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Method for determining total chlorine content in direct coal liquefaction product

A technology of direct coal liquefaction and total chlorine content, which is applied in the field of analytical chemistry, can solve problems such as inaccurate determination of total chlorine content, and achieve the effects of complete absorption, high analysis accuracy, and high conversion efficiency

Inactive Publication Date: 2013-12-18
CHNA ENERGY INVESTMENT CORP LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention aims to provide a method for measuring the total chlorine content in direct coal liquefaction products to solve the technical problem of inaccurate determination of total chlorine content in direct coal liquefaction products in the prior art

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1) Take 0.2237g of standard chlorine aqueous solution (the chlorine content per gram of standard chlorine aqueous solution is 100.1715μg), put it into a high-temperature combustion furnace and burn for 30 minutes, and the furnace temperature is set at 1500°C to obtain combustion tail gas.

[0026] 2) Pass the combustion tail gas into an aqueous solution of sodium bicarbonate with a mass percentage concentration of 2% (after chlorine removal treatment) under the drive of oxygen, and fully absorb it to obtain the sample to be tested, in which the flow rate of oxygen is 0.1ml / min.

[0027] 3) Send the sample to be tested into the ion chromatographic analyzer, repeat the measurement 3 times, take the average value, and determine the total chlorine content per gram of standard chlorine aqueous solution to be 100.0538μg.

[0028] Visible adopt method of the present invention to measure standard aqueous solution of chlorine, measure the average content of total chloride ion to ...

Embodiment 2

[0030] 1) Take 0.1332g of standard oil (the chlorine content per gram of standard oil is known to be 10μg), put it into a high-temperature combustion furnace and burn for 10 minutes, and the furnace temperature is set at 900°C to obtain combustion tail gas.

[0031] 2) Pass the combustion tail gas into deionized water without chlorine ions under the drive of oxygen, fully absorb it, and obtain the sample to be tested. The flow rate of oxygen is 1.0ml / min.

[0032] 3) Send the sample to be tested into the ion chromatography analyzer, repeat the measurement 3 times, take the average value, and determine the total chlorine content per gram of the standard oil product to be 10.9925 μg.

[0033] It can be seen from the data comparison that the assay method of the present invention has high accuracy and simple operation.

Embodiment 3

[0035] 1) Take 0.1134g of coal liquefaction residue A, put it into a high-temperature combustion furnace and burn it for 10 minutes, and set the furnace temperature to 1400°C to obtain combustion tail gas.

[0036] 2) Pass the combustion exhaust gas into the ammonium bicarbonate solution without chloride ions with a mass percentage concentration of 2% under the drive of oxygen, and fully absorb it to obtain the sample to be tested; the flow rate of oxygen is 0.05ml / min.

[0037] 3) Send the sample to be tested into the ion chromatography analyzer, repeat the measurement 3 times, take the average value, and determine the total chlorine content in each gram of coal liquefaction residue A is 197.4138μg.

[0038]4) Add spectroscopically pure sodium chloride with an equivalent chlorine content of 100.1526 μg to each gram of coal liquefaction residue A, repeat the above steps for testing, take the average value of three measurements, and determine the total chlorine content in each g...

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Abstract

The invention discloses a method for determining total chlorine content in a direct coal liquefaction product. The method comprises the following steps: S1, combusting the direct coal liquefaction product at 900-1500 DEG C for 10-60 minutes; introducing combustion tail gas into an absorption solution to be absorbed sufficiently to obtain a sample to be detected; and S2, conveying the sample to be detected into an ion chromatographic analyzer to be determined to obtain the total chlorine content in the direct coal liquefaction product. The method disclosed by the invention has the advantages of high conversion efficiency of chlorine-containing compounds, complete absorption and high precision of ion chromatographic analysis; the invention provides an accurate, simple and effective method for analyzing and determining the total chlorine content in the direct coal liquefaction product, particularly analyzing and determining the trace total chlorine content in a complicated base material.

Description

technical field [0001] The invention relates to the technical field of analytical chemistry, in particular to a method for measuring the total chlorine content in direct coal liquefaction products. Background technique [0002] The direct coal liquefaction process, as an efficient and clean coal technology to alleviate the contradiction between the supply and demand of my country's petroleum resources, has entered the stage of commercial demonstration operation. However, there are a certain amount of chlorine-containing compounds, such as organic chlorine and / or inorganic chlorine salts, in the coal direct liquefaction crude oil, residue, bitumen and its hydro-upgrading products produced by the direct coal liquefaction process. During the further processing of liquefied products, they will be hydrolyzed or decomposed to produce hydrogen chloride gas, which will cause corrosion of equipment in a humid environment. Therefore, how to accurately measure the total chlorine conten...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 姜元博李克健高山松杨葛灵章序文李永伦向春兰苏娟
Owner CHNA ENERGY INVESTMENT CORP LTD
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