Anhydrous and anaerobic reaction device and application thereof

A water-free, oxygen-free, reaction device technology, applied in chemical/physical/physical-chemical stationary reactors, pressure vessels used in chemical processes, and methods of chemically changing substances by using atmospheric pressure, etc. Materials and liquid materials are added in batches, the quality of the anhydrous and oxygen-free environment is reduced, and the risk of damage to the reaction flask is increased, so as to improve the anhydrous and oxygen-free environment, high airtightness, and low damage rate.

Pending Publication Date: 2019-05-28
ZHENGZHOU UNIVERSITY OF LIGHT INDUSTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the existence of the three-way branch increases the risk of damage to the reaction bottle during the cleaning process, and the addition of solid materials and liquid materials in

Method used

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  • Anhydrous and anaerobic reaction device and application thereof
  • Anhydrous and anaerobic reaction device and application thereof
  • Anhydrous and anaerobic reaction device and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027]A reaction bottle for chemical anhydrous and oxygen-free reaction, the anhydrous and oxygen-free reaction bottle includes a bottle body 2 and a rubber stopper 3, the bottle body is eggplant-shaped, and the volume is 10 mL, 25 mL, 50 mL , 100 mL, 150 mL, 200 mL or 250 mL; the bottle stopper 3 is provided with an aluminum cover 4, the cover 4 is fastened at the mouth of the bottle, and there is a maximum reaction liquid level line 2 on the bottle; One side of the rubber stopper is a smooth plane 3-2, which is tightly fitted to the cover body, and the other side is provided with a hollow cylindrical protrusion 3-1, the outer diameter of the hollow cylindrical protrusion is the same as the inner diameter of the reaction bottle mouth. Fit to achieve a tight fit between the rubber stopper and the bottle mouth. The material of the rubber stopper has a small permanent deformation value and good resilience, and can withstand at least five insertions of the injection needle withou...

Embodiment 2

[0032] A water-free and oxygen-free reaction device comprising the water-free and oxygen-free reaction bottle, the water-free and oxygen-free reaction device also includes double-row pipes, one of the double-row pipes is connected to an inert gas cylinder, and the other branch pipe It is connected with a vacuum pump, and the two pipes of the double-row pipe are connected with a connecting pipe, and the connecting pipe is connected with a needle, and the needle passes through the rubber stopper at the through hole to communicate with the anhydrous and oxygen-free reaction bottle; the anhydrous anaerobic reaction bottle in this embodiment The oxygen reaction device also includes a sample injection syringe, the needle of the sample injection syringe communicates with the anhydrous and oxygen-free reaction bottle through the rubber stopper located at the through hole. The specific structure of the anhydrous and oxygen-free reaction flask of this embodiment is the same as that of em...

Embodiment 3

[0034] like Image 6 As shown, the application method of the anhydrous and oxygen-free reaction device in Example 2, the steps are as follows: for all liquid materials, first add a stirring magnet in the reaction bottle, plug the rubber stopper into the bottle mouth, and then under the action of external force Fasten the cap on the reaction bottle, insert one end of the needle into the rubber plug at the through hole of the cap, and connect the other end to the double-row tube through a connecting tube. One tube in the double-row tube is connected to the inert gas cylinder, and the other tube is Connect with the vacuum pump, rotate the valve on the double row pipe to connect the reaction bottle to the vacuum pump, evacuate the reaction bottle, burn the reaction bottle with flame at the same time, discharge the oxygen and water vapor in the reaction bottle, and then rotate the valve to make the reaction bottle Connect with the inert gas cylinder, fill the reaction bottle with i...

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PUM

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Abstract

The invention discloses an anhydrous and anaerobic reaction device and application thereof. The anhydrous and anaerobic reaction device comprises a reaction bottle, a rubber bottle plug and an aluminum cap; the rubber bottle plug and a bottleneck are tightly matched, the cap is arranged outside the bottle plug and buckled on the bottleneck, a through hole is formed in the middle of the aluminum cap, under the effect of external force, the aluminum cap can be fastened to the outer edge of the bottleneck of the reaction bottle, and thus a reaction system can withstand the high temperature and high pressure; and one face of the rubber bottle plug tightly makes contact with the cap, the outer diameter of a hollow rubber cylinder protruded on the other face of the rubber bottle plug is matchedwith the inner diameter of the bottleneck, thus the reaction bottleneck is sealed, an injector is directly applied to add a liquid material into the reaction bottle through the rubber plug without opening the bottleneck, and oxygen or vapor is prevented from entering in the adding process. The anhydrous and anaerobic reaction device is suitable for an anhydrous and anaerobic reaction under the normal temperature and normal pressure, and also suitable for an anhydrous and anaerobic reaction under the high temperature and high pressure; and a solid material and the liquid material can be added separately to avoid the situation that the anhydrous and anaerobic environment of the reaction system is damaged due to addition of the materials.

Description

technical field [0001] The invention belongs to the field of chemical synthesis equipment, in particular to a water-free and oxygen-free reaction device and its application. Background technique [0002] In recent years, anhydrous and oxygen-free reactions have been widely used in modern organic synthesis reactions. For example, the direct construction of unsaturated carbon-carbon bonds in the synthesis of small molecular compounds, due to the participation of organometallic catalysts, most of them need to be carried out under anhydrous and oxygen-free conditions. For reactions that require heating, the reaction device is required to have a certain high temperature and high pressure resistance. Properties (As Shengming. Modern organic synthesis reactions involving metals. Guangzhou: Guangdong Science and Technology Press, 2001: 1-258); in the synthesis of conjugated polymer materials, the content of oxygen in the reaction environment affects the molecular weight of polymer m...

Claims

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Application Information

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IPC IPC(8): B01J19/18B01J3/03B01J3/00
Inventor 杜俊平方少明陈庆涛韩光鲁周菁张华林田俊峰秦鹏举黄献
Owner ZHENGZHOU UNIVERSITY OF LIGHT INDUSTRY
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