A method for realizing anhydrous and oxygen-free operation and a process for producing cyclomanganese reaction of methylcyclopentadienyl manganese using the method

A technology of methylcyclopentadienyl manganese and an operation method is applied in the field of cyclomanganese reaction production technology of methylcyclopentadienyl manganese, which can solve the problems of large nitrogen consumption, economic loss and high energy consumption, and achieves Improve the success rate of the reaction, good economic benefits, and simple operation

Active Publication Date: 2016-01-20
山东东昌精细化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main reason is that the pressure in the kettle changes slightly due to the materials entering and leaving the reactor, and even the temperature of the kettle fluctuates greatly due to the mixing of hot and cold materials. At this time, the air outside the kettle will "suck back" into the kettle along the part that communicates with the air (such as the venting line of the reactor), so that the number of replacements needs to be increased, the consumption of nitrogen is relatively large, and the energy consumption is also high.
In actual production, operators are often unaware of the "suck back" air in the kettle, resulting in reaction failure, affecting the normal operation of industrial devices, and causing huge economic losses

Method used

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  • A method for realizing anhydrous and oxygen-free operation and a process for producing cyclomanganese reaction of methylcyclopentadienyl manganese using the method
  • A method for realizing anhydrous and oxygen-free operation and a process for producing cyclomanganese reaction of methylcyclopentadienyl manganese using the method

Examples

Experimental program
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Effect test

Embodiment 1

[0031] A kind of cyclomanganese reaction production technique of methylcyclopentadienyl manganese, its processing step is as follows:

[0032] (a) After the ring manganese reaction in the reactor 3 is completed, a certain amount of high-purity nitrogen gas is filled into the reactor, and after the pressure in the reactor rises to 0.2-0.3 MPa, the discharge valve of the reactor is opened, and the reaction liquid is discharged from the discharge pipeline 1. Discharge the reaction kettle 3 until the reaction kettle is emptied and the pressure drops to a slight positive pressure, then close the discharge valve and keep the reaction kettle with a slight positive pressure and a nitrogen atmosphere, ready to enter the next ring manganese reaction cycle;

[0033] (b) Fill the kettle with micro-flow high-purity nitrogen through the small-range flowmeter 6 and the inert gas inlet line 7, and the small-range rotameter 6 controls the flow rate of the micro-flow high-purity nitrogen at 70 l...

Embodiment 2

[0037] A cyclomanganese reaction production process of methylcyclopentadienyl manganese, on the basis of keeping other steps and process parameters unchanged in Example 1, only the inert gas is changed from high-purity nitrogen to helium.

example 3-10

[0039] A ring manganese reaction production process of methylcyclopentadienyl manganese, on the basis of embodiment 1, keep other steps and process parameters unchanged, the only difference is that the micro positive pressure single call valve 8 adopts different opening pressures (i.e. different micro positive pressure control ranges) and the small range rotameter 6 adopts different micro flow rates, see Table 1 for details.

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Abstract

The invention relates to a method for realizing anhydrous anaerobic operation and a ring manganese reaction production process of methyl cyclopentadienyl manganese by the method. The method comprises the following steps: (1) arranging a micro-positive pressure breather valve on a venting pipeline of a reaction still, and injecting inert gas to keep the micro-positive pressure state in the reaction still before feeding, wherein the gauge pressure of the micro-positive pressure is not greater than 400 Kpa; and (2) filling the reaction still with micro-flow inert gas through a small-range flowmeter, and opening a charging hole for charging, wherein inert gas always flows out of the still, and the flow of inert gas is controlled within 20-200 L / minute. According to the method, the reaction still is capable of using inert gas as less as possible and completing material charging and discharging under the protection of inert gas, so that the risk of reaction failure is decreased.

Description

technical field [0001] The invention relates to the field of fine chemical production, and more specifically relates to a method for realizing anhydrous and oxygen-free operation and a cyclomanganese reaction production process of methylcyclopentadienyl manganese using the method. Background technique [0002] Many substances, especially some substances synthesized by humans, are sensitive to air, that is, unstable to oxygen and moisture in the air, such as alkali metals, organic alkali metals, free radicals, anaerobic organisms, cyclopentadienyl Manganese, methylcyclopentadienyl manganese, etc. Therefore, if these compounds are involved in research and production, such as in the production of MMT (ie: methylcyclopentadiene manganese tricarbonyl) and CMT (ie: cyclopentadiene manganese tricarbonyl), it is necessary to produce Operate under oxygen conditions. [0003] In the case of ensuring that the reaction material does not contain water, three methods are currently used ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J19/14C07F17/00
Inventor 司志华吕家鑫杨飞飞孙海洋于娜
Owner 山东东昌精细化工科技有限公司
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