chapter  II
3. Experimental
Pages 12

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


The required volume of the substance for analysis is sampled by a microsyringe and then injected to the chromatographic column.