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Gas-phase polymerization method for catalyzing olefin homopolymerization by using late transition metal catalyst

A post-transition metal, gas-phase polymerization technology, which is applied in the field of gas-phase polymerization of olefin homogeneous polymerization catalyzed by late-transition metal catalysts, can solve the problem of polyolefins needing to be dried, the discharge of organic waste liquid has a great impact on the environment, and the post-treatment process requires higher requirements, etc. problems, to achieve the effect of improving industrial production efficiency, zero organic waste discharge, and reducing production costs

Active Publication Date: 2020-07-14
合肥中科科乐新材料有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the heterogeneous system catalytic polymerization process in the industry is quite mature, a large amount of organic solvents need to be used in the process flow of these existing methods to serve as reaction solvents and eluents, and there are problems such as polyolefins need to be dried ; This has higher requirements for the post-treatment process of the olefin polymerization industry and the discharge of organic waste liquid has a greater impact on the environment

Method used

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  • Gas-phase polymerization method for catalyzing olefin homopolymerization by using late transition metal catalyst
  • Gas-phase polymerization method for catalyzing olefin homopolymerization by using late transition metal catalyst
  • Gas-phase polymerization method for catalyzing olefin homopolymerization by using late transition metal catalyst

Examples

Experimental program
Comparison scheme
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Embodiment

[0046] The following examples are used to illustrate specific embodiments of the present invention. The data provided include the gas phase polymerization data of different catalysts and the test data of the resulting polymer. All sensitive substances are stored in a glove box. Ethylene gas is removed by water removal. Oxygen column purification.

[0047] All preparations of the following examples were carried out according to standard Schlenk techniques.

[0048] The reagents used in the following examples were obtained from commercial sources unless otherwise specified, and were used directly without purification (dehydration and drying treatment may be performed if necessary).

[0049] The degree of branching of the polymer obtained in the following examples is obtained by nuclear magnetic resonance, and the deuterated solvent used for nuclear magnetic resonance is dried and distilled before use. Unless otherwise stated, 1 H and 13 C NMR spectra were recorded by a JNM-EC...

Synthetic example 1-8

[0054] Synthesis Example 1-8: Using Catalyst 1-8 to Catalyze Gas Phase Polymerization of Ethylene to Obtain Homopolymer of Ethylene

[0055] In a glove box or a fume hood, in a narrow-necked flask, mix 10 μmol of the corresponding α-diimine palladium complex of formula 1-8 (as a late transition metal catalyst) with 20 μmol of tetrakis(3,5-bis(tri Fluoromethyl)phenyl)sodium borate (NaBArF, as a cocatalyst) was mixed in 2 mL of dichloromethane and fully stirred to dissolve to obtain a catalyst solution.

[0056] The obtained catalyst solution was poured into a dried 350mL glass thick-walled pressure reactor along the reactor wall, and the catalyst solution was evenly coated on the reactor wall by gentle shaking, and in dichloromethane solvent After volatilization, a catalyst film layer is formed on the reactor wall.

[0057] The reactor with the catalyst film layer formed on the wall is connected with the ethylene high-pressure gas cylinder through a vacuum pipeline, and after ...

Synthetic example 9-14

[0066] Synthesis Examples 9-14: In the case of using the same catalyst (i.e. Catalyst 6), investigate the gas phase polymerization of ethylene under different reaction pressures, times and temperatures

[0067] The reaction process was the same as that of Synthesis Example 6 above, except that the reaction pressure, time and temperature were changed as shown in Table 2 below to carry out gas-phase polymerization, and the desired ethylene homopolymer was obtained. The results are shown in Table 2.

[0068] Table 2

[0069]

[0070] a Activity unit is 10 4 g / (mol Pd h);

[0071] b m n is the number average molecular weight of the obtained ethylene homopolymer;

[0072] c PDI is the molecular weight distribution of gained ethylene homopolymer;

[0073] d b rs For the degree of branching of the obtained ethylene homopolymer, i.e. the number of methyl groups corresponding to every 1000 methylene groups;

[0074] e T m Be the fusing point of gained ethylene homopolyme...

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Abstract

The invention relates to a gas-phase polymerization method for catalyzing olefin homogeneous polymerization by a late transition metal catalyst. The gas-phase polymerization method comprises the following steps: dissolving a mixture of the late transition metal catalyst and a cocatalyst in a volatile organic solvent according to a molar ratio of 1:1-1:3 to form a catalyst solution; putting the obtained catalyst solution into a pressure reactor and uniformly coating the catalyst solution on the wall of the pressure reactor so as to form a catalyst film layer on the wall after the volatile organic solvent is volatilized; and introducing olefin gas, and carrying out a contact reaction on olefin and the catalyst film layer at a reaction pressure of 1-10 atmospheres and a reaction temperature of 20-80 DEG C to obtain the required olefin polymer. The polyolefin material with excellent performance can be synthesized by using the homogeneous gas-phase polymerization method, and the mechanicalproperties of the polyolefin material can be regulated and controlled by controlling the polymerization conditions. In addition, the homogeneous gas-phase polymerization method provided by the invention significantly reduces the use of organic solvents, and belongs to an economic and environment-friendly olefin polymerization mode.

Description

technical field [0001] The invention relates to the field of synthesizing polymer polyolefin materials, in particular to a gas-phase polymerization method for olefin homogeneous polymerization catalyzed by late transition metal catalysts. Background technique [0002] Polyolefin materials are indispensable in people's production, life and industrial applications, and are widely used. Since the discovery of heterogeneous titanium and chromium catalysts in the 1950s, the polyolefin industry has developed rapidly, and by 2015 the global polyolefin production had reached 178 million tons, making the polyolefin industry a multi-billion dollar business. Due to the superior performance of heterogeneous systems in terms of product morphology control, avoiding reactor fouling and applicability in continuous polymerization processes, the industrial production of polyolefins is mainly based on the use of heterogeneous systems, such as Ziegler-Natta and Phillips catalysts etc.; but con...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F110/00C08F2/34C08F4/70C08F110/02
CPCC08F110/00C08F110/02C08F2/34C08F4/7006C08F2500/12C08F2500/03
Inventor 陈昶乐代胜瑜
Owner 合肥中科科乐新材料有限责任公司
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