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Method for determining molecular sieve and adsorbate affinity AT value

A technology for molecular sieves and adsorbates, which is applied in the field of determination of the AT value of the affinity between molecular sieves and adsorbates, and can solve problems such as poor accuracy

Inactive Publication Date: 2012-10-24
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is to measure molecular sieve and adsorbate affinity A T value, in the past this method of determination, because the molecular sieve is easy to absorb the moisture in the air, the measured molecular sieve and adsorbate affinity A T The problem of poor accuracy of the value, to provide a new molecular sieve and adsorbate affinity A T Value determination method

Method used

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  • Method for determining molecular sieve and adsorbate affinity AT value
  • Method for determining molecular sieve and adsorbate affinity AT value
  • Method for determining molecular sieve and adsorbate affinity AT value

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] ZSM-5 / silicalite-1 core-shell molecular sieve A T Determination of value

[0016] Put the 13mg ZSM-5 / silicalite-1 core-shell molecular sieve sample into the vacuum desiccator quickly after removing water, and put the container containing solid n-hexane into the vacuum desiccator quickly; cover the lid of the vacuum desiccator and vacuumize For 15 minutes, the sample was equilibrated under the saturated vapor pressure of the adsorbate under study at an absolute pressure gauge of 43KPa and an operating temperature of 17°C for 24 hours. °C / min heating rate from room temperature to 470 °C to measure the weight loss of the molecular sieve sample, and calculate the affinity A between the molecular sieve and the adsorbate from the DTG peak temperature T The value is 111.86.

[0017] Table 1

[0018]

[0019] The above sample was repeatedly measured once, and the results of the repeated measurement twice were shown in Table 1, and its secondary determination A T The rela...

Embodiment 2

[0021] Silicalite-1 Molecular Sieve A T Determination of value

[0022] Put the 14mg Silicalite-1 molecular sieve sample into the vacuum desiccator quickly after removing the water, and put the container containing solid n-hexane into the vacuum desiccator quickly; cover the vacuum desiccator cover, and vacuumize for 20min to make the sample dry in the vacuum The temperature is 30KPa, the operating temperature is 25°C, and the adsorbate under study is equilibrated for 28 hours under the saturated vapor pressure. The equilibrated sample is taken out, and the temperature is raised from room temperature to Measure the weight loss of molecular sieve samples at 520°C, and calculate A from the DTG peak temperature T The value is 88.40.

[0023] Table 2

[0024]

[0025] The above sample was repeatedly measured once, and the results of the repeated measurement twice were shown in Table 2, and its secondary determination A T The relative standard deviation RSD of the value is o...

Embodiment 3

[0027] ZSM-5 Molecular Sieve A T Determination of value

[0028] Put the 15mg ZSM-5 molecular sieve sample into the vacuum desiccator quickly after dehydrating, and put the container containing solid n-pentane into the vacuum desiccator quickly; cover the vacuum desiccator, and vacuumize for 30min to make the sample At a vacuum degree of 22KPa and an operating temperature of 28°C, equilibrate for 30 hours under the saturated vapor pressure of the adsorbate under study, take out the balanced sample, and use a thermal analyzer to increase the temperature from room temperature at a rate of 19°C / min under a nitrogen atmosphere. Rise to 580°C to measure the weight loss of the molecular sieve sample, and calculate A from the DTG peak temperature T The value is 76.90.

[0029] table 3

[0030]

[0031] The above sample was repeatedly measured once, and the results of the repeated measurement twice were shown in Table 3, and its secondary determination A T The relative standard...

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Abstract

The invention relates to a method for determining the molecular sieve and adsorbate affinity AT value to mainly solve a problem of bad accuracy of the determined molecular sieve and adsorbate affinity AT value in previous literatures because water in air is easily adsorbed by the molecular sieve. The method comprises the following steps: a required amount of a molecular sieve sample which is dewatered and a solid organic solvent to be adsorbed by the molecular sieve are placed in a closed container having a vacuum degree of below 50KPa by absolute pressure and an operation temperature of 15-30DEG C; the solid organic solvent naturally melts to a liquid organic solvent under the vacuum condition, and the liquid organic solvent naturally volatilizes and is adsorbed by the molecular sieve; and after the adsorption of the molecular sieve reaches saturation, the molecular sieve and adsorbate affinity AT value is determined through a thermal analyzer. The method well solves the problem through above technical scheme, and can be applied to the test of the molecular sieve and adsorbate affinity AT value.

Description

technical field [0001] The invention relates to a molecular sieve and adsorbate affinity A T method of value determination. Background technique [0002] Zeolite molecular sieve is a kind of inorganic aluminosilicate crystal material whose skeleton is composed of regular channels or cage structure. It has good structural stability, special channel shape selection and adsorption properties. , ion exchange and other fields have important application value. [0003] Zeolite molecular sieve is conducive to the selective adsorption of molecules because of its uniform and regular pores and large specific surface area. Therefore, the research on the adsorption properties of molecular sieves can reveal the zeolite pores and the interaction between the adsorbate and the framework, which is of great significance for understanding the mechanism of zeolite catalysis and separation. The silicon-oxygen framework is the structural basis of zeolites. Studying the interaction between zeol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N5/04
Inventor 蒙根许中强
Owner CHINA PETROLEUM & CHEM CORP