Polor monomer homopolymerization and copolymerization titanium-substituted beta-dione-cobalt acetylacetonate composite catalyst and its preparing method

A technology of polar monomers and catalysts, applied in the field of titanium-substituted β-diketone-cobalt acetylacetonate Co2 composite catalysts and its preparation, which can solve problems such as performance and application limitations, and complex preparation of catalysts

Inactive Publication Date: 2004-01-28
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the preparation of this catalyst is complicated, and high-valence MAO or boron compounds need to be used as cocatalysts. The obtained product ester is mainly located at the end group, and its performance and application are limited.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1. Catalyst preparation:

[0024] 1-1 mix 0.3g Co(acac) 2 Dissolve in 15ml of dichloromethane to make a homogeneous solution.

[0025] 1-2 Add 1g of anhydrous MgCl 2 Place in another reaction flask, add 15ml THF and 2ml absolute ethanol, heat to 60-75°C and stir for 2 hours until completely dissolved to obtain MgCl 2 mother liquor.

[0026] 1-3 in N 2 Under air flow, 3g SiO 2 Heating and dehydration, heating to 600°C and cooling for 6 hours to obtain pretreated SiO 2 , add 1-2 to the prepared mother liquor, stir and react at 65-70°C for 2 hours, and drain the solvent at 65-80°C.

[0027] 1-4 Add 15ml of dichloromethane to the product of 1-3, and add 0.12ml of TiCl under stirring 4 , react at 60~70°C for 1-2h; add 0.24ml benzoylacetone (bzac) and 1-1 to prepare Co(caca) 2 The solution is reacted at 60-70° C. for 1-2 hours, and the solvent is drained to obtain a composite main catalyst.

[0028] 1-5 composite main catalyst and AlEt 2 Cl or AlEt 2 Cl-AlR 3 The ...

Embodiment 2

[0035] In embodiment 1 step 1-1 " will 0.3g Co(acac) 2 Dissolved in 15ml of dichloromethane" was changed to "0.15g Co(acac) 2 Dissolved in 7.5ml of dichloromethane", all the other conditions and operations are the same as in Example 1. The prepared catalyst is used for the polymerization reaction under the same conditions as in Example 1.

[0036] Under the above conditions, the homopolymerization reaction prepares P4-VP, and the catalytic efficiency is 43kg. PMA / mol(Ti+Co), MA conversion 52%. Copolymerization reaction prepares P (E-4-VP) catalytic efficiency is 24kg P (E-4-VP) mol (Ti+Co), contains 17.5% 4-VP in the copolymer; Prepares P (E-MA), catalytic efficiency It is 18.3kg P(E-MA), and the copolymer contains 6.5% MA.

Embodiment 3

[0038] In Step 2 of Example 1, "...then add 4-VP or MA, stir and react at 30°C for 5h" to "...then add 4-VP or MA, stir and react at 30°C for 0.5h, then add AlEt with Al / Ti molar ratio 50 / 1 3 , Continue to react for 5h ", and all the other conditions and operations are the same as in Example One. The prepared catalyst is used for the polymerization reaction under the same conditions as in Example One.

[0039] Under the above conditions, the homopolymerization reaction prepares P4-VP, the catalytic efficiency is 65kg P4-VP / mol (Ti+Co), and the 4-VP conversion rate is 95%; the preparation of PMA, the catalytic efficiency is 59kg PMA / mol (Ti+Co) , MA conversion was 53%. Copolymerization prepared P(E-4VP), the catalytic efficiency was 32kg P(E-4-VP) / mol(Ti+Co), containing 22% 4-VP in the copolymer; prepared P(E-MA), the catalytic efficiency It is 20.5kg P(E-MA) / mol(Ti+Co), and the copolymer contains 12% MA.

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Abstract

The present invention relates to a titanium-substituted beta-diketone-Co-(acac)2 (cobalt acetylacetonate) compound catalyst for homopolymerization and copolymerization of polar monomer 4-vinylpyridine and methyl acrylate to prepare polyvinylpyridine (P4-VP), polymethyl acrylate (PMA) and copolymer of the above-mentioned materials and ethylene and its preparation method. The composition of said catalyst includes compound main catalyst made up by loading titanium compound, cobalt acetylacetonate and substituted beta-diketone on the MgCl2-SiO2 composite carrier and cocatalyst formed from AlEt2Clor alkylaluminium and AlEt2Cl, and its preparation method adopts impregnation reaction process, and said invented product is a spherical compound catalytic system.

Description

technical field [0001] The present invention relates to a kind of titanium that is used for polar monomer 4-vinylpyridine, methyl acrylate homopolymerization and copolymerization to prepare polyvinylpyridine (P4-VP), polymethyl acrylate (PMA) and their and ethylene copolymer - Substituted β-diketone-cobalt acetylacetonate Co(acac) 2 Composite catalyst and its preparation method. Background technique [0002] It is well known that it is difficult to polymerize and copolymerize polar monomers to obtain homopolymers and copolymers using traditional Ziegler-Natta (Z-N) catalysts. It is reported in the literature that the double imine complexes of late transition metal Pd and methyl Aluminoxane (MAO) catalyzed the copolymerization of methyl acrylate to produce a random copolymer, which has attracted widespread attention (Johnsom L.K., Mecking, S, Brookhart M., J.Am.Chem.Soc, 1996,118:267. ). However, the preparation of this catalyst is complicated, and high-valence MAO or boro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F4/70C08F10/02C08F20/14C08F26/06
Inventor 王海华张启兴胡志华范新刚
Owner SUN YAT SEN UNIV
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