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Method for preparing methyl cyclopentadienyl tricarbonyl manganese through continuous reaction

A technology of methylcyclopentadiene manganese tricarbonyl and methylcyclopentadiene, which is applied in the field of chemical product preparation, can solve problems such as unstable batch yield and quality, inconvenient operation, and insufficient reaction, etc. To achieve the effect of widening the scope of use, stable product quality and sufficient response

Inactive Publication Date: 2012-01-11
HEBEI HUAGE FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are many defects in this batch reaction method, such as insufficient reaction, many by-products, inconvenient operation, unstable yield and quality between batches, etc.

Method used

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  • Method for preparing methyl cyclopentadienyl tricarbonyl manganese through continuous reaction
  • Method for preparing methyl cyclopentadienyl tricarbonyl manganese through continuous reaction

Examples

Experimental program
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Effect test

Embodiment 1

[0016] In a 1L continuous flow tank reactor, add 400 mL of 1,4-dioxane and replace it with a nitrogen atmosphere. Add 20 g of sodium metal and 100 mL of methylcyclopentadiene monomer continuously into the tank for 1 hour, and keep The reaction temperature is 150°C; the material in the continuous flow tank is continuously introduced into a 1L bubbling stirred tank, and 24g of anhydrous manganese chloride is continuously added to the bubbling stirred tank for 1 hour, and the reaction is carried out with CO for 6 hours, and the temperature is maintained. It is 70°C and the pressure is 5MPa. After the reaction is completed, the solvent is removed and rectification is carried out to obtain the product methylcyclopentadiene manganese tricarbonyl, and the product yield is 86% in terms of manganese chloride.

Embodiment 2

[0018] Continuously feed tetrahydrofuran into the tube reactor, and at the same time, 40 g of sodium metal and 180 mL of methylcyclopentadiene monomer are continuously fed into the tube reactor for 3 hours, keeping the reaction temperature at 200 ° C; In a 1L bubbling stirred tank, 90g of anhydrous manganese chloride was continuously added into the bubbling stirred tank for 2 hours, and reacted with CO for 2 hours, keeping the temperature at 110°C and the pressure at 9MPa. After the reaction is completed, the solvent is removed and rectification is carried out to obtain the product methylcyclopentadiene manganese tricarbonyl, and the product yield is 85% in terms of manganese chloride.

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Abstract

The invention provides a method for preparing methyl cyclopentadienyl tricarbonyl manganese through continuous reaction. The method comprises the following steps of: (1) continuously adding methyl cyclopentadiene monomer and metal sodium into a reactor A in which a dehydration solvent is held; and (2) continuously feeding feed liquor into a reactor B from the reactor A, continuously adding anhydrous manganese chloride into the reactor B, and introducing CO gas into the reactor B to perform reaction. The method has the obvious advantages of full reaction, less byproducts, high yield and easiness in large-scale industrialization due to adoption of continuous reaction in an entire reaction process.

Description

technical field [0001] The invention belongs to a method for preparing chemical products, in particular to a method for preparing methylcyclopentadiene manganese tricarbonyl. technical background [0002] With the development of the automobile industry and the increasingly stringent requirements for environmental protection, methylcyclopentadiene manganese tricarbonyl (MMT for short) is increasingly favored by people as an efficient additive to increase the octane number, and has been recognized as the best choice for tetraethyl lead. good substitute. Since the advent of MMT, the synthesis process of methylcyclopentadiene manganese tricarbonyl has gone through four stages: (1) high temperature and high pressure two-step synthesis method; (2) normal temperature and pressure two-step synthesis method; (3) improved high temperature and high pressure Two-step synthesis method; (4) high temperature and high pressure one-step synthesis method. People continue to improve their sy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F17/00
Inventor 刘江宁于万鹏晋平
Owner HEBEI HUAGE FINE CHEM
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