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Method for measuring morphological distribution of C5 raw material and sulfide in fractions

A sulfide and analysis method technology, applied in the direction of material excitation analysis, material electrochemical variables, preparation of test samples, etc., can solve problems such as blank, complex sulfide form, difficult sulfide form, etc., and achieve good repeatability , high precision effect

Active Publication Date: 2009-10-14
SINOPEC LANZHOU GASOLINEEUM CHEM IND CORP
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Problems solved by technology

[0004] However, the sulfide forms in C5 raw materials and fractions are relatively complex, including mercaptans (mainly ethanethiol, isobutyl mercaptan, cyclopentyl mercaptan, n-octyl mercaptan), thioethers (mainly methyl sulfide , butyl sulfide, propyl sulfide), disulfides (including ethyl disulfide, butyl disulfide, bicyclohexyl disulfide, etc.) and thiophenes (mainly dimethylthiophene, trimethylthiophene) , it is difficult to analyze and determine the form of its sulfide
At present, the research on the analysis method of sulfide speciation distribution in C5 raw materials and fractions is still blank in China

Method used

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  • Method for measuring morphological distribution of C5 raw material and sulfide in fractions
  • Method for measuring morphological distribution of C5 raw material and sulfide in fractions
  • Method for measuring morphological distribution of C5 raw material and sulfide in fractions

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Embodiment Construction

[0022] C5 raw materials and fraction samples: Lanzhou Petrochemical Company.

[0023] Reagents: glacial acetic acid, sodium acetate, silver nitrate, isonewane, isopropanol (analytical grade, Tianjin Kemeo), nitrogen, oxygen, argon (Lanzhou Lizhong Gas Co., Ltd.).

[0024] The analysis method for the distribution of sulfide forms in C5 raw materials and fractions: including the following process steps:

[0025] (1) Determination of total sulfur content by ultraviolet fluorescence method

[0026] ①Working curve creation: use EA-3100 ultraviolet fluorescence instrument, set instrument parameters (combustion temperature 1050°C, flow rate of argon and oxygen respectively 120 and 100mL / min; injection speed 1μL / S, maximum integration time 360, baseline approximate value 25 , the threshold value is 100); 0.5-400 mg / L benzothiophene is selected as the sulfide standard sample, the abscissa is the absolute amount of sulfur (μg), and the ordinate is the peak area. The working curve is sh...

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Abstract

The invention provides a method for analyzing morphological distribution of C5 raw materials and sulfide in fractions; the method comprises the steps: firstly, an ultraviolet fluorescence method is adopted to measure the total sulfur content of a sample; secondly, a potentiometric titration method is used for measuring the sulfur content of sulfide hydrogen and mercaptan in the sample; thirdly, the sample is washed by silver nitrate solution, the ultraviolet fluorescence method is adopted to measure the total sulfur content of the washed sample; finally, the sulfur content of alkyl sulfide is converted by a subtration method; and a Zn-HAc reduction method is used for measuring the sulfur content of disulfide in the washed sample. The invention has the advantages of good repeatability and high precision, effectively solves the problem that the analysis of the sulfide morphology of the C5 raw materials and the sulfide in fractions is difficult due to the complex morphological distribution thereof, and provides technical data support for analyzing the desulfuration, equipment corrosion and the influence of different sulfur morphologies on the production processes.

Description

technical field [0001] The invention belongs to the technical field of petrochemical industry and relates to a method for measuring the form distribution of sulfides in C5 raw materials and fractions. Background technique [0002] C5 raw materials and fractions are very important chemical raw materials. The C5 hydrogenated solid functional resin obtained by separating and polymerizing the C5 fractions from ethylene cracking has low acid value, good miscibility, low melting point and good adhesion. , water resistance, ethanol resistance, chemical corrosion resistance and other characteristics, so it is widely used in rubber, adhesive tackifier and high solid content coatings, traffic paint, ink, paper and other industries. [0003] In the C5 hydrogenated petroleum resin unit, the determination of total sulfur and sulfur form distribution in C5 raw materials and fractions is a very important analysis content. Take desulfurization measures; in the device unit, especially befor...

Claims

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Application Information

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IPC IPC(8): G01N21/64G01N27/42G01N1/34
Inventor 邢龙春刘海生杨慧明俞燕龙刘沛温金萍朱殿军李延李婷胡庆和李斌
Owner SINOPEC LANZHOU GASOLINEEUM CHEM IND CORP
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