Synthesis method of malononitrile
A synthetic method and technology of malononitrile, applied in the fields of carboxylic acid nitrile purification/separation, organic chemistry, cyanide reaction preparation, etc., can solve problems affecting compound yield and quality, avoid hydrolysis or alcoholysis loss, and ensure High yield and quality, the effect of stable quality
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Examples
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...
PUM
| Property | Measurement | Unit |
|---|---|---|
| boiling point | aaaaa | aaaaa |
| flash point | aaaaa | aaaaa |
Abstract
Description
Claims
Application Information
Login to View More