Purification method of acetonitrile
A purification method and acetonitrile technology, applied in the direction of carboxylic acid nitrile purification/separation, separation methods, chemical instruments and methods, etc., can solve problems such as unstable quality and increased concentration of impurities in the purified stream
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment
[0075] The present invention will be described in more detail below through examples, but the present invention is not limited to these examples.
[0076] The impurity concentration in acetonitrile was measured using a gas chromatograph, and the conditions at this time were as follows.
[0077] HP-6890 manufactured by Hewlett-Packard Company was used as a gas chromatograph, and DB-624 manufactured by Agilent Technologies Company was used as a column (60 m in length×0.32 mm in inner diameter, 5.0 μm in film thickness). An FID was used as a detector, and helium was used as a carrier gas.
[0078] The column temperature conditions are as follows.
[0079] Initial temperature: 70°C
[0080] Initial time: 10 minutes
[0081] Heating rate: 5.0°C / min
[0082] Intermediate temperature: 120°C
[0083] Post-run time (posttime): 10 minutes
[0084] Final temperature: 220°C
Embodiment 1
[0100] Such as figure 2 As shown, a reboiler 3b is added to the high boiling separation column 3, and the distilled steam from the product column 6 is circulated and utilized as a heat source. In addition, a steam drain tank (not shown) for storing steam drain generated in the reboiler 3b and a pump (not shown) for sending the steam drain in the tank to the condenser of the product column 6 are provided. Acetonitrile was purified using the same equipment as in Comparative Example 1 except for these.
[0101] Initially, the valve 6v to the condenser of the product column 6 is fully opened. The valve 6v was slowly closed over one week, and the heat supply to the reboiler 3b of the high boiling separation column 3 was increased. At the same time, the vapor in the reboiler 3a of the high boiling separation column 3 is reduced. Finally, the valve 6v is fully closed. At this time, the top pressure of the product column 6 (denoted as gauge pressure "A") is 0.0100MPaG, and the sh...
Embodiment 2
[0109] Except the distilled steam of product tower 6, also further utilize the distilled steam of low-boiling separation tower 5 as the heat source of reboiler 3c of high-boiling separation tower 3, except that, purify acetonitrile with the equipment same as embodiment 1 . The flow of the distillate steam of the low boiling separation tower 5 is as follows: image 3 shown.
[0110] Initially, the valve 5v leading to the condenser of the low boiling separation column 5 is fully opened. During the period when the valve 5v is fully opened, there is no process fluctuation, and the quality of the obtained acetonitrile is also no problem. The valve 5v was slowly closed over one week, and finally closed by 10% (90% open state). At this time, the pressure at the top of the low-boiling separation column 5 (denoted as gauge pressure "A") was 0.0172 MPaG, and the temperature at the top and bottom of the tower were 78.8°C and 86.4°C, respectively. The shell pressure of the reboiler 3c...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More