Identification and separation of the organic compounds in coal-gasification condensate waters. [5,5 dimethyl hydantoin, dihydroxy benzenes, acetonitrile]

Technical Report · Mon Aug 01 04:00:00 EDT 1983

DOI:https://doi.org/10.2172/5878653· OSTI ID:5878653

Mohr, Jr., D. H.; King, C. J.

A substantial fraction of the organic solutes in condensate waters from low-temperature coal-gasification processes are not identified by commonly employed analytical techniques, have low distriution coefficients (K/sub C/) into diisopropyl ether (DIPE) or methyl isobutyl ketone (MIBK), and are resistant to biological oxidation. These compounds represent an important wastewater-treatment problem. Analytical techniques were developed to detect these polar compounds, and the liquid-liquid phase equilibria were measured with several solvents. A high-performance liquid - chromatography (HPLC) technique was employed to analyze four condensate-water samples from a slagging fixed-bed gasifier. A novel sample-preparation technique, consisting of an azeotropic distillation with isopropanol, allowed identification of compounds in the HPLC eluant by combined gas chromatography and mass spectrometry. 5,5-dimethyl hydantoin and related compounds were identified in condensate waters for the first time, and they account for 1 to 6% of the chemical oxygen demand (COD). Dimethyl hydatoin has a K/sub D/ of 2.6 into tributyl phosphate (TBP) and much lower K/sub D/ values into six other solvents. It is also resistant to biological oxidation. Phenols (59 to 76% of the COD), dihydroxy benzenes (0.02 to 9.5% of the COD), and methanol, acetonitrile, and acetone (15% of the COD in one sample) were also detected. Extraction with MIBK removed about 90% of the COD. MIBK has much higher K/sub D/ values than DIPE for dihydroxy benzenes. Chemical reactions occurred during storage of condensate-water samples. The reaction products had low K/sub D/ values into MIBK. About 10% of the COD had a K/sub D/ of nearly zero into MIBK. These compounds were not extracted by MIBK over a wide range of pH. 73 references, 6 figures, 35 tables.

• Research Organization: Lawrence Berkeley Lab., CA (USA)
• DOE Contract Number: AC03-76SF00098
• OSTI ID: 5878653
• Report Number(s): LBL-15869; ON: DE83017520
• Country of Publication: United States
• Language: English

Related Subjects

01 COAL, LIGNITE, AND PEAT
010404 -- Coal
Lignite
& Peat-- Gasification
010600* -- Coal
Lignite
& Peat-- Properties & Composition
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
400104 -- Spectral Procedures-- (-1987)
400105 -- Separation Procedures
ACETONE
ALCOHOLS
AROMATICS
BUTYL PHOSPHATES
CHEMICAL ANALYSIS
CHEMICAL OXYGEN DEMAND
CHROMATOGRAPHY
COAL GASIFICATION PLANTS
CONDENSATES
DATA
ESTERS
ETHERS
EXPERIMENTAL DATA
EXTRACTION
GAS CHROMATOGRAPHY
HYDROGEN COMPOUNDS
HYDROXY COMPOUNDS
INDUSTRIAL PLANTS
INFORMATION
KETONES
LIQUID COLUMN CHROMATOGRAPHY
LIQUID WASTES
MASS SPECTROSCOPY
METHANOL
NUMERICAL DATA
ORGANIC COMPOUNDS
ORGANIC OXYGEN COMPOUNDS
ORGANIC PHOSPHORUS COMPOUNDS
OXYGEN COMPOUNDS
PHENOL
PHENOLS
PHOSPHORIC ACID ESTERS
POLAR COMPOUNDS
SAMPLE PREPARATION
SEPARATION PROCESSES
SOLVENT EXTRACTION
SPECTROSCOPY
TBP
TOPO
WASTE WATER
WASTES
WATER