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Preparation and application of nitro-containing ligand doped zeolite imidazate framework material ZIF-71-clnImx

A technology of zif-71-clnimx and zeolite imidazolate, which is applied in the field of inorganic functional materials, can solve the problems of difficult waste liquid and increase energy consumption, and achieve the effects of high material yield, shortened time, and improved mass transfer rate

Active Publication Date: 2022-02-08
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Since the concentration of 2,3-BDO in biological fermentation is slightly lower than that of 1,3-PDO, there are few studies on ZIFs materials for the adsorption and separation of 2,3-BDO, and most of them use extraction and distillation to enrich 2,3- BDO, which tends to increase energy consumption and generate large volumes of effluent that is difficult to treat

Method used

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  • Preparation and application of nitro-containing ligand doped zeolite imidazate framework material ZIF-71-clnImx
  • Preparation and application of nitro-containing ligand doped zeolite imidazate framework material ZIF-71-clnImx
  • Preparation and application of nitro-containing ligand doped zeolite imidazate framework material ZIF-71-clnImx

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Embodiment 1: Synthesis of ZIF-71-clnIm x

[0026] ZIF-71-clnIm x The synthesis method was stirred at room temperature, and the sources of reagents were zinc acetate dihydrate (98%, Sigma-Aldrich Company), 4,5-dichloroimidazole (fluorochem company ), 4-nitro-5-chloro-1-hydroimidazole (95%, Bi De Pharmaceutical Co., Ltd.), methanol (99.5%, Sinopharm Chemical Reagent Co., Ltd.).

[0027] Concrete synthetic steps are:

[0028] (a) Preparation of ZIF-71: Zinc acetate dihydrate (6 mmol, 1.32 g) was dissolved in 70 ml of methanol. 4,5-Dichloroimidazole (18.0 mmol, 2.46 g) was dissolved in 30 ml of methanol, then the zinc acetate dihydrate solution was transferred to the imidazole solution and stirred at room temperature for 24 h.

[0029] (b) Preparation of ZIF-71-clnIm 5 : Dissolve zinc acetate dihydrate (6 mmol, 1.32 g) in 70 ml of methanol. Mix 4,5-dichloroimidazole (17.1 mmol, 2.34 g) and 4-nitro-5-chloro-1-hydroimidazole (0.9 mmol, 0.13 g) and dissolve in 30 ml of...

Embodiment 2

[0037] Embodiment 2: Single-component static adsorption experiment

[0038] This embodiment adopts ZIF-71-clnIm prepared in Example 1 x (x= 0, 3.8, 12.7) (x is the actual molar doping amount), before the experiment, the sample was activated with methanol for 3 times at room temperature, each time for 12 h, and then prepared into 500-600 μm particles, and then in Vacuum activation at 150 ºC for 12 h to remove solvent molecules. Single-component 2,3-BDO (5-150 g / L) and 1,3-PDO (5-150 g / L) static adsorption experiments were performed as follows: Weigh 0.05 g of adsorbent particles and put them in a 10 mL circle Add 1.5 mL of 2,3-BDO (5-150 g / L) or 1,3-PDO (5-150 g / L) solutions of different concentrations into glass bottles at the bottom, then seal and store at 25 ºC. Set aside for 24 h to ensure adsorption saturation. After the adsorption, the supernatant of the solution was permeated through the filter membrane, and the concentration was analyzed by gas chromatography. ima...

Embodiment 3

[0039] Example 3: Two-component dynamic column penetration adsorption experiment

[0040] This embodiment adopts ZIF-71-clnIm prepared in Example 1 x (x = 0, 3.8, 12.7) (x is the actual molar doping amount) for two-component dynamic column penetration adsorption experiments. ZIF-71-clnIm x Activation with methanol at room temperature for 3 times, 12 h each time, and then prepared into 500-600 μm particles, and then vacuum activation at 150 ºC for 12 h to remove solvent molecules, and then use two-component 2,3-BDO and 1 , 3-PDO mixed solution (50 / 50 g / L) rinses the penetrating pipeline to clean the pipeline and ensure uniform solution concentration; ZIF-71-clnIm x The particles were loaded into a stainless steel packing column with an inner diameter of 8 mm, and the two ends of the packing column were fixed with quartz wool, and the height of the packing layer was 25 cm; at an ambient temperature of 25 ºC, the two-component 2,3-BDO and The 1,3-PDO mixture (50 / 50 g / L) flowed...

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Abstract

The invention discloses a preparation method and an application of a nitro-containing ligand doped zeolite imidazate framework material ZIF-71-clnImx. ZIF-71-clnImx is prepared by introducing 4-nitro-5-chloro-1-hydroimidazole (clnIm) with different contents into a ZIF-71 skeleton to replace 4, 5-dichloroimidazole (dclIm). The material has relatively strong adsorption affinity on a byproduct 2, 3-butanediol (2, 3-BDO) in a biological fermentation liquid, so that 1, 3-propylene glycol (1, 3-PDO) with relatively high purity is obtained. The synthesis method provided by the invention is simple to operate, and the dynamic adsorption capacity of the synthesized ZIF-71-clnIm3.8 (x is the actual molar doping amount) on 2, 3-BDO in simulated fermentation liquor is as high as 157.9 mg / g. The separation technology provided by the invention is simple in process, low in energy consumption, good in material stability and wide in application prospect.

Description

technical field [0001] The invention relates to a zeolite imidazolate framework material ZIF-71-clnIm doped with a nitro ligand x The preparation method and its application in adsorption and separation belong to the application field of inorganic functional materials. Background technique [0002] 1,3-PDO is an important chemical raw material, which is widely used in cosmetics, pharmaceutical intermediates, coatings, lubricants, inks and other fields. Its important use is to polymerize with terephthalic acid (PTA) to produce polyparaphenylene Propylene glycol dicarboxylate (PTT). However, in the process of microbial fermentation, what is usually obtained after purification is a mixed aqueous solution of low-concentration 1,3-PDO (30-150 g / L) and 2,3-BDO (20-70 g / L), in order to obtain The finished products 1,3-PDO and 2,3-BDO need to be separated. In view of the low concentration of 1,3-PDO and 2,3-BDO, and the similar physical and chemical properties of the two substance...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00B01D15/14B01D15/20B01D15/26
CPCC08G83/008B01D15/206B01D15/14B01D15/265
Inventor 石琪张健爽高美珍王梦瑶董晋湘
Owner TAIYUAN UNIV OF TECH
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