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A kind of three-phase catalyst uio-67-im and its preparation method and application

A technology of uio-67-im and catalysts, which is applied in catalytic reactions, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of low yield, long time consumption, high reaction temperature, etc., and achieve cost reduction and easy recycling , the effect of less dosage

Active Publication Date: 2018-10-02
SHANDONG NORMAL UNIV
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

Such as the organic-water two-phase system composed of 1-bromo-n-octane and sodium cyanide aqueous solution, the reaction is carried out at 103 ° C for 3 hours, the yield is only 2.3%, the reaction temperature is high, the time is long, and the yield is low

Method used

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  • A kind of three-phase catalyst uio-67-im and its preparation method and application
  • A kind of three-phase catalyst uio-67-im and its preparation method and application
  • A kind of three-phase catalyst uio-67-im and its preparation method and application

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Embodiment 1: the preparation of organic ligand L

[0046] Concrete preparation steps are as follows:

[0047] (1)N 2 Under protection, methyl 4-bromo-3-methylbenzoate (5mmol, 1.15g), 4-methoxycarbonylphenylboronic acid (5.1mmol, 0.92g), CsF (20mmol, 3.0g), placed in a 100ml three-necked flask Add Pd catalyst 5% (0.3 ~ 0.5g), 50ml of anhydrous THF as a solvent, reflux at 67 ° C, after the reaction, silica gel column chromatography to separate the product (petroleum ether, dichloromethane) to obtain a pink solid 1.05g , yield 74%.

[0048]

[0049] (2) Intermediate A (8.96mmol, 2.54g), NBS (10.3mmol, 1.83g), AIBN (0.90mmol, 0.15g), was placed in a 100ml round bottom flask, and 45ml of carbon tetrachloride was added as a solvent, 90 Reflux at ℃ for 3h, track the reaction by thin-layer column chromatography (ethyl acetate: n-hexane = 2:8), after the reaction, filter, wash the filter cake with dichloromethane, combine the filtrates, evaporate the solvent under reduced...

Embodiment 2

[0058] Embodiment 2: Synthesis of UiO-67-IM

[0059] ZrCl 4 (0.12mmol, 28.8mg), 50 equivalents of acetic acid, DMF4.8ml was added to the beaker, ultrasonicated for 30min, the organic ligand L (0.12mmol, 68.31mg) prepared in Example 1 was added and continued ultrasonicated for 20min, put into a kettle, put into pre-heated Place in an oven at 120°C, keep the temperature constant for 24 hours, after the reaction is completed, cool to room temperature, centrifuge, take out the precipitate, soak in DMF solution at 80°C for 2 hours, centrifuge, soak the precipitate in 70°C absolute ethanol solution for 12 hours, repeat the ethanol soaking three times , The precipitate was taken out and dried under high vacuum to obtain 0.04g. Yield: 47.3% (based on L).

[0060] We characterized the compound by IR, TGA, and PXRD, and the results are shown in 3, 4, and 5, respectively.

Embodiment 3

[0062] Take benzyl chloride (1mmol, 115.1uL), NaN 3 (2mmol, 0.13g), water 2mL into a 25mL single-necked round-bottom flask, stirred at room temperature for 5min, then added UiO-67-IM (0.02mmol, 0.014g) (catalyst dosage is based on imidazolium salt), heated to 80°C , maintain stirring reaction at 80°C, and track the reaction by gas chromatography (the reaction diagram is as follows Figure 6 shown). After the reaction, the reaction system was lowered to room temperature, 2ml of double distilled water and 5mL of dichloromethane were added, fully extracted, liquid separated, the organic phase and the aqueous phase were rapidly centrifuged, the catalyst was recovered, and directly put into the next reaction, and the catalyst was used for 5 cycles , the organic phase is tested by gas chromatography to calculate the yield, and the catalytic effect is shown in Table 1. The recovered catalyst was characterized by PXRD, and UiO-67-IM still kept its original framework (as Figure 7 sh...

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Abstract

The invention discloses an organic ligand L for synthesizing a triphase catalyst UiO-67-IM and the triphase catalyst UiO-67-IM. The triphase catalyst UiO-67-IM has the structural formula of [Zr6O4(OH)4L6]n, wherein n is a nonzero natural number. A preparation method of the triphase catalyst UiO-67-IM comprises the steps that the organic ligand L, ZrCl4 and acetic acid are dissolved into DMF, heat preservation is conducted for 24 hours at 120 DEG C, the temperature is lowered to room temperature, and then the metal organic framework UiO-67-IM is obtained. The catalyst can effectively catalyze a benzyl chloride azidation reaction, heavy metal salt does not need to serve as the catalyst, heterogeneous catalysis is achieved, the catalyst can be repeatedly utilized 5 times or above and is easy to recycle, the utilization rate of the catalyst is increased, and the cost is reduced; meanwhile, the catalyst is mild in reaction temperature, short in reaction time, low in dosage, free of other additives and beneficial for industrialized application and popularization.

Description

technical field [0001] The invention belongs to the technical field of catalyst preparation, in particular to a three-phase catalyst UiO-67-IM and its preparation method and application. Background technique [0002] Metal-organic framework (Metal-organic Framework, MOF) is a research hotspot in recent years. Compared with traditional porous materials, MOF has porosity, larger specific surface area and pore volume in the framework, and is used as a porous functional material. Applications in catalysis show great advantages. [0003] Phase transfer catalysts have been widely used in organic synthesis since the 1970s. It is well known that many organic synthesis reactions are easy to carry out under homogeneous phase but difficult to carry out under heterogeneous phase. For example, in the organic-water two-phase system composed of 1-bromo-n-octane and aqueous sodium cyanide solution, the reaction is carried out at 103° C. for 3 hours, and the yield is only 2.3%. The reactio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D233/60B01J31/22C07C247/10
CPCB01J31/2213B01J2231/4283B01J2531/0213B01J2531/0241B01J2531/48C07C247/10C07D233/60
Inventor 董育斌胡玉红王建成
Owner SHANDONG NORMAL UNIV
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