A kind of synthetic method of malononitrile
A synthesis method and technology of malononitrile, applied in the fields of purification/separation of carboxylic acid nitrile, organic chemistry, cyanide reaction preparation, etc., can solve the problems affecting the yield and quality of compounds, and avoid hydrolysis or alcoholysis loss, quality Stable and ensure high yield and quality effect
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Embodiment 1
[0035] Add 1200g of methylene bromide, 30g of DMSO, 15g of sodium iodide, and 650g of NaCN successively in the pressure reactor, seal the pressure reactor, and pass N 2 Replace the system, raise the temperature to 140°C under stirring, and wait for the temperature and pressure of the system to be stable, and then react for 16 hours with a heat preservation timer.
[0036] After the reaction was finished, the temperature was lowered, the solid and liquid were separated, and the solid sodium bromide was recovered. The filtrate was collected in a rectifying bottle, and directly carried out rectification under reduced pressure. The front fraction was collected separately for use, and 410.2 g of the normal fraction collected at 85 to 95 ° C (4 to 8 mmHg) was the target product malononitrile. The rate is 93.64%. The purity of the product was determined to be 99.52% by GC method.
[0037] With FT-IR and 1 H-NMR characterizes the product structure. where FT-IR σ / cm -1 : 2965(vs, ...
Embodiment 2
[0039] In the pressure reactor, add methylene chloride 500g, DMI 25g, potassium iodide 12g, KCN 725g successively, airtight pressure reactor, logical N 2Replace the system, raise the temperature to 155°C under stirring, and wait for the temperature and pressure of the system to be stable, then keep warm and react for 12 hours.
[0040] After the reaction is finished, the temperature is lowered, the solid and liquid are separated, and the solid potassium chloride is recovered. The filtrate was collected in a rectifying bottle, and directly carried out rectification under reduced pressure. The front fraction was collected separately for use, and 334.8 g of the positive fraction collected at 85-95 ° C (4-8 mmHg) was the target product malononitrile. The rate is 91.04%. The purity of the product was determined to be 99.36% by GC method.
[0041] FT-IR with 1 The H-NMR characterization results are the same as in Example 1.
Embodiment 3
[0043] The former fraction collected in Example 1 is added in the pressure reactor, and dibromomethane 1200g, sodium iodide 15g, NaCN 650g are added successively, and the pressure reactor is closed, and N 2 Replace the system, raise the temperature to 140°C under stirring, and wait for the temperature and pressure of the system to be stable, and then react for 18 hours with a heat preservation timer.
[0044] After the reaction was finished, the temperature was lowered, the solid and liquid were separated, and the solid sodium bromide was recovered. The filtrate was collected in a rectifying bottle, and directly subjected to vacuum distillation. The first fraction was collected for use, and 415.4 g of the normal fraction at 85-95°C (4-8mmHg) was collected, which was the target product, malononitrile, with a yield of 94.83%. . The purity of the product was determined to be 99.41% by GC method.
[0045] FT-IR with 1 The H-NMR characterization results are the same as in Exampl...
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Abstract
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