension is prolonged.

EFFECT: improved preparing method, improved and valuable properties of compounds.

3 cl, 3 tbl, 2 ex

FIELD: chemical technology.

SUBSTANCE: invention relates to a method for treatment of aluminum alcoholates. Method involves passing aluminum alcoholates through a column filled with extrudates of aluminum oxide in γ-form with pore volume from 0.4 to 0.8 cm3/g prepared by preliminary hydrolysis of aluminum alcoholates, molding the prepared aluminum oxide to extrudates with diameter from 1.6 to 3 mm and length 3-4 mm and their following purification by calcinations at temperature 400-500°C. As a rule, the treatment of alcoholates is carried out at temperature 20-150°C in column for 1-5 h. Method provides the development of simple and available technology for treatment of aluminum alcoholates with hydrocarbon chain length from C3 to C6 and above from impurities up to the level 10-3-10-4 wt.-%.

EFFECT: improved treatment method.

2 cl, 5 ex

FIELD: chemistry of metalloorganic compounds, chemical technology.

SUBSTANCE: invention relates to the improved method for preparing higher organoaluminum compounds, namely, to trialkyl aluminum. Method is carried out by interaction of aluminum preliminary subjected for activation with triethyl aluminum, hydrogen and olefin or olefin hydrocarbons at increased temperature and pressure. Activation of aluminum is carried out by interaction of aluminum, triethyl aluminum and part of olefin or olefin hydrocarbon and kept at temperature 40-50°C followed by feeding hydrogen and by increasing temperature to 125-135°C, kept at this temperature for 0.5-2 h, the remained amount of olefin or olefin hydrocarbon is fed and kept the formed reaction mass at temperature 135-155°C for 5-10 h. method provides enhancing conversion of olefins in the process for synthesis of trialkyls aluminum that are used broadly in different branches of industry, in particular, in production of polyolefins, higher saturated alcohols and others.

EFFECT: improved preparing method.

2 cl, 5 ex

FIELD: chemistry of organometallic compounds, chemical technology, organic synthesis.

SUBSTANCE: invention relates to a method for synthesis of new organoaluminum compounds. Method involves interaction of phenylallyl acetylene with ethylaluminum dichloride in the presence of metallic magnesium and zirconacene dichloride as a catalyst in argon atmosphere at room temperature in tetrahydrofuran medium for 8-12 h. Synthesized organoaluminum compound can be used as a component of catalytic systems in processes of oligomerization and polymerization of olefins and diene hydrocarbons, and in fine and industrial organic and organometallic synthesis also.

EFFECT: improved method of synthesis.

2 cl, 1 tbl, 9 ex

FIELD: chemistry, chemical technology.

SUBSTANCE: invention relates to quaternized phthalocyanines and their using for treatment of water against bacterial pollution. Invention describes novel quaternized phthalocyanines representing poly-(trialkylammoniomethyl)-substituted zinc and aluminum phthalocyanines that are sensitizing agents in formation of singlet oxygen by effect of visible light. Also, invention relates to a method for photodisinfection of water by using these quaternized phthalocyanines or their mixtures with dyes of acridine, rhodamine or phenothiazine series and radiation in visible range in the presence of oxygen that provides the effective treatment of water against bacterial pollution.

EFFECT: valuable properties of compounds, improved method of water treatment.

3 cl, 5 tbl, 16 ex

FIELD: medicine, in particular photosensitizing agents for photodynamic therapy.

SUBSTANCE: invention relates to quaternary phthalocyanines of general formula MPc(CH2X)nCln, wherein Pc is phthalocyanine rest C32H16N8; M is Zn, AlY; n = 6-8; X is Y is Cl, OH, OSO3H, useful as photosensitizing agents in photodynamic therapy having high photoinduced activity in vivo and in vitro.

EFFECT: new class of effective photosensitizing agents useful in treatment of various tumors by photodynamic therapy.

1 dwg, 8 ex

FIELD: medicine, in particular photosensitizing agents for antimicrobial photodynamic therapy.

SUBSTANCE: invention relates to new photosensitizing agents for antimicrobial photodynamic therapy namely cationic phthalocyanines of general formula MPc(CH2X)nCln, wherein Pc is phthalocyanine rest C32H16N8; M is Zn, AlY; n = 6-8; X is Y is Cl, OH, OSO3H. Claimed agents is characterized by wide range of antimicrobial activity. Single complex action of nontoxic in darkness micromolar (up to 2.0 muM) concentration thereof and low dose of red irradiation make it possible to produce high inactivation levels (up to 97-99 %) both gram-negative bacteria and yeast fungi of genus Candida.

EFFECT: improved agents for treatment of various severe complications of inflammation diseases.

3 dwg, 13 ex, 2 tbl

FIELD: chemistry of metalloorganic compounds, chemical technology, metalloorganic synthesis.

SUBSTANCE: invention relates to a method to synthesis of 1-chloro-2,3,4,5-tetraalkylaluminacyclopenta-2,4-dienes. Method is carried out by interaction of disubstituted acetylenes with aluminum trichloride in the presence of metallic magnesium and zirconacen dichloride as a catalyst in argon atmosphere at room temperature for 8-12 h. Invention provides using available reagents and simplifying method.

EFFECT: improved method of synthesis.

1 tbl, 12 ex

FIELD: chemistry of metalloorganic compounds, chemical technology.

SUBSTANCE: invention relates to organic synthesis, namely, to a method for synthesis of novel organoaluminum compounds. Method involves interaction of phenylallylacetylene with dialkylaminoaluminum dichloride in the presence of metallic magnesium and zircocene dichloride as a catalyst, in argon atmosphere at room temperature, in tetrahydrofuran medium for 8-12 h. Invention provides simplifying method and using available reagents.

EFFECT: improved method of synthesis.

1 tbl, 11 ex

Up!