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Preparation method and application of ruthenium-carbene catalyst

A catalyst and carbene complex technology, applied in the field of preparation of ruthenium carbene complexes, can solve the problems of limited application scope, many synthesis steps, complicated processes, etc., and achieve the effects of simple equipment and process, high activity, and rational utilization of resources

Inactive Publication Date: 2015-04-29
CHANGCHUN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to many synthesis steps, complex process, high price, etc., the scope of industrial application is limited.

Method used

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  • Preparation method and application of ruthenium-carbene catalyst
  • Preparation method and application of ruthenium-carbene catalyst
  • Preparation method and application of ruthenium-carbene catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Example 1 A kind of preparation method of ruthenium carbene complex, described ruthenium carbene complex is two-triphenylphosphine-phenylethylene ether-dichlororuthenium complex, and its chemical formula is (PCy 3 ) 2 Cl 2 Ru=CHCH 2 OPh, the conditions and steps of the preparation method of described ruthenium carbene complex are as follows:

[0027] (one) Allyl phenyl ether C 9 h 10 Preparation of O: Add 50 mL of solvent acetone to the three-necked flask, then add 4.71 g (0.05 mol) of phenol, 7.26 g (0.06 mol) of 3-bromopropene and 7.60 anhydrous potassium carbonate in sequence at a molar ratio of 1:1.2:1.1 g (0.055 mol), the reaction temperature is 50 ℃, the reaction time is 6 h, and the reaction is carried out under the condition of reflux. After the reaction is completed, allyl phenyl ether C is obtained by suction filtration and vacuum distillation 9 h 10 O is 6.37 g, and the productive rate of the product obtained by the reaction is 95%, and the product ...

Embodiment 2

[0032] Example 2 A kind of preparation method of ruthenium carbene complex, described ruthenium carbene complex is two-triphenylphosphine-phenylethylene ether-dichlororuthenium complex, and its chemical formula is (PCy 3 ) 2 Cl 2 Ru=CHCH 2 Oph, the conditions and steps of the preparation method of the described ruthenium carbene complex are as follows:

[0033] (one) Allyl phenyl ether C 9 h 10 Preparation of O: Add 50 mL of solvent acetone into the three-necked flask, then add 4.71 g (0.05 mol) of phenol, 6.05 g (0.05 mol) of 3-bromopropene and 6.91 g of anhydrous potassium carbonate in sequence at a molar ratio of 1:1:1. g (0.05 mol), the reaction temperature is 40 ℃, the reaction time is 7 h, and the reaction is carried out under the condition of reflux. After the reaction is completed, allyl phenyl ether C is obtained by suction filtration and vacuum distillation 9 h 10 O was 6.00 g, and the yield of the product obtained by the reaction was 90%.

[0034] (two)...

Embodiment 3

[0038] Example 3 A kind of preparation method of ruthenium carbene complex, described ruthenium carbene complex is two-triphenylphosphine-phenylethylene ether-dichlororuthenium complex, and its chemical formula is (PCy 3 ) 2 Cl 2 Ru=CHCH 2 Oph, the conditions and steps of the preparation method of the described ruthenium carbene complex are as follows:

[0039] (one) Allyl phenyl ether C 9 h 10 Preparation of O: Add 50 mL of solvent acetone into a three-necked flask, then add 4.71 g (0.05 mol) of phenol, 12.10 g (0.1 mol) of 3-bromopropene and 13.82 anhydrous potassium carbonate in sequence at a molar ratio of 1:2:2 g (0.1 mol), the reaction temperature is 60 °C, the reaction time is 4 h, and the reaction is carried out under the condition of reflux. After the reaction is completed, allyl phenyl ether C is obtained by suction filtration and vacuum distillation 9 h 10 O was 5.90 g, and the yield of the product obtained by the reaction was 88%.

[0040] (two) Prepa...

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Abstract

The invention discloses a preparation method and application of a ruthenium-carbene catalyst. According to the invention, a ruthenium-carbene complex is prepared by a method of olefin metathesis, the device and technology used for preparation are simple, only two-step reaction is needed, the cost is lower, and the production rate can reach 95%. According to the invention, the ruthenium-carbene complex is used as a catalyst for a ring-opening metathesis polymerization reaction of dicyclopentadiene so as to prepare polydicyclopentadiene. The activity of the ring-opening metathesis polymerization reaction is high, the transformation rate to the polymerization of the dicyclopentadiene is 99.8%, the reaction condition is moderate, high temperature and high pressure are not needed, resources are reasonably utilized, the reaction has no bad influence on the environment, and therefore, the method disclosed by the invention is a green process route, and is suitable for industrial popularization.

Description

technical field [0001] The invention relates to a preparation method of a ruthenium carbene complex and its use in the ring-opening metathesis polymerization of dicyclopentadiene, belonging to the field of polymerization catalysis. Background technique [0002] Dicyclopentadiene is derived from ethylene cracking C 5 Distillate, rich in sources, low in price, space structure is divided into bridging ring type and hanging ring type, bridging ring type is more common, it has two unsaturated double bonds, relatively active chemical properties, widely used in polymer materials and fine chemicals Applications. [0003] Polydicyclopentadiene is an important new thermosetting polymer engineering material. It has excellent mechanical properties, medium resistance and thermal stability, and has a wide range of uses in the fields of transportation, sports facilities, building materials, electrical equipment and communications. [0004] The ring-opening metathesis polymerization cata...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/00C08F132/08C08F4/80
CPCC07F15/0046C08F4/80C08F132/08
Inventor 张龙刘晶晶
Owner CHANGCHUN UNIV OF TECH
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