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Dual-core cage-shaped earth samarium (III) organic complex, and preparation method and application thereof

An organic complex and cage-like technology, which is applied in the field of synthesis of new catalytic materials, achieves the effects of mild reaction conditions, mild catalytic reaction conditions, and simple operation

Active Publication Date: 2017-07-07
HENGYANG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The traditional rare earth catalyst system mainly focuses on the activity research of catalyzing the polymerization of diene, the synthesis of rubber and the regularity of polyolefin, etc., but there are few catalytic reports on the reaction of alkyd resin, and most of these rare earth catalysts are Inorganic complex

Method used

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  • Dual-core cage-shaped earth samarium (III) organic complex, and preparation method and application thereof
  • Dual-core cage-shaped earth samarium (III) organic complex, and preparation method and application thereof
  • Dual-core cage-shaped earth samarium (III) organic complex, and preparation method and application thereof

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Experimental program
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Effect test

Embodiment 1

[0038] A Novel Dinuclear Caged Rare Earth Samarium(III) Organic Complex Sm 2 (C 7 h5 ClCOO) 6 (C 12 h 8 N 2 ) 2 (H 2 O) 2 The synthesis, its reaction steps are as follows:

[0039] Add 0.64mmol (100.20mg) o-chlorobenzoic acid, 0.32mmol (82.15mg) samarium chloride and 0.32mmol (63.40mg) 1,10-phenanthroline into a mixed solvent of 20mL acetonitrile and water (volume ratio 5: 1), react for 1 hour, adjust the pH value to 6.5 with a concentration of 0.3mol / L sodium hydroxide solution, and react for 14 hours at 80°C. After the reaction is completed, a red solution is obtained, filtered, and the filtrate is covered with a fresh-keeping film, and placed Naturally volatilized at room temperature, a colorless crystal suitable for X-ray single crystal structure analysis was precipitated after one month, and the yield was 45.36%. M.P.205~207℃; IR main absorption peaks are: 1678(vs), 1595(vs), 1484(vs), 1423(vs),, 1290(m), 1234(w), 1105(w), 1072( m), 841(m), 806(w), 727(vs), 694(...

Embodiment 2

[0041] A Novel Dinuclear Caged Rare Earth Samarium(III) Organic Complex Sm 2 (C 7 h 5 ClCOO) 6 (C 12 h 8 N 2 ) 2 (H 2 O) 2 The synthesis of:

[0042] Add 0.87mmol (136.21mg) o-chlorobenzoic acid, 0.36mmol (143.77mg) samarium acetate tetrahydrate and 0.24mmol (47.55mg) 1,10-phenanthroline to 25mL N,N'-dimethylacetamide, ethanol In a mixed solvent with water (volume ratio 5:3:2), react. After 2 hours, use 0.5mL of concentrated ammonia water to adjust the pH value to 6.8, and react at 70°C for 13 hours. After the reaction is completed, a red solution is obtained and filtered. , the filtrate is covered with a layer of fresh-keeping film, placed at room temperature to volatilize naturally, and after two weeks, colorless crystals suitable for X-ray single crystal structure analysis are precipitated, with a yield of 43.21%.

Embodiment 3

[0044] A Novel Dinuclear Caged Rare Earth Samarium(III) Organic Complex Sm 2 (C 7 h 5 ClCOO) 6 (C 12 h 8 N 2 ) 2 (H 2 O) 2 The synthesis of:

[0045] Add 0.56mmol (87.68mg) of o-chlorobenzoic acid, 0.28mmol (139.65mg) of samarium carbonate hydrate and 0.36mmol (71.32mg) of 1,10-phenanthroline into a mixed solvent of 20mL of acetonitrile, ethanol and water (volume ratio 2:3:1), after 2 hours, adjust the pH value to 6.0 with triethylamine, and react at 75°C for 15 hours. It evaporates naturally at room temperature, and after three weeks, a colorless crystal suitable for X-ray single crystal structure analysis is precipitated, with a yield of 48.02%.

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Abstract

The invention discloses a dual-core cage-shaped earth samarium (III) organic complex, and a preparation method and application thereof. The complex adopts o-chlorobenzoic acid as a main ligand and 1,10-phenanthroline as an auxiliary ligand, and has a dual-core cage-shaped structure; the preparation method is characterized by adopting the o-chlorobenzoic acid, samarium salt and the 1,10-phenanthroline as raw materials, synthesizing through a solvent method, and obtaining an Sm2(C7H5OClCOO)6(C12H8N2)2 crystal through self-volatilization crystallization. The preparation method is simple to operate, moderate in reaction condition, high in product yield, and uniform in crystal particles; the earth samarium (III) organic complex is stable in structure, is used as a catalyst to be applied to catalyzing binary acid and polyhydric alcohols for carrying out esterification reaction to prepare an alkyd resin, and shows excellent catalytic activity.

Description

technical field [0001] The invention relates to a rare earth samarium (III) organic complex, in particular to a novel dinuclear cage rare earth samarium (III) organic complex and a preparation method thereof and the dinuclear cage rare earth samarium (III) organic complex as a catalyst in alcohol The application in the preparation of acid resin belongs to the field of synthesis of new catalytic materials. Background technique [0002] The rare earth catalytic system is the most significant catalytic system discovered in the past 40 years, which has greatly expanded the scope and connotation of Ziegler-Natta directional polymerization. At present, the application of rare earth catalysts in the synthesis of various polymers is a field of concern and research in China and many countries around the world. The traditional rare earth catalyst system mainly focuses on the activity research of catalyzing the polymerization of diene, the synthesis of rubber and the regularity of pol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/00C08G63/84C08G63/49
CPCC07F5/003C08G63/48C08G63/84
Inventor 李薇李翀宇李昶红谭雄文付伟伟
Owner HENGYANG NORMAL UNIV
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