Safe, environment-friendly and cheap method and device for producing deuterated aromatic ring compound

An aromatic ring compound, safe and environmentally friendly technology, applied in the fields of hydrocarbons, hydrocarbons, organic chemical methods, etc., can solve the problems of inability to commercialize production, expensive aromatic ring compounds, etc., to improve the utilization rate of deuterium and avoid volatilization. Loss, avoidance of effects on human injury and environmental pollution

Active Publication Date: 2020-05-05
XIAN RUILIAN NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Regardless of whether it is a single reaction or multiple reactions, a large amount of deuterium source is required, and the deuterium source itself is very expensive, so the obtained aromatic ring compound with high deuteration rate is more expensive and cannot be produced commercially in large quantities

Method used

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  • Safe, environment-friendly and cheap method and device for producing deuterated aromatic ring compound
  • Safe, environment-friendly and cheap method and device for producing deuterated aromatic ring compound
  • Safe, environment-friendly and cheap method and device for producing deuterated aromatic ring compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] see Figure 1-3As shown, a safe, environmentally friendly and inexpensive device for producing deuterated aromatic ring compounds provided by the embodiment of the present invention includes an autoclave R101 for deuteration reaction, a liquid separation tank V101 for liquid separation treatment, and a liquid separation tank V101 for the reaction The enamel still R102 for distillation treatment of the final organic phase, the rectification device for the rectification operation of the reaction liquid, the receiving bottle V102 for receiving the product after rectification, and the heat exchange device for providing heat transfer medium,

[0041] The top of the autoclave R101 is equipped with a material inlet and an inert gas inlet. The liquid outlet of the autoclave R101 is connected to the liquid separation tank V101 through the pressure filter F101. The liquid outlet is provided with a control valve, the bottom of the control valve is provided with an aqueous phase li...

Embodiment 2

[0065] The difference from the above examples is that the equipment for avoiding product volatilization loss and the experimental scheme for recovering deuterated heavy water are used at the same time. The specific operation steps are as follows:

[0066] Preparation of the second batch of deuterated benzene:

[0067] The first reaction: In the 2000L R101 autoclave, add recovered heavy water (1), catalyst 10% Pd / C 36kg and benzene 528Kg. After the feeding is completed, the autoclave R101 is sealed, stirred and heated to 180°C for reaction, and kept at 180°C for 4 hours. Turn off the heating, and cool down to 15°C through the V103 oil tank cold oil. Open the discharge valve, under stirring, use nitrogen gas to press the reaction solution from the discharge port into the 2000L V101 liquid separation tank through the F101 pressure filter, and the pressure filtration is completed. Close the nitrogen inlet valve and outlet valve, and open the vent valve of the 2000L R101 autoclave...

Embodiment 3

[0078] The difference from the above examples is that the equipment for avoiding product volatilization loss and the experimental scheme for recovering deuterated heavy water are used at the same time. The specific operation steps are as follows:

[0079] Preparation of the third batch of deuterated benzene:

[0080] The first reaction: in the 2000L R101 autoclave, add reclaimed heavy water (8), catalyst 10%Pd / C 36kg and benzene 528Kg. After the feeding is completed, the autoclave R101 is sealed, stirred and heated to 180°C for reaction, and kept at 180°C for 4 hours. Turn off the heating, and cool down to 15°C through the V103 oil tank cold oil. Open the discharge valve, under stirring, use nitrogen gas to press the reaction solution from the discharge port into the 2000L V101 liquid separation tank through the F101 pressure filter, and the pressure filtration is completed. Close the nitrogen inlet valve and outlet valve, and open the vent valve of the 2000L R101 autoclave...

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Abstract

The invention provides a safe, environment-friendly and cheap method and device for producing a deuterated aromatic ring compound. The device is mainly composed of a reaction system, a post-treatmentsystem, a rectification system and a heat exchange system. By adopting the device, the yield of the deuterated aromatic ring compound can be increased to 95%, and the cost is reduced to 74.74% of theoriginal cost. For a product with stronger volatility under lower boiling point, the effect is more obvious when the device is used. Therefore, after the device is used, the volatilization loss of theproduct can be avoided, the cost is reduced, meanwhile, personnel harm and environmental pollution caused by volatilized toxic deuterated aromatic ring compounds are basically avoided, and the problems of safety and environmental protection cost are solved. According to the method, the product yield is increased, the heavy hydrogen utilization rate is increased and the catalyst is recycled and reused through a set of designed equipment and experimental scheme, finally, the aromatic ring compound with the high deuteration rate can be produced, and in industrial production, along with increaseof production batches, the cost can be further saved, and the yield is increased.

Description

technical field [0001] The invention relates to the technical field of preparation of deuterated aromatic ring compounds, in particular to a method and device for producing deuterated aromatic ring compounds in a safe, environment-friendly and cheap manner. Background technique [0002] Deuterated aromatic ring compounds have been used to study chemical reactions and substance metabolism, and are widely used to track and label compounds. In addition, the deuterated compounds are changed due to their own stability and properties. Therefore, deuterated compounds are usually widely used in the fields of medicine, pesticides, organic EL materials (Organic Electro-Luminescence) and the like. [0003] Studies have shown that some deuterated electroluminescent materials, compared with their non-deuterated isomers, show the characteristics of improving the efficiency and life of the material, such as: Lecloux, et al.PCT Int.Appl. (2010), WO2010114583A1 20101007 and Tong, et al. J. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C7/04C07C5/00C07C15/04C07B59/00B01D3/00B01J8/10B01J3/04
CPCC07C7/04C07C5/00C07B59/00B01D3/009B01J8/10B01J3/04C07B2200/05C07C15/04Y02P20/52Y02P20/584
Inventor 王震冯光军何汉江崔磊磊王毅赵佳宁宋辉王小伟
Owner XIAN RUILIAN NEW MATERIAL CO LTD
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