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Synthesizing method for 2-tricarbonyl(methylcyclopentadienyl)manganese

A kind of methylcyclopentadiene manganese tricarbonyl, synthetic method technology, applied in chemical instruments and methods, organic chemistry, metallocene and other directions, can solve the problems of limiting MMT production efficiency, low yield, long time consumption, etc. The effect of shortening the dropping time, improving the yield and purity, and shortening the reaction time

Active Publication Date: 2019-04-12
YANGPU AOLI PETROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing process for synthesizing MMT takes a long time, and its yield is not high, which limits the production efficiency of MMT

Method used

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  • Synthesizing method for 2-tricarbonyl(methylcyclopentadienyl)manganese

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preparation example Construction

[0027] A kind of synthetic method of 2-methylcyclopentadiene manganese tricarbonyl, comprises the following steps:

[0028] S1, cyclosodium reaction:

[0029] Use white oil to soak the metal sodium wire for 3-5 minutes; prepare a sodium ring kettle, add metal sodium wire to the sodium ring kettle, and then add an organic solvent, the organic solvent is made of tetrahydrofuran and dichloromethane with a volume ratio of 1:1.2 to 3.5 obtained, temperature controlled to 0-15°C for dehydration;

[0030] Then add an auxiliary agent of 0.5-1 times the mass of metal sodium wire to the ring sodium kettle, the auxiliary agent is made of zinc oxide powder, nano silicon dioxide and dry ice in a mass ratio of 10:4-7:3-5, the preferred mass The ratio is 10:5:4.

[0031] Then add monocyclopentadiene dropwise, the molar ratio of the metal sodium wire to monocyclopentadiene is 1:0.9-1.2, and the dropwise addition is completed within 1h, and the reaction temperature is controlled to be 45-53°...

Embodiment 1

[0038] A kind of synthetic method of 2-methylcyclopentadiene manganese tricarbonyl, comprises the following steps:

[0039] S1, cyclosodium reaction:

[0040] Use white oil to soak the metal sodium wire for 3 minutes; prepare a sodium ring kettle, add metal sodium wire to the sodium ring kettle, and then add an organic solvent. The organic solvent is made of tetrahydrofuran and dichloromethane with a volume ratio of 1:1.2, and the temperature is controlled. To 0-15 ℃ for dehydration treatment;

[0041] Then add an auxiliary agent of 0.5 times the mass of the metal sodium wire to the ring sodium kettle, and the auxiliary agent is made of zinc oxide powder, nano silicon dioxide and dry ice in a mass ratio of 10:4:3;

[0042] Then add monocyclopentadiene dropwise, the molar ratio of the metal sodium wire to monocyclopentadiene is 1:0.9, and the dropwise addition is completed within 1 hour, and the reaction temperature is controlled to be about 45°C after the dripping to obtain c...

Embodiment 2

[0049] A kind of synthetic method of 2-methylcyclopentadiene manganese tricarbonyl, comprises the following steps:

[0050] S1, cyclosodium reaction:

[0051] Use white oil to soak the metal sodium wire for 5 minutes; prepare a sodium ring kettle, add metal sodium wire to the sodium ring kettle, and then add an organic solvent. The organic solvent is made of tetrahydrofuran and dichloromethane with a volume ratio of 1:3.5, and the temperature is controlled. To 0-15 ℃ for dehydration treatment;

[0052] Then add an auxiliary agent of 1 times the mass of metal sodium wire to the ring sodium kettle, and the auxiliary agent is made of zinc oxide powder, nano silicon dioxide and dry ice in a mass ratio of 10:7:5;

[0053] Then add monocyclopentadiene dropwise, the molar ratio of the metal sodium wire to monocyclopentadiene is 1:1.2, and the dropwise addition is completed within 1 hour, and the reaction temperature is controlled to be about 53°C after the dripping to obtain cyclope...

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Abstract

The invention provides a synthesizing method for 2-tricarbonyl(methylcyclopentadienyl)manganese. The synthesizing method includes the following steps that white oil is adopted for soaking metallic sodium wires; a sodium cyclizing kettle is prepared, the metallic sodium wires are added into the sodium cyclizing kettle, then an organic solvent is added, and temperature control is conducted for dewatering treatment; then an addition agent is added into the sodium cyclizing kettle and prepared from zinc oxide powder, nanosilicon dioxide and dry ice through pressing; then, mono-cyclopentadiene is dropwise added, reaction temperature is controlled after dropwise addition is completed, and a cyclopentadiene solution is prepared; the cyclopentadiene solution is conveyed to a high-pressure synthesizing kettle, and manganese chloride is pressed into the high-pressure synthesizing kettle through nitrogen gas; then, a catalyst is added and prepared from particles of rhodium oxide, ruthenium oxideand aluminum oxide; stirring is conducted, multiple times of backlash operations are conducted, and a reaction is conducted; carbon monoxide is constantly input into the high-pressure synthesizing kettle, temperature and pressure are controlled, and finally the 2-tricarbonyl(methylcyclopentadienyl)manganese is obtained. The synthesizing method shortens the period of synthesizing, the purity of theproduct is high, and the yield is high.

Description

technical field [0001] The invention relates to the technical field of 2-methylcyclopentadiene manganese tricarbonyl, in particular to a synthesis method of 2-methylcyclopentadiene manganese tricarbonyl. Background technique [0002] The full name of MMT is 2-methylcyclopentadiene manganese tricarbonyl. MMT has a wide range of applications, such as gasoline antiknock agent, gasoline standard increase agent, unleaded gasoline antiknock agent, gasoline octane number improver, and standard increase agent. and additives, etc. The existing process for synthesizing MMT takes a long time, and its yield is not high, which limits the production efficiency of MMT. Therefore be badly in need of a kind of synthetic method of 2-methylcyclopentadiene manganese tricarbonyl, solve above-mentioned technical problem. Contents of the invention [0003] In view of this, the present invention proposes a kind of synthetic method of 2-methylcyclopentadiene manganese tricarbonyl, solves the abo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F17/00
Inventor 郭银亮胡君
Owner YANGPU AOLI PETROCHEM
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