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Preparation method of deuterated ethylene

A technology of deuterated ethylene and deuterated acetylene, applied in the field of isotope gas preparation, can solve the problems of low utilization rate of raw materials, undisclosed reaction pressure, high price, etc., so as to improve the operation safety, improve the utilization rate of raw materials, and reduce the preparation cost. Effect

Active Publication Date: 2016-08-17
众宇氢能技术(荆州)有限公司
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Problems solved by technology

[0003] However, due to the key raw material heavy water (D 2 O) scarcity of resources and high price have restricted the production technology research of this compound. At present, there is no research report on the perfect deuterated ethylene production process in China, resulting in almost no deuterated ethylene commodity supply in the domestic market; the import of deuterated ethylene is also restricted. control, the import volume is very small, which seriously restricts the application range of deuterated ethylene
[0004] At present, the prior art discloses a preparation method of deuterated ethylene, deuterated acetylene (C 2 D. 2 ) Add deuterium gas (D in the presence of catalyst 2 ) generates deuterated ethylene, but it does not disclose the reaction pressure, and the proportion of by-product deuterated ethane is as high as 22%, the utilization rate of raw materials is low, and it is not suitable for large-scale industrial production
In addition, the acetylene hydrogenation process is mostly completed in the pressurized process, which requires high pressure resistance of the reaction equipment and high selectivity of the catalyst, which greatly increases the production cost

Method used

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  • Preparation method of deuterated ethylene
  • Preparation method of deuterated ethylene
  • Preparation method of deuterated ethylene

Examples

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Effect test

Embodiment 1

[0038] Carbide (CaC 2 ) and heavy water (D 2O) reacts as starting material, generates deuterated acetylene (C 2 D. 2 ); Deuterated acetaldehyde reacts with heavy water under acidic conditions to make high-content deuterated acetaldehyde (C 2 D. 4 O); with deuterated acetaldehyde and deuterium gas (D 2 ) is that raw material reacts with deuterium to make deuterated ethanol (C 2 D. 5 OD); The obtained deuterated ethanol is dehydrated by catalyst to obtain high-purity deuterated ethylene (C 2 D. 4 ). Based on heavy water, the total yield is greater than 41.51%.

[0039] The reaction principle is as follows:

[0040] Deuterated acetylene synthesis

[0041]

[0042] Synthesis of deuterated acetaldehyde

[0043] C 2 D. 2 +D 2 O→C 2 D. 4 o

[0044] Synthesis of deuterated ethanol

[0045]

[0046] Synthesis of deuterated ethylene

[0047]

[0048] Attached below Figure 1-3 The preparation process of deuterated acetaldehyde, deuterated ethanol and deuter...

Embodiment 2

[0050] In a specific embodiment, the step of synthesizing deuterated acetylene is as follows: put calcium carbide qualified for processing into the deuterated acetylene generator 101 in excess. Under the condition of 0~100℃, add D dropwise at a uniform speed 2 O, maintain the pressure in the acetylene reactor 101 at 0-0.5Mpa. The acetylene release rate is adjusted through the outlet valve of the acetylene generator 101.

Embodiment 3

[0052] In a specific embodiment, in order to improve the purity of acetylene, the deuterated acetylene from the acetylene generator 101 passes through the buffer tank 102 and the flow meter 103, and then passes through the neutralization tanks 104-106 sequentially, using D 2 O, D 2 SO 4 and Na 2 S 2 o 3 The deuterated acetylene is washed with the solution, and the dust, NH 3 , S, As and other impurities.

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Abstract

The invention discloses a preparation method of high-deuterated ratio deuteroethylene. According to the preparation method, calcium carbide is reacted with D2O to generate deuteroacetylene; the prepared deuteroacetylene is reacted with the D2O under an acidic condition to obtain deuteroacetaldehyde; the acetaldehyde is reacted with deuterium gas to obtain deuteroethanol; the deuteroethanol is catalytically dehydrated to obtain the deuteroethylene. The preparation method of the deuteroethylene is applicable to industrial production and has been verified in an industrial experimental facility having the annual output of 300kg; the products obtained in the steps of rections are high in purity; the reaction conditions are mild; the superfluous deuterium gas and D2O in the reactions can be recycled as the raw materials.

Description

technical field [0001] The invention relates to a method for preparing isotope gas, in particular to a method for preparing deuterated ethylene and its intermediate deuterated ethanol. Background technique [0002] Deuterated ethylene (C 2 h 4 ) is a special isotopic gas with special functions, which can be used as an intermediate for laser target materials, and is widely used in pharmaceutical synthesis, special engineering plastics and the construction of important national engineering projects. Its large-scale industrial production has very broad market prospects and extremely important social benefits. [0003] However, due to the key raw material heavy water (D 2 O) scarcity of resources and high price have restricted the production technology research of this compound. At present, there is no research report on the perfect deuterated ethylene production process in China, resulting in almost no deuterated ethylene commodity supply in the domestic market; the import o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C11/04C07C1/24
Inventor 余启富李骁刘英平
Owner 众宇氢能技术(荆州)有限公司
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