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Preparation method of isotope 13C-marked aldehyde

An isotope and acetaldehyde technology, which is applied in the field of preparation of isotope 13C-labeled acetaldehyde, can solve the problems of high temperature requirements, low acetylene yield and low purity, and achieves the effects of optimizing the process, optimizing the synthesis route, and being easy to prepare.

Inactive Publication Date: 2010-07-07
SHANGHAI RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process is suitable for the production of acetylene on an industrial scale. The device has high temperature requirements, and the yield and purity of acetylene are low, so it is not suitable for the synthesis of isotope-labeled acetylene.

Method used

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  • Preparation method of isotope 13C-marked aldehyde
  • Preparation method of isotope 13C-marked aldehyde
  • Preparation method of isotope 13C-marked aldehyde

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] an isotope 13 The preparation method of C mark acetaldehyde, the method comprises the following steps:

[0031] (1) Active metal and carbon dioxide generate metal carbide: adopt such as figure 1 The shown reactor includes a screw clamp 1, a stop valve 2, a heating reactor 3, and a vacuum gauge 4. Accurately weigh 15.6g (2.25mol) of lithium metal (purity higher than 99.9%), and release it quickly under the protection of argon. into the heating reactor 1, vacuumize after airtight and raise the temperature to 1200°C, open the screw clamp and start to feed 0.30mol 13 CO 2 , 13 CO 2 by Ba 13 CO 3 Quantitatively converted to get, 13 C abundance 99atom%. Observe the vacuum gauge 4, and control the vacuum degree in the heating reactor 1 through the stop valve 3 to keep it at -0.05~-0.1MPa, and pass it in about 4 hours 13 CO 2 , naturally cooled to room temperature after the reaction to obtain carbide of metal lithium.

[0032] (2) Hydrolysis of metal carbides to gene...

Embodiment 2

[0035](1) Active metals and carbon dioxide form metal carbides: Weigh 5.47g (0.225mol) of magnesium metal, quickly put it into the heating reactor under the protection of argon, vacuumize after sealing, and slowly raise the temperature. When the temperature reaches 500-700 ℃ stop vacuuming, continue to heat up to 600 ℃, open the screw clamp and feed 0.225molCO 2 , observe the vacuum gauge, control the vacuum degree in the heating reactor at -0.05~-0.1MPa through the stop valve, and pass the CO in about 10 hours 2 , After the reaction is completed, it is naturally cooled to 20°C to obtain carbides of metallic magnesium.

[0036] (2) Hydrolysis of metal carbides to generate acetylene: connect the reactor in step (1) to the hydrolysis reactor, turn on the vacuum pump and use the stop valve to control the vacuum degree of the system at 0.05Mpa, slowly add about 2L of deionized water dropwise, the The generated acetylene was absorbed by a cold trap with a temperature of -30°C, and...

Embodiment 3

[0039] Step (1) is the same as step (2) and embodiment 1, prepare catalyst mother liquor according to following ratio in step (3): HgSO 4 (6.0g, 0.02mol), concentrated H 2 SO 4 (12.2g, 0.124mol) and deionized water (100ml, 5.55mol), while adding ferric sulfate (4.0g, 0.01mol) as a cocatalyst.

[0040] Vacuumize the reaction system, replace it with argon three times, feed 0.223mol acetylene, and keep the reaction temperature at 85°C. Under the action of a constant flow pump, acetylene gas bubbles into the reaction vessel first, and acetaldehyde is generated in the reaction vessel, and the product acetylene The aldehyde enters the reflux condenser and the alcohol-liquid nitrogen cold trap along with the unreacted acetylene, and the acetaldehyde is collected in the cold trap, and the unreacted acetylene enters the reactor again to continue the reaction until the amount of acetaldehyde produced no longer increases. After the reaction is complete, get 13 C labeled anhydrous acet...

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Abstract

The invention relates to a preparation method of isotope 13C-marked aldehyde. The method includes the following steps that firstly, metallic carbide is generated by active metal and carbon dioxide, namely, the active metal is put in a reactor, the vacuum degree and the temperature of the reactor are controlled, 13 carbon dioxide and the active metal are put in the reactor to generate the metallic carbide; secondly, the metallic carbide is hydrolyzed to generate acetylene, and the by-product hydrogen is discharged by a vacuum pump; the acetylene is catalyzed and hydrated to generate aldehyde, namely, a catalyst system is added to the reactor provided with a cold trap and a constant flow pump and then hydrated to generate the 13C-marked aldehyde which is liquefied in the cold trap and collected. Compared with the prior art, the invention selects proper synthetic precursors, self-designs the reactor and optimizes synthetic path and technique. The method has a simple process, the preparation is easy, the purity of the product aldehyde is more than 99 percent, and the abundance of the isotope 13C is equal to or more than 98 atom percent.

Description

technical field [0001] The present invention relates to a kind of preparation method of acetaldehyde, especially relate to a kind of isotope 13 The preparation method of C labeled acetaldehyde. Background technique [0002] Carbon-13 (referred to as 13 C, the same below) is a stable isotope of carbon, and its natural abundance is 1.108 atom%. Since the 1950s, with the breakthrough of stable isotope separation technology and the rapid development of testing instruments, 13C stable isotope has the characteristics of no radiation damage to the human body, so it can be used as a tracer, widely used in organic chemistry, biological Chemistry, medicine and clinical diagnosis, pharmacology, agricultural science and other fields are of great significance especially to the fields of life science research and food safety. [0003] Due to the expensive raw materials, small yields, and high requirements for purity and abundance of such products, there are also special requirements fo...

Claims

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Application Information

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IPC IPC(8): C07C47/06C07C45/26
Inventor 罗勇谭树波李美华
Owner SHANGHAI RES INST OF CHEM IND
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