Method for preparing naphthenic acid sample in wastewater

A naphthenic acid and sample technology, which is applied in the field of preparation of naphthenic acid samples in wastewater, can solve the problems that the extraction efficiency of naphthenic acid is difficult to evaluate, and the non-solvent organic carbon is difficult to measure, and achieves the effect of good purity

Active Publication Date: 2012-01-11
CHINA PETROLEUM & CHEM CORP +1
View PDF3 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for preparing naphthenic acid sample in wastewater
  • Method for preparing naphthenic acid sample in wastewater

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 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.

[0022] MSC H Form cation exchange resin 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 HCl and deionized wate...

Embodiment 2

[0026] The effluent of electric desalination biochemical treatment in a refinery was left to stand for 24 hours. After the suspended solids were fully settled, 15L of clear water from the upper layer was taken, and 63mg of macromolecular naphthenic acid solid samples and 462mg of small molecule solid samples were prepared according to the separation and pretreatment procedures of Example 1. . The contents of large molecule naphthenic acid and small molecule naphthenic acid in the electric desalination biochemical effluent of the refinery are 4.2mg / L and 40.8mg / L respectively.

Embodiment 3

[0028] The biochemical treatment of produced water produced by polymer flooding in an oilfield was left to stand for 24 hours. After the suspended solids were fully settled, 20 L of clear water from the upper layer was taken, and 84 mg of macromolecular naphthenic acid solid samples and small molecular solids were prepared according to the separation and pretreatment procedures in Example 1. Sample 336 mg. The contents of macromolecular naphthenic acid and small molecular naphthenic acid in the biochemically treated water produced by polymer flooding in this oilfield are 4.2 mg / L and 16.8 mg / L, respectively.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

PropertyMeasurementUnit
boiling pointaaaaaaaaaa
Login to view more

Abstract

The invention discloses a method for preparing a naphthenic acid sample in petroleum wastewater. The method comprises the following steps of: adjusting a wastewater sample to be acid, and adsorbing acid and neutral organic matters in the wastewater sample by using an adsorption resin column; backwashing the resin column subjected to adsorption by using alkali liquor, and eluting an acid organic matter; making a backwashing solution pass through an H-type cation exchange resin column, evaporating the passed solution in a rotating way, freeze-drying, and thus obtaining a small molecule naphthenic acid solid sample; and backwashing precipitates on the H-type cation exchange resin column by using the alkali liquor, adjusting the pH value of the backwashing solution to be less than or equal to 2 by using hydrochloric acid, standing, collecting the precipitates, and recycling a macromolecule naphthenic acid solid sample from the precipitates. By the method, the mass of the small molecule naphthenic acid solid sample or the macromolecule naphthenic acid solid sample is tested respectively to determine the content of the two samples in the wastewater, and the molecular weight and the structural features of naphthenic acid can be represented by an element analysis and solid 13C nuclear magnetic resonance method, a Fourier infrared spectrum method and an atmospheric pressure ionization mass spectrometry.

Description

technical field [0001] The invention relates to a separation and sample preparation method for determining naphthenic acid in waste water, which is suitable for the enrichment, separation and sample preparation of naphthenic acid in various oil refining or oilfield waste water, especially for the electric desalting waste water of oil refinery processing high-acid crude oil , Extraction and preparation of naphthenic acid in oilfield produced water for high-acid crude oil production, alkali-containing polymer flooding produced water and oil sand extraction bitumen process wastewater. The prepared samples can be used for naphthenic acid content, molecular weight distribution or structural 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...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/28G01N1/34
Inventor 李凌波
Owner CHINA PETROLEUM & CHEM CORP
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap