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A kind of preparation method and application thereof with nafion film loaded rare earth metal catalyst

A rare earth metal, catalytic preparation technology, applied in catalyst activation/preparation, preparation of organic compounds, preparation of carbon-based compounds, etc. The effect of catalyst with high continuous use performance, high glycerol conversion rate and good industrialization prospects

Active Publication Date: 2019-12-31
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Aiming at the problems existing in the prior art such as low concentration of glycerin, high reaction temperature, low yield of acrylic acid, high cost of production process and post-treatment, difficulty in continuous use, etc., the present invention proposes a catalyst that uses Nafion film to support rare earth metals. It has high activity in catalyzing the preparation of acrylic acid from glycerol, and has good continuous use characteristics

Method used

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  • A kind of preparation method and application thereof with nafion film loaded rare earth metal catalyst
  • A kind of preparation method and application thereof with nafion film loaded rare earth metal catalyst
  • A kind of preparation method and application thereof with nafion film loaded rare earth metal catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] The preparation method of the catalyst supporting rare earth metals with Nafion film is as follows:

[0026] (1) Pretreatment Nafion 115 membrane material:

[0027] Put Nafion 115 membrane in 50mL 2mol / L H at 75℃ 2 o 2 Soak in the solution for 1.5h to remove organic impurities, then in 50mL 2mol / L H at 75℃ 2 SO 4 Soak in the solution for 1 hour to remove metal impurities, and finally boil and rinse the film in twice-distilled water to obtain a colorless and transparent sulfonyl fluoride Nafion-F resin film.

[0028] (2) Preparation of rare earth metal chlorides:

[0029] Add 20mL concentrated hydrochloric acid and 15mL distilled water to a 50mL round bottom flask, then add 10g La 2 o 3 , Stirring with a magnet makes La 2 o 3The solid dissolved until the solution was clear. Weigh 15g of ammonium chloride solid and add it into the reaction solution, stir to dissolve the ammonium chloride solid. When the solution is concentrated to about 25mL, transfer it to an e...

Embodiment 2

[0043] The preparation of catalyst and reaction condition are the same as embodiment 1, just change the kind of catalyst into Nafion thin film supported cerium catalyst, the consumption of cerium chloride is 5mmol in the step (3), the volume of tetrahydrofuran is 20mL, contains 50mmol allyllithium Tetrahydrofuran-diethyl ether solution was 18mL, and the supported phosphine-containing ligand was 10g.

[0044] The conditions for preparing acrylic acid are the same as those in Example 1, except that the type of catalyst is changed to Nafion film-supported cerium catalyst, the dosage of Nafion film-supported cerium catalyst is 4g, and the reaction time is 7h.

[0045] The catalytic activity of Nafion film-supported cerium catalysts for the catalytic conversion of glycerol to acrylic acid is shown in Table 2:

[0046] Table 2 Effect of different reaction parameters on Nafion thin film-supported cerium catalyst for catalytic conversion of glycerol to acrylic acid

[0047]

[004...

Embodiment 3

[0054] The preparation and reaction conditions of the catalyst are the same as in Example 1; the conditions for preparing acrylic acid are the same as in Example 1, except that the type of catalyst is changed to Nafion film-supported praseodymium catalyst.

[0055] The catalytic activity of Nafion film-supported praseodymium catalysts for the catalytic conversion of glycerol to acrylic acid is shown in Table 3:

[0056] Table 3 The effect of different reaction parameters on Nafion film-supported praseodymium catalyst for the conversion of glycerol to acrylic acid

[0057]

[0058] Table 3 reflects the effects of water content in glycerin, temperature, volume ratio of vaporized glycerin to gas, total space velocity of gas, and reaction time on the preparation of acrylic acid from glycerin catalyzed by Nafion film-supported praseodymium catalysts.

[0059] Effect of water content in glycerol: Wherein keeping other conditions constant, only changing the water content in glycer...

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Abstract

The invention belongs to the technical field of acrylic acid preparation, and specifically relates to a preparation method and application of a rare earth metal catalyst supported by a Nafion film. The method of preparing a rare earth metal catalyst supported by a Nafion film is as follows: anhydrous rare earth metal chloride, a suspension of tetrahydrofuran, a tetrahydrofuran-ether solution containing allyl lithium, and a supported phosphine-containing ligand are used as raw materials. Under certain conditions, A rare earth metal catalyst supported on a Nafion film was prepared. In addition, the present invention catalyzes the preparation of acrylic acid by using a Nafion film-supported rare earth metal catalyst as a raw material and a Nafion film-supported rare earth metal catalyst as a catalyst. The reaction under certain catalytic conditions produces acrylic acid; the glycerol conversion rate reaches 100%. , the acrylic acid yield reached 80.0%. The preparation method provided by the invention has high glycerin conversion rate, high acrylic acid yield, simple post-processing, high continuous use performance of the catalyst, simple preparation process, safety and environmental protection, and has good industrial prospects.

Description

technical field [0001] The invention belongs to the technical field of acrylic acid preparation, and in particular relates to a preparation method and application of Nafion thin film loaded rare earth metal catalyst. Background technique [0002] Acrylic acid (Acrylic acid) is one of the very important chemical raw materials. It is widely used in rubber synthesis, plastics and paint industries. At present, the main preparation method is to produce propylene or propane through a two-step oxidation process in the air. However, as diesel engines gradually start to use biodiesel as fuel in recent years, the global demand for biodiesel is increasing. It is estimated that the production of biodiesel will reach 4.0×10 in 2023. 10 L. The production of biodiesel mostly uses the transesterification method. According to statistics, about 0.1 tons of glycerin is produced for every ton of biodiesel produced. In addition, glycerin can also ferment starch by microorganisms, convert starch...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/10B01J31/24B01J35/06B01J37/06C07C51/235C07C57/04C07C45/38C07C45/52C07C47/22
CPCC07C45/002C07C45/38C07C45/52C07C51/235B01J31/069B01J31/10B01J31/2404B01J37/06B01J35/59C07C57/04C07C47/22
Inventor 周心沈灵沁殷恒波王爱丽
Owner JIANGSU UNIV