Catalyst for metathesis polymerisation of dicyclopentadiene, production method thereof (versions) and polymerisation method thereof

FIELD: chemistry.

SUBSTANCE: catalysts for metathesis polymerisation of dicyclopentadiene are described, which are represented by [1,3-bis-(2,4,6-trimethylphenyl)-2-imidazolidinylidene]dichloro(o-N,N-diethylaminomethylphenylmethylene)ruthenium of formula (1) or [1,3-bis-(2,4,6-trimethylphenyl)-2-imidazolidinylidene]dichloro(o-N-pyrrolidinylmethylphenylmethylene)ruthenium of formula (2) . A method is described for producing a catalyst of formula (1), involving successively reacting a first generation Grubb catalyst with 1,3-bis-(2,4,6-trimethylphenyl)-2-trichloromethylimidazolidine and N,N-diethyl-(2-vinylbenzyl)amine in an inert atmosphere at temperature between 40 and 70°C in the presence of a solvent. In another version of the said method, a second generation Grubb catalyst is reacted with N,N-diethyl-(2-vinylbenzyl)amine in an inert atmosphere at temperature between 40 and 70°C in the presence of a solvent. A method is described for producing a catalyst of formula (2), involving successively reacting a first generation Grubb catalyst with 1,3-bis-(2,4,6-trimethylphenyl)-2-trichloromethylimidazolidine and 1-(2-vinylbenzyl)pyrrolidine in an inert atmosphere at temperature between 40 and 70°C in the presence of a solvent. In another version of the method, a second generation Grubb catalyst is reacted with 1-(2-vinylbenzyl)pyrrolidine in an inert atmosphere at temperature between 40 and 70°C in the presence of a solvent. A method is described for metathesis polymerisation of dicyclopentadiene, involving polymerisation using catalysts of formulae (1) or (2) in molar ratio monomer:catalyst ranging from 70000:1 to 100000:1.

EFFECT: increased output of catalyst and simpler synthesis due to less number of stages, obtaining polydicyclopentadiene with good application properties with low catalyst consumption.

7 cl, 6 ex

 

The technical field to which the invention relates.

The invention relates to the field of catalysis for the production of catalysts metathetical polymerization of cyclic olefins, in particular Dicyclopentadiene (DCPD).

The level of technology

The number of known catalysts with controlled catalytic activity, published by Grabban and patented the California Institute of Technology [UNG THAY; YANN SCHRODI, US 2005261451, 2005-11-24; A.Hejl, M.W.Day, R.H.Grubbs Organometallics 2006, 25, 6149-6154, .Ung, A.Hejl, R.H.Grubbs, Y.Schrodi Organometallics 2004, 23, 5399-5401]. The catalysts used to produce polymers of cycloolefins and bicycloalkanes reaction metathetical polymerization disclosure of the cycle when the molar ratio of monomer: catalyst in the range of 30,000:1 to 50000:1.

The disadvantage of existing catalysts is their high consumption and, as a consequence, the high cost of obtaining polydicyclopentadiene.

A known method of producing catalyst metathetical polymerization of Dicyclopentadiene (US 2005261451, 2005-11-24), namely, that the catalyst for the verification of the second generation or its derivatives are processed by the corresponding styrene in methylene chloride at 40°C.

The drawback of the method according to patent US 2005261451 is the low yield of the target product, which ranges from 50 to 65% based on the catalyst of the first generation. Uh what about due to the multi-stage synthesis and imperfection of methods.

From the above patent also known way metathetical polymerization of Dicyclopentadiene, which consists in the fact that the polymerization of Dicyclopentadiene is carried out at a ratio of monomer: catalyst 30000:1.

Disclosure of inventions

The problem solved by the claimed invention is to create a new efficient catalyst metathetical polymerization of Dicyclopentadiene, method of its production, and method of polymerization of Dicyclopentadiene.

In accordance with the task was created two new catalyst metathetical polymerization of Dicyclopentadiene (options).

The first catalyst metathetical polymerization of Dicyclopentadiene is a [1,3-bis-(2.4,6-trimetilfenil)-2-imidazolidinone]sodium dichloro(o-N,N-diethylaminocarbonylmethyl)ruthenium formula:

The structure and purity of the compounds is confirmed by the method of1H NMR (300 MHz, CD2Cl2) δ [n]: 0,41 (6N, t, J 7.0 Hz), 1,89-of 1.95 (2H, m), 2,30 (N, C), 2,58 (6N, (C), 2,81-is 2.88 (2H, m), 4,00-a 4.03 (4H, m), 4,17 (2H, s), 6,56 (1H, d, J 7,6 Hz), 6,97 (1H, d, J 7,6 Hz), 6,99 (4H, s), 7,14 (1H, t, J 7,6 Hz), 7,49 (1H, t, J 7,6 Hz) 18.65 (1H, s).

The second catalyst metathetical polymerization of Dicyclopentadiene is a [1,3-bis-(2,4,6-trimetilfenil)-2-imidazolidinone]sodium dichloro(o-N-pyrrolidinylcarbonyl)ruthenium formula:

The structure and purity of the compounds is confirmed by the method of1H NMR (300 MHz, CD2Cl2) δn: 1,27 (2H, m)of 1.44 (2H, m), is 2.09 (2H, m), 2,38 (N, C), 2,47 (6N,) 4,07 (4H, m), is 4.21 (2H, m), 6,69 (1H, d, J 7.5 Hz), 6,97 (1H, d, J 7.5 Hz), 7,03 (4H, s), 7,16 (1H, t, J 7.5 Hz), of 7.48 (1H, t, J 7.5 Hz,) 18.79 (1H, s).

The claimed catalysts are superior to the catalysts disclosed in the patent [US 2005261451], and allow you to get polydicyclopentadiene with high consumer properties at a molar ratio of monomer: catalyst from 70000:1 to 200000:1, while for known catalysts the ratio of 30000:1 and 40,000:1. (US 2005261451 2005-11-24).

The synthesis of the catalysts (1) and (2) includes one or two stages. One-step process represents the processing of a commercially available catalyst for the verification of the second generation (GII) the corresponding derivatives of aminosterol: (N,N-diethyl-(2-vinylbenzyl) - amine or 1-(2-vinylbenzyl)pyrrolidine. Two-stage process includes a preliminary introduction N-heterocyclic ligand 1,3-bis-(2,4,6-trimetilfenil)-2-imidazolidinone in the catalyst for the verification of the first generation (GI), resulting in a catalyst for the verification of the second generation (GII), which is then converted into the claimed catalysts similar one-step process. In the two-stage process stage can be carried out without separating the tick complex, which improves the yield of the target compound.

The claimed methods allow to increase the output of the catalyst and to simplify circuit synthesis by reducing the number of stages.

The way metathetical polymerization of Dicyclopentadiene is that the polymerisation process is carried out using the catalysts of (1) or (2) at a molar ratio of substrate: catalyst from 70000:1 to 100000:1. Holding metathetical polymerization with the use of the claimed catalysts can reduce the cost of obtaining a polymer by reducing the flow rate of the catalyst.

The implementation of the invention

The synthesis of the claimed catalysts for one-step process of the catalyst of the verification of the second generation (GII) is carried out in toluene or methylene chloride by the reaction:

The yield of the target product is 70-83%.

Obtaining catalysts for the two-stage process of the catalyst of the verification of the first generation (1-6) is carried out in toluene at 70°C. the outline of this process:

Synthesis of complexes is carried out without isolating the intermediate catalyst for the verification of the second generation (Gll-b). The yield of the target compound is 70-75%.

The complexes (1), (2) exhibit catalytic properties in the polymerization DCPD when the molar ratio is Oseni substrate:catalyst of from 100:1 to 200,000:1. Optimal for getting polydicyclopentadiene with high thermo-mechanical properties (high glass transition temperature and toughness) is the ratio of 100000:1. The catalysts are easily dissolved in the monomer at 35°C. the Exothermic polymerization occur when using the catalyst (1) (50°C, 20 min) and catalyst (2) (50°C, 40 min). Polymers do not have a smell, mechanical and thermal indices correspond to, and in some cases surpass those for industrial materials from polydicyclopentadiene (Thelen and Meton) [J.C.Mol J.Mol. Cat. A: Chemical, 2004, 213, 39-45; www.telene.com; www.metton.com].

The invention is illustrated by the following examples.

Example 1.

The synthesis of the catalyst is carried out in the conditions preventing ingress of moisture and air in the reaction system. Use equipment and reactors of the Harness connected to the vacuum system and line dry argon. Solvents: methylene chloride, toluene, hexane, methanol absolutetruth by standard methods and stored in an inert atmosphere [Armarego, Wilfred, L.F.; Chai, Christina, L.L. (2003). Purification of Laboratory Chemicals (5th Edition). Elsevier.] 2-vinyl-N,N-alkyl-benzylamine get well-known technique [Kolesnikov G.S. Synthesis of the vinyl derivatives of aromatic and heterocyclic compounds, 1960].

A mixture of GI-b 0.4 g (0.5 mmol) in 10 ml of toluene and 0,365 g (0.85 mmol, 1.7 EQ.) adduct of imidazole with chloroform (H2IMesCCl 3) is heated at 70°C in sealed vials under inert atmosphere for 12 hours, then add 0,237 g (1.25 mmol, 2.5 EQ.) N,N-diethyl-(2-vinylbenzyl)amine and the reaction mixture is heated for another 3.5 hours. The toluene evaporated in vacuo, to the residue add 5 ml of hexane, the precipitated precipitate is filtered off, washed with 5 ml of hexane and 4 ml of methanol. After drying in vacuo get 0.232 g (71%) catalyst (1) in the form of green crystals.1H NMR (300 MHz, CD2Cl2) δ [n]: 0,41 (6N, t, J 7.0 Hz), 1,89-of 1.95 (2H, m), 2,30 (N, C), 2,58 (6N, (C), 2,81-is 2.88 (2H, m), 4,00-a 4.03 (4H, m), 4,17 (2H, s), 6,56 (1H, d, J 7,6 Hz), 6,97 (1H, d, J 7,6 Hz), 6,99 (4H, s), 7,14 (1H, t, J 7,6 Hz), 7,49 (1H, t, J 7,6 Hz) 18.65 (1H, s).

Example 2.

In the flask Slanka 25 ml placed 170 mg (0.2 mmol) of the catalyst for the verification of the second generation (GII). The flask was filled with argon and poured a solution of 114 mg (0.6 mmol) of N,N-diethyl-(2-vinylbenzyl)amine in 4 ml of dry dichloromethane. The reaction mixture is boiled for 5 hours (40°C), then cooled and the solvent is distilled off in vacuum. The product distinguish using preparative chromatography on silica gel, elwira with a mixture of cyclohexane: tetrahydrofuran=4:1. Get the catalyst (1) 92.8 mg (57%) in the form of green crystals.

Example 3.

In the flask Slanka 25 ml was placed 200 mg (0.23 mmol) of the catalyst for the verification of the second generation (GII). The flask was filled with argon and poured a solution of 110 mg (or 0.57 mmol) of 1-(2-vinylbenzyl)pyrrolidine 4 m the absolute toluene. The reaction mixture is heated for 20 minutes at 70°C, then cooled and the solvent is distilled off in vacuum. The residue is washed with methanol and dried in vacuum. Get the catalyst (2) 109 mg (71%) in the form of green crystals.1H NMR (300 MHz, CD2Cl2) δH: 1,27 (2H, m)of 1.44 (2H, m), is 2.09 (2H, m), 2,38 (N, C), 2,47 (6N,) 4,07 (4H, m), is 4.21 (2H, m), 6,69 (1H, d, J 7.5 Hz), 6,97 (1H, d, J 7.5 Hz), 7,03 (4H, s). 7,16 (1H, t, J 7.5 Hz), of 7.48 (1H, t, J 7.5 Hz) 18.79 (1H,s).

Example 4.

A mixture of GI-b 0,219 g (0.26 mmol) in 5.5 ml of toluene and 0,198 g (0.46 mmol, 1.7 EQ.) adduct of imidazole with chloroform (H2IMesCCl3) is heated at 70°C in sealed vials under inert atmosphere for 18 hours, then add 0,132 g (of 0.65 mmol, 2.5 EQ.) 1-(2-vinylbenzyl)pyrrolidine and the reaction mixture is heated for another 3.5 hours. The toluene evaporated in vacuo, to the residue add 5 ml of methanol, the precipitated precipitate is filtered off, washed with 2 ml hexane and 2 ml of methanol. After drying in vacuo get complex (2) 0.113 g with a yield of 67%.

Example 5.

Complex "1" 1.37 mg (0.0017 mmol) dissolved at 35°C in at 26.87 g (173 mmol) of Dicyclopentadiene (DCPD) purity 99% (the molar ratio of catalyst: DCPD=1:100000). The mixture is heated in a beaker at 50°C for 20 min, then at 200°C 30 minutes Get a solid transparent sample polydicyclopentadiene (PGCPD) odorless. The glass transition temperature Tg of 152°C, the modulus of elasticity of 1.80 GPA, coefficient of linear mention the mini-expansion 81,6, yield strength tensile 52,0 MPa.

Example 6.

Complex "1" 1.89 mg (0.0024 mmol) dissolved at 35°C in at 26.87 g (173 mmol) DCPD purity 99% (the molar ratio of catalyst: DCPD=1:70000). The mixture is heated in a beaker at 50°C for 20 min, then To 200°C in 30 minutes Get a solid transparent sample PGCPD odorless. The glass transition temperature of 161°C., the modulus of elasticity of 1.86 GPA, coefficient of linear thermal expansion 45,8, yield strength tensile 56,1 MPa.

Example 7.

Complex "2" 1.87 mg (0.0024 mmol) dissolved at 35°C in at 26.87 g (173 mmol) DCPD 99% (the molar ratio of catalyst: DCPD=1:70000). The mixture is heated in a beaker at 50°C for 20 min, then at 200°C 30 minutes Get a solid transparent sample PGCPD odorless. The glass transition temperature of 173°C, the modulus of elasticity 1,68 GPA, coefficient of linear thermal expansion 66,0, yield strength tensile 52.4 MPa.

Example 8.

Complex "2" 1.3 mg (0.0017 mmol) dissolved at 35°C in at 26.87 g (173 mmol) DCPD 99% (the molar ratio of catalyst: DCPD=1:100000). The mixture is heated in a beaker at 50°C for 20 min, then at 200°C 30 minutes Get a solid transparent sample PGCPD odorless. The glass transition temperature of 153°C, the modulus of elasticity of 1.78 GPA, coefficient of linear thermal expansion 86,0, yield strength tensile 52,1 MPa.

1. A catalyst is metathetical polymerization of Dicyclopentadiene, representing [1,3-bis-(2.4,6-trimetilfenil)-2-imidazolidinone]sodium dichloro(o-N,N-diethyl-aminomethylpyrimidine)ruthenium formula:

2. The catalyst metathetical polymerization of Dicyclopentadiene, representing [1,3-bis-(2,4,6-trimetilfenil)-2-imidazolidinone]sodium dichloro(o-N-pyrrolidinylcarbonyl)ruthenium formula:

3. A method of obtaining a catalyst according to claim 1, characterized in that the catalyst for the verification of the first generation successively subjected to interaction with 1,3-bis-(2,4,6-trimetilfenil)-2-trichloromethylpyridine and (N,N-diethyl-(2-vinylbenzyl)amine in an inert atmosphere at a temperature of 40-70°C in the presence of a solvent.

4. The method of preparation of the catalyst according to claim 1, characterized in that the catalyst for the verification of the second generation is subjected to interaction with (N,N-diethyl-(2-vinylbenzyl)amine in an inert atmosphere at temperatures of 40-70°C in the presence of a solvent.

5. A method of obtaining a catalyst according to claim 2, characterized in that the catalyst for the verification of the first generation successively subjected to interaction with 1,3-bis-(2,4,6-trimetilfenil)-2-trichloromethylpyridine and 1-(2-vinylbenzyl) pyrrolidine in an inert atmosphere at a temperature of 40-70°C in the presence of a solvent.

6. The method of preparation of the catalyst according to claim 2, characterized erisugusest fact, the catalyst for the verification of the second generation is subjected to interaction with 1-(2-vinylbenzyl) pyrrolidine in an inert atmosphere at a temperature of 40-70°C in the presence of a solvent.

7. The way metathetical polymerization of Dicyclopentadiene, characterized in that the polymerization is performed with the use of catalysts according to claim 1 or 2 at a molar ratio of monomer: catalyst from 70000:1 to 100000:1.



 

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