Preparation method of deuteroethylene

A technology of deuterated ethylene and deuterated acetylene, which is applied in the field of isotope gas preparation, can solve the problems of restricting compound production technology research, high price, low conversion rate of deuterated ethylene, etc., and meets the requirements of equipment pressure resistance and is basically pollution-free and equipment. Low pressure resistance requirements and the effect of improving the utilization rate of raw materials

Active Publication Date: 2015-06-10
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] Currently, the prior art discloses deuterated acetylene (C 2 D. 2 ) plus deuterium (D 2 ) generates deuterated ethylene, yet it does not disclose the reaction pressure, and the proportion of by-product deuterated ethane is as high as 22%, and heavy water (D 2 O) low conversion to deuterated ethylene, not suitable for large-scale industrial production

Method used

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  • Preparation method of deuteroethylene

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Experimental program
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Embodiment 1

[0026] Carbide (CaC 2 ) and heavy water (D 2 O) reacts as starting material, generates deuterated acetylene (C 2 D. 2 ); deuterated acetylene in Cu-Ni / SiO 2 Under the catalysis of composite catalyst and deuterium gas (D 2 ) carries out deuterium addition reaction and makes deuterated ethylene (C 2 D. 4 ), the deuterated acetaldehyde and deuterium gas are in a volume ratio of 1:10 to 60.

[0027] In a specific embodiment, Cu-Ni / SiO 2 The active metal accounts for 1.75-2.00wt% of the total amount of oxides in the composite catalyst. In a specific embodiment, Cu-Ni / SiO 2 The composite catalyst is activated at high temperature (300-650°C, for example, 400°C). Those skilled in the art know that the above ratios and temperatures are not intended to limit the present invention, and their specific contents and temperatures can be adjusted according to actual needs.

[0028] The reaction principle is as follows:

[0029] Deuterated acetylene synthesis

[0030]

[0031] T...

Embodiment 2

[0038] 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

[0040] 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 deuteroethylene. According to the preparation method, calcium carbide is reacted with D2O to generate deuteroacetylene; a deuteration reaction is performed on the prepared deuteroacetylene and deuterium gas in the presence of a composite catalyst Cu-Ni/SiO2 to obtain the deuteroethylene; the volume ratio of the deuteroacetylene to the deuterium gas is 1: (10-60). The preparation method of the deuteroethylene is applicable to industrial production and has been verified and utilized in an industrial pilot plant already; experimental results prove that the preparation method has the advantages of simple reaction steps, mild reaction conditions, high deuteroethylene yield, recyclability of superfluous deuterium gas in the reaction as the raw material, and great reduction of the production cost.

Description

technical field [0001] The invention relates to a method for preparing isotope gas, in particular to a method for preparing deuterated ethylene. 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 of deuterated ethylene is also restricted...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C5/09C07C11/04C07C5/08C07C9/06C07B59/00
CPCY02P20/52
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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