Method for separating low-concentration naphthenic acid in wastewater and preparing naphthenic acid sample

A naphthenic acid, low-concentration technology, applied in the field of separation and sample preparation of low-concentration naphthenic acid in wastewater, can solve problems such as difficulty in evaluating the extraction efficiency of naphthenic acid and difficult determination of non-solvent organic carbon, and achieve good purity Effect

Active Publication Date: 2012-01-11
CHINA PETROLEUM & CHEM CORP +1
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Problems solved by technology

[0007] Solvent extraction method is difficult to prepare sufficient amount of high-purity samples from low-concentration naphthenic acid wastewater for comprehensive spectroscopic characterization of naphthenic acid. Due to the difficulty in determining non-solvent organic carbon in water samples after solvent extraction, the extraction efficiency of naphthenic acid also difficult to assess

Method used

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  • Method for separating low-concentration naphthenic acid in wastewater and preparing naphthenic acid sample
  • Method for separating low-concentration naphthenic acid in wastewater and preparing naphthenic acid sample

Examples

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Embodiment 1

[0026]Amberlite DAX-8 resin (SUPELCO) was soaked with 0.1mol / L NaOH for 24h, and then washed with deionized water to remove residual NaOH. The washed resin was sequentially extracted by Soxhlet with dichloromethane, acetone and methanol for 16 hours. Put the purified 800mL DAX-8 resin into a glass column with a length of 700mm and an inner diameter of 40mm, and the two ends of the glass column are fixed with glass wool. Next, wash with deionized water, 0.1mol / L NaOH, deionized water, 0.1mol / L HCl and deionized water in sequence until the total organic carbon (TOC) of the eluate is lower than 1.0mg / L.

[0027] MSC H Form cation exchange resin (MTO-Dowex Marathon) was Soxhlet extracted with methanol for 16h and stored in methanol. About 800mL of purified MSC H Form cation exchange resin was loaded into a glass column with the same specifications as the DAX-8 resin column. The resin column was washed sequentially with deionized water, 0.1mol / L NaOH, deionized water, 0.1mol / L HC...

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Abstract

The invention discloses a method for separating low-concentration naphthenic acid in wastewater and preparing a naphthenic acid sample. The method comprises the following steps of: concentrating a dissolvable organic matter in the wastewater by using a reverse osmosis device; adjusting the pH value of reverse osmosis concentrated solution to be acid, and allowing the reverse osmosis concentrated solution to pass through an adsorption resin column to adsorb acid and neutral organic matters in the concentrated solution; backwashing the adsorption resin column by using alkali liquor; allowing the backwashing solution to pass through an H-type cation exchange resin column; putting the passed solution into a dialysis bag, and dialyzing in hydrofluoric acid solution for desilicification; evaporating in a rotating way, freeze-drying, and thus obtaining a small molecule naphthenic acid solid sample; backwashing precipitates on the H-type cation exchange resin column by using the alkali liquor; acidifying the backwashing solution, standing and collecting the precipitates; and filtering the precipitates, washing, centrifuging, freeze-drying, and thus obtaining a macromolecule naphthenic acid solid sample. By the method, the naphthenic acid can be separated from low-concentration naphthenic acid-containing wastewater, the recovery rate of the naphthenic acid is not less than 80 percent, and the prepared naphthenic acid samples have higher purity and are suitable for representation of various kinds of spectroscopy.

Description

technical field [0001] The invention relates to a method for the separation and sample preparation of low-concentration naphthenic acid in petroleum industry wastewater, which is suitable for the enrichment, concentration, separation and sample preparation of naphthenic acid in various oil refining or oilfield wastewater, and is especially suitable for biochemical treatment of oil refining or oilfield wastewater Extraction and preparation of naphthenic acid with lower concentration in effluent, the prepared sample can be used for naphthenic acid content, molecular weight distribution or structure characterization. Background technique [0002] Naphthenic acid is a complex mixture of alkyl-substituted acyclic or alkyl-substituted alicyclic carboxylic acids. It is a natural component of petroleum and can enter oilfield produced water or refinery wastewater through crude oil production and processing, such as the production of high-acid Oilfield produced water from crude oil, p...

Claims

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Application Information

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IPC IPC(8): G01N1/28G01N1/34G01N1/40
Inventor 李凌波
Owner CHINA PETROLEUM & CHEM CORP
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