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Method for evaluating hydrogen donating ability of hydrogen donor for reaction matrix

A technology of reaction matrix and hydrogen supply capacity, applied in measurement devices, instruments, scientific instruments, etc., can solve the problems of complicated operation, time-consuming, dangerous situations, etc., and achieve the effect of simple operation

Active Publication Date: 2015-03-18
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is cumbersome and time-consuming, and because it involves high temperature and high pressure, dangerous situations may occur from time to time during the operation

Method used

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  • Method for evaluating hydrogen donating ability of hydrogen donor for reaction matrix
  • Method for evaluating hydrogen donating ability of hydrogen donor for reaction matrix
  • Method for evaluating hydrogen donating ability of hydrogen donor for reaction matrix

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0021] In the preferred process of preparing the mixture of the hydrogen donor and the reaction substrate, the amount of the low-boiling organic solvent used is not particularly limited, as long as the hydrogen donor can be fully dissolved. Preferably, the amount of the low-boiling organic solvent is such that the concentration of the hydrogen-donating agent in the solution in which the hydrogen-donating agent is dissolved is 10-30% by weight. The low-boiling point organic solvent is also a volatile solvent, and its boiling point is lower than 80°C. Preferably, the low boiling point solvent is selected from at least one of acetone, dichloromethane, chloroform, methanol and tetrahydrofuran.

[0022] In the above preferred process of preparing the mixture of the hydrogen donor and the reaction substrate, the amount of the hydrogen donor and the reaction substrate is such that the content of the hydrogen donor in the prepared mixture of the hydrogen donor and the reaction substra...

preparation example 1

[0044] Weigh 4 parts of 2 g of 80-100 mesh Longkou coal samples obtained after pulverization, sieving and deashing respectively, add 20% by weight tetrahydronaphthalene dichloromethane solution, 20% by weight tetrahydroquinoline dichloromethane solution therein, respectively. Chloromethane solution, 20% by weight 9,10-dihydrophenanthrene in dichloromethane and 20% by weight octahydrophenanthrene in dichloromethane, sonicated for 10 minutes, then evaporated to dryness, and vacuum the sample at 80°C Dry for 24 hours to obtain a sample 1 with a tetralin content of 1.0% by weight, a sample 2 with a tetrahydroquinoline content of 1.4% by weight, a sample 3 with a 9,10-dihydrophenanthrene content of 1.8% by weight, and an octahydro Sample 4 with a phenanthrene content of 2.0% by weight was sealed and stored for later use.

Embodiment 1

[0046] This example is used to illustrate the method for evaluating the hydrogen donor of the present invention.

[0047] Such as figure 1 As shown, weigh 1 mg of sample 1, sample 2, sample 3 and sample 4 respectively, place them in the cracking crucible (i.e. sample cup 3), put the cracking crucible into cracker 2 through push rod 1, Thermal cracking was carried out at 250°C, 300°C, 350°C, 400°C, 450°C, 500°C and 550°C, respectively, and carried by connecting tube 4 and The chromatographic inlet 5 enters the chromatographic column 8 (high temperature resistant OV-1 chromatographic column) of the gas chromatograph-mass spectrometer 7. At the head of the chromatographic column, low-temperature nitrogen gas is used for cryofocusing. The cryofocusing temperature is -170°C. Thermal cracking and cryofocusing The time is set to 30s. After cryofocusing, the temperature is raised to 350°C at a heating rate of 20°C / min. After being separated by the chromatographic column, the separate...

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Abstract

The invention relates to a method for evaluating hydrogen donating ability of a hydrogen donor for a reaction matrix. The method comprises the following steps: mixing the hydrogen donor with the reaction matrix, then heating to the pyrolysis temperature of the reaction matrix to perform pyrolysis, carrying carrier gas for a reaction product to enter a chromatographic column head of a GC / MS (gas chromatography-mass spectrometry) analyzer to perform freezing and focusing, heating the reaction product after freezing and focusing till the formation of a gas phase after the end of pyrolysis of the reaction matrix, entering a chromatographic column of the GC / MS analyzer to perform separation, performing chromatography and mass spectrometry analysis on effluent of the chromatographic column respectively, and evaluating the hydrogen donating ability of the hydrogen donor according to chromatography and mass spectrometry analysis results. According to the method for evaluating the hydrogen donor, provided by the invention, the hydrogen donating ability, the reaction activity and the range of using temperature of the hydrogen donor can be simply, safely and rapidly evaluated, and the optimal pyrolysis temperature of the reaction matrix can be further known. The method is applicable to the fields of direct liquefaction of coal, coking and the like.

Description

technical field [0001] The invention relates to a method for evaluating the hydrogen-supplying ability of a hydrogen-donating agent to a reaction substrate, in particular, a method for evaluating the hydrogen-supplying ability of a hydrogen-donating agent for a reaction substrate such as coal and heavy oil. Background technique [0002] Hydrogen donating agent refers to partially hydrogenated polycyclic aromatic hydrocarbons, which is a very special type of organic reducing agent, which can supply hydrogen free radicals in a thermal reaction system with a large number of free radicals to make free radicals with higher activity than them. It becomes a neutral compound and stabilizes to achieve the purpose of stabilizing the thermal reaction system, reducing the generation of coke, and inhibiting the further cracking of long-chain free radicals to generate gas. The hydrogen donor can act as a free radical stabilizer, a free radical scavenger, a heat stabilizer, etc., and can b...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 韩江华王树青
Owner CHINA PETROLEUM & CHEM CORP
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