Gas-chromatography filler capable of separating and analyzing hydrogen isotopes and preparation method of gas-chromatography filler

A hydrogen isotope and gas chromatography technology, which is applied in the field of loaded chromatographic packing and its preparation, can solve the problems of high energy consumption, clogging of chromatographic columns, and affecting the separation effect, and achieve accurate quantitative analysis, short separation time and good separation effect Effect

Inactive Publication Date: 2017-11-14
BEIJING UNIV OF CHEM TECH
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

However, the problems of these methods are high energy consumption and high cost, so people have developed a new separation method: gas chromatography to separate hydrogen isotopes
However, when metal-organic framework compound materials are used as chromatographic stationary phases, they have disadvantages such as poor mechanical strength and difficulty in controlling particle size.
The low mechanical strength of the stationary phase will cause the loss of the chromatographic column or cause the clogging of the chromatographic column, and the non-uniform particle size of the stationary phase will reduce the column efficiency and affect the separation effect

Method used

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  • Gas-chromatography filler capable of separating and analyzing hydrogen isotopes and preparation method of gas-chromatography filler
  • Gas-chromatography filler capable of separating and analyzing hydrogen isotopes and preparation method of gas-chromatography filler
  • Gas-chromatography filler capable of separating and analyzing hydrogen isotopes and preparation method of gas-chromatography filler

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] (1) 3.0g of γ-Al with a particle size of 80-100 mesh 2 o 3 Add to a solution consisting of 0.5mmol copper perchlorate hexahydrate, 0.5mmol sodium pyrazine-2,3-dioate, 0.625mmol pyrazine and 20mL deionized water, and immerse for 2h;

[0037] (2) Take the product in step (1) out of the soaking solution, rinse it with deionized water, and then dry it in an oven at 110°C for 30 minutes;

[0038] (3) Steps (1)-(2) are used as a cyclic process, and the product obtained in step (2) is substituted for γ-Al in step (1) 2 o 3 Repeat this cycle for 7 times.

[0039] (4) Add 3.00 g of the product obtained in step (3) to MnCl composed of 3.58 mmol of manganese chloride tetrahydrate and 20 mL of deionized water 2 The solution was immersed for 2 hours; transferred together to a 100mL round bottom flask, the solvent was evaporated to dryness with a rotary evaporator, and the product was dried at 100°C for 10 hours to obtain a supported composite material.

Embodiment 2

[0041] (1) 3.00g pre-activated γ-Al 2 o 3 Dipping in the following order: a) 100mL 10mM trimesic acid ethanol solution, 40min, b) 20mL ethanol, 5min, c) 100mL 10mM copper acetate trihydrate ethanol solution, 20min, d) 20mL ethanol, 5min

[0042] (2) In the step (1), a) to d) constitute one cycle, and thus cycle impregnation 4 times to obtain a supported composite material, which is then dried at 100° C. for 30 min.

[0043] (3) Add 3.00 g of the sample in step (2) to MnCl composed of 3.58 mmol of manganese chloride tetrahydrate and 20 mL of deionized water 2 The solution was immersed for 2 hours; transferred together to a 100mL round bottom flask, the solvent was evaporated to dryness with a rotary evaporator, and the product was dried at 100°C for 10 hours to obtain a supported composite material.

Embodiment 3

[0045] (1) Add 0.182mmol 2,5-dihydroxyterephthalic acid and 0.613mmol nickel nitrate hexahydrate to 15mL (volume ratio 1:1:1) of DMF-ethanol-water mixed solvent, sonicate until completely dissolved ;

[0046] (2) Transfer the solution in step (1) to a 23mL hydrothermal reaction kettle with PTFE lining, and add 0.60g of 80-100 mesh γ-Al at the same time 2 o 3 , at 1.5°C·min -1 After rising to 100°C, keep it for 24 hours, then cool down to room temperature naturally;

[0047] (3) The product obtained in step (2) is separated from the mother liquor by decantation, and the sample is soaked in 15mL of methanol solvent for solvent exchange, and solvent exchange is carried out 4 times within 48h to exchange the DMF adsorbed in the composite material, and finally in 100 Dry in a drying oven at ℃ for 5 hours to remove methanol to obtain the product.

[0048] (4) Add 3.00 g of the product in step (3) to MnCl composed of 3.58 mmol of manganese chloride tetrahydrate and 20 mL of deion...

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Abstract

The invention relates to a gas-chromatography filler capable of separating and analyzing hydrogen isotopes and a preparation method of the gas-chromatography filler and belongs to the technical field of functional materials. The material takes gamma-Al2O3 as a carrier. The synthesis method comprises the steps of loading a metal-organic skeleton compound to the surface of the gamma-Al2O3, carrying out washing and drying, and then, dipping the gamma-Al2O3 in an aqueous solution of a transition metal salt MXn, thereby obtaining a loaded type composite material. The gas-chromatography fixed-phase material is applied to the separation of hydrogen isotopes H2/D2, the separation effect is good, the quantitative analysis is accurate, and the material can be repeatedly used and is low in price; due to good mechanical properties, the recovery and reuse are very convenient.

Description

technical field [0001] The invention belongs to the technical field of functional materials, in particular to a hydrogen isotope H 2 / D 2 Loaded chromatographic filler with good separation / analysis performance and preparation method thereof. Background technique [0002] Deuterium (D 2 ) has irreplaceable applications in thermonuclear fusion reaction, neutron scattering technology and isotope tracking, so D 2 obtaining is of great significance. However, in nature D 2 The abundance of is very low, people get D 2 The main means is from H 2 / D 2 D in the mixture 2 seperate. Currently H 2 / D 2 Separation methods mainly include cryogenic distillation, chemical exchange, and thermal diffusion. However, the problems of these methods are high energy consumption and high cost, so a new separation method has been developed: gas chromatography to separate hydrogen isotopes. The key to the separation of hydrogen isotopes by gas chromatography lies in the selection of the st...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/281B01J20/30B01D59/00
CPCB01J20/281B01D59/00
Inventor 张立娟谢辉朱宏伟周云山
Owner BEIJING UNIV OF CHEM TECH
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