ABSTRACT
The initial substances for the synthesis of quaternary ammonium salts were hexamethylenetetramine, N ,N' -tetramethyldiaminomethane, piperidine, morpholine, methyl chloride and corresponded production wastes (tertiary butyl chloride, allyl halides - 1 ,3-dich1oro-2-methylpropenes (cis-, trans-isomers)) and 3-chloro-2-chloromethylpropene, which were extracted from the DDB fraction of the following composition:
Component 2-chloro-2-methylpropene (isocrotyl chloride) 3-chloro-2-methylpropene (methally I chloride) 1 ,2-dichloro-2-methylpropane Heavy (1,2,3-trichloro-2-methylpropane, etc.) Dichloroisobutylenes, including: 1 ,3-dichloro-2-methylpropene, cis1 ,3-dichloro-2-methylpropene, trans3-dichloro-2-chloromethylpropene
Content, wt.% 1.21 1.57
50.62 6.34
40.26 7.62 10.38 22.26
Individual allyl halides were extracted from the DDB composition with purity 96 wt.% or higher in a laboratory column of OB-508 type possessing the following parameters:
Cylindrical part height, m Diameter, m Number of theoretical plates Static capacity, ml Dynamic capacity, ml Boiling rate (max), kglh Maximal temperature of distillation, °C
1.55 0.015-0.019
24 24 24
15.5 200
Qualitative and quantitative analysis of extracted compounds was carried out using gas-liquid chromatography on chromatograph LCM-80. Mixture separation was performed in a chromatographic column possessing the following parameters:
Column length, m Carrier Phase Gas-carrier
Running mode of the chromatograph:
Desiccator temperature, oc Detector temperature, oc Thermostat temperature, oc Gas-carrier rate, 1/h Sample dose, J.ll
2.6 chromaton N-A W (0.2 - 0.35 mm)
SCTPT-50C nitrogen
180 160 160 30
0.2
The required volume of the substance for analysis is sampled by a microsyringe and then injected to the chromatographic column.