Preparation method and application of immobilized cesium phosphotungstate catalyst

A cesium phosphotungstate catalyst technology, which is used in the preparation of medium and long-chain fatty acid glycerides, and in the field of preparation of solid-supported cesium phosphotungstate catalysts, can solve the problem of poor reusability and tediousness of free enzymes Separation and purification process, lipase is expensive and other problems, to achieve the effect of improving physical and chemical stability, wide application range, and conducive to adsorption and diffusion

Active Publication Date: 2016-10-12
河南正通食品科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, lipase is expensive, and the reusability of free enzymes is poor, resulting in higher production costs, and the obtained product components are more complex, in addition to medium and long-chain fatty acid oils, there are diglycerides, monoglycerides and raw oils, A more complicated separation and purification process is required (see Chinese invention patent "A Method for Separation and Purification of Medium- and Long-Chain Fatty Acid Triglycerides", application number 2012100042302.6)

Method used

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  • Preparation method and application of immobilized cesium phosphotungstate catalyst
  • Preparation method and application of immobilized cesium phosphotungstate catalyst
  • Preparation method and application of immobilized cesium phosphotungstate catalyst

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Embodiment 1

[0035] Immobilized cesium phosphotungstate catalyst of the present invention 20% (w) UiO-66-Cs 2.5 h 0.5 PW 12 o 40 The preparation method comprises the following steps:

[0036] The first step: active center Cs 2.5 h 0.5 PW 12 o 40 Preparation of:

[0037] Take 1.00 g cesium carbonate (Cs 2 CO 3 ) and 7.07 g phosphotungstic acid (H 3 PW 12 o 40 ) into 0.25 mol / L and 0.08 mol / L aqueous solutions, at room temperature, Cs 2 CO 3 The solution was added dropwise to H 3 PW 12 o 40 In the solution, the speed was kept at 1mL / min, and the magnetic force was strongly stirred for 8h, and the mixture was left to age for 12h, and then the mixture was slowly evaporated to dryness at 50°C; the obtained white solid was dried at 383 K for 12h, Calcined for 2 h to obtain cesium phosphotungstate (Cs 2.5 h 0.5 PW 12 o 40 )spare.

[0038] The second step: catalyst 20% (w) UiO-66-Cs 2.5 h 0.5 PW 12 o 40Preparation of:

[0039] The reactor was placed in a 35°C water bath,...

Embodiment 2

[0041] Immobilized cesium phosphotungstate catalyst of the present invention 35% (w) UiO-66-Cs 2.5 h 0.5 PW 12 o 40 The preparation method comprises the following steps:

[0042] The first step: with embodiment 1.

[0043] The second step: catalyst 35% (w) UiO-66-Cs 2.5 h 0.5 PW 12 o 40 Preparation of:

[0044] The reactor was placed in a 35°C water bath, 80mL DMF (N,N-dimethylformamide) was added to the reactor, and 2.0g of terephthalic acid H 2 (BDC) and 2.8g ZrCl 4 Dissolve in DMF, stir to dissolve, then add 1.5mL concentrated hydrochloric acid to it, stir for 3h, then add 1.05g cesium phosphotungstate salt, continue stirring for 2h, after mixing evenly, transfer the above reaction materials into a stainless steel reaction kettle, 120 Crystallize at ℃ for 30h, take out, filter, wash and dry. Before use, it was activated at a constant temperature of 180°C in an air atmosphere for 10 hours to obtain 35% (w) UiO-66-Cs 2.5 h 0.5 PW 12 o 40 Catalyst with a BET spe...

Embodiment 3

[0046] Immobilized cesium phosphotungstate catalyst of the present invention 50% (w) UiO-66-Cs 2.5 h 0.5 PW 12 o 40 The preparation method comprises the following steps:

[0047] The first step: with embodiment 1.

[0048] The second step: Catalyst 50% (w) UiO-66-Cs 2.5 h 0.5 PW 12 o 40 Preparation of:

[0049] The reactor was placed in a 35°C water bath, 80mL DMF (N,N-dimethylformamide) was added to the reactor, and 2.0g of terephthalic acid H 2 (BDC) and 2.8g ZrCl 4 Dissolve in DMF, stir to dissolve, then add 1.5mL concentrated hydrochloric acid to it, stir for 3h, then add 1.5g cesium phosphotungstic acid salt, continue stirring for 2h, after mixing evenly, transfer the above reaction materials into a stainless steel reaction kettle, 120 Crystallize at ℃ for 30h, take out, filter, wash and dry. Before use, it was activated at a constant temperature of 180°C in an air atmosphere for 10 hours to obtain 50% (w) UiO-66-Cs 2.5 h 0.5 PW 12 o 40 Catalyst with a BET ...

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Abstract

The invention discloses an immobilized cesium phosphotungstate catalyst. Cesium phosphotungstate is introduced in the synthesis process of a metal-organic skeletal material UiO-66 to make the mass ratio of the active component cesium phosphotungstate to the metal-organic skeletal material UiO-66 in the metal organic skeletal immobilized cesium phosphotungstate catalyst reach 0.2-0.65 and the specific surface area of the immobilized catalyst reach 794-1045m<2>/g. A preparation method adopting one-step in situ synthesis can effectively prevent loss of the active site cesium phosphotungstate, so the physical and chemical stability of the catalyst is improved; the Keggin structure, the strong acidity and the oxidation reduction property of cesium phosphotungstate are well kept, so the catalyst has wide application range; adsorption and diffusion of reaction substances on the catalyst are facilitated, so the catalysis efficiency of the catalyst is increased; and the preparation method has the advantages of simplicity, easy operation, easy filtration and separation of the catalyst from products, no corrosion, and no pollution to environment.

Description

technical field [0001] The invention relates to a catalyst used in the chemical industry, in particular to a preparation method of an immobilized cesium phosphotungstate catalyst, and also relates to the application of the catalyst in the preparation of medium and long-chain fatty acid glycerides. Background technique [0002] Phosphotungstic acid is a polyoxometalate with Keggin structure, which has dual characteristics of super acidity and redox. As a super strong solid acid, it can replace most of the inorganic acid catalysts (in non-aqueous solvents, its acid strength is 100 times that of sulfuric acid), and can be used in various acid-catalyzed reactions. However, phosphotungstic acid is a homogeneous catalyst, the post-treatment process of the reaction product is cumbersome, pollutes the environment, and cannot be recycled. Cesium phosphotungstic acid not only retains the advantages of strong acidity, high activity, and high selectivity of phosphotungstic acid, but al...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/18B01J27/188C07C67/10C07C69/30
CPCB01J27/188C07C67/10C07C69/30Y02P20/50
Inventor 谢文磊胡朋涛王宏雁
Owner 河南正通食品科技有限公司
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