Loaded metal hydrogenation catalyst, its preparation method and application in ethylene glycol preparation

A hydrogenation catalyst, metal catalyst technology, applied in physical/chemical process catalysts, chemical instruments and methods, preparation of hydroxyl compounds, etc., can solve problems such as unindustrialization, and achieve the effect of high mechanical strength and high temperature resistance.

Active Publication Date: 2012-03-28
JIANGSU SOPO GRP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

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  • Loaded metal hydrogenation catalyst, its preparation method and application in ethylene glycol preparation
  • Loaded metal hydrogenation catalyst, its preparation method and application in ethylene glycol preparation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment 1 Ni-Cu-La / SiC-C catalyst

[0023] 1. Polymer / SiO2 2 Preparation of spherical complexes:

[0024] Dissolve 2.4g of cetyltrimethylammonium chloride in 20ml of deionized water, then add 9.0g of tetraethyl silicate, store at 35°C for 24 hours, cool to 5°C, and dissolve metadichloride Add 5ml of ethylene (25wt%) and azobisisoheptanonitrile (1.5wt%) toluene solution directly, stir rapidly, heat up to 40°C and polymerize for 24 hours, thus obtaining polymer / SiO 2 spherical complexes;

[0025] 2. Preparation of SiC / C spherical molecular sieve:

[0026] Polymer / SiO 2 The spherical composite is carbonized by temperature programming in an argon gas flow. The carbonization temperature is 150°C for 3 hours; SiC / C spherical molecular sieves are obtained, the shape is as figure 1 shown.

[0027] 3. Impregnation aging of SiC / C spherical molecular sieve:

[0028] Soak the SiC / C spherical molecular sieve with 30% nitric acid for 24h, then wash it with deionized water ...

Embodiment 2

[0030] Embodiment 2 Preparation of Ni-Cu-Zn-La / SiC-C catalyst:

[0031] Immersion aging of SiC / C spherical molecular sieves: SiC / C spherical molecular sieves were treated with 30% nitric acid overnight, then washed with deionized water and dried in vacuum. Take Ni(NO 3 ) 2 , Cu(NO 3 ) 2 , Zn(NO 3 ) 2 , La(NO 3 ) 3 and nitrilotriacetic acid to form a methanol solution composed of (Ni: 1.5wt%, Cu: 0.5wt%, Zn: 0.5wt%, La: 0.5wt%, nitrilotriacetic acid: 1.5wt%), and then use SiC / C spherical molecular sieve impregnated, dried, heated to 150°C for 3 hours in the air, and activated with hydrogen at 350°C for 3 hours to obtain a supported metal hydrogenation catalyst.

[0032] In a 100ml autoclave, use methanol as a solvent, add methyl oxalate or glycolic acid and 1.5g of catalyst, the reaction hydrogen pressure is 5.0MPa, the reaction temperature is 150-220 ° C, and the progress of the reaction is monitored by gas chromatography. The conversion rate reaches 95%, and the sel...

Embodiment

[0034] Embodiment 3Ni-Co-Zn-La / SiC-C catalyst:

[0035]Immersion aging of SiC / C spherical molecular sieves: SiC / C spherical molecular sieves were treated with 30% nitric acid, washed with deionized water, and dried in vacuum. Take Ni(NO 3 ) 2 , Co(NO 3 ) 2 , Zn(NO 3 ) 2 , La(NO 3 ) 3 and nitrilotriacetic acid to form a methanol solution composed of (Ni: 1.5wt%, Co: 0.5wt%, Zn: 0.5wt%, La: 0.5wt%, nitrilotriacetic acid: 1.5wt%), and then use SiC / C spherical molecular sieve impregnated, dried, heated to 150°C for 3 hours in the air, and activated with hydrogen at 350°C for 3 hours to obtain a supported metal hydrogenation catalyst.

[0036] In a 100ml autoclave, use methanol as a solvent, add methyl oxalate or glycolic acid and 1.5g of catalyst, the reaction hydrogen pressure is about 5.0MPa, the reaction temperature is Si0-220°C, and the progress of the reaction is monitored by gas chromatography. The conversion rate of the product reaches 98%, and the selectivity to ...

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Abstract

The invention relates to a loaded metal hydrogenation catalyst, its preparation method and application in ethylene glycol preparation. With a spherical SiC / C molecular sieve as a carrier and a metal loading capacity of 0.1-15 wt%, the catalyst adopts nickel as a main metal catalyst, and contains the metal auxiliary agents of Zn, Cu, Co, Fe, Cr, Sn, Bi, Re, La, Ce, Nd, Sm, and Gd. In a catalytic process, a certain amount of methyl oxalate, glycolic acid and the above loaded metal hydrogenation catalyst are added into a solvent, under a hydrogen atmosphere as well as a certain temperature and pressure, ethylene glycol can be prepared. The catalyst of the invention is suitable for the gas-solid phase or liquid-solid phase catalytic hydrogenation process of methyl oxalate and glycolic acid, and the catalytic process is characterized by high activity and selectivity to ethylene glycol. Meanwhile, the catalyst provided in the invention has excellent stability, and is suitable for a long time reaction process of batches.

Description

technical field [0001] The invention belongs to the technical field of catalysts, and in particular relates to a SiC / C spherical molecular sieve-supported nickel-based bimetallic or multimetallic hydrogenation catalyst, a preparation method thereof, and an application thereof in catalyzing the synthesis of ethylene glycol. Background technique [0002] Ethylene glycol (EG for short), also known as glycol and 1,2-ethylene glycol, is used as a hydrating agent in the leather industry and as a solvent in the pharmaceutical industry. The progress of the preparation process is as follows: In 1859, Wurtz made ethylene glycol by reacting ethylene glycol diacetate with potassium hydroxide for the first time, and developed a method for preparing ethylene glycol by direct hydration of ethylene oxide in the following year. In 1937, the UCC company of the United States built the world's first industrial device for the production of ethylene oxide by gas-phase oxidation of ethylene with a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/224B01J27/228C07C31/20C07C29/149
CPCY02P20/52
Inventor 宋勤华黄志军邵守言袁国卿凌晨李峰波曹宏兵周波
Owner JIANGSU SOPO GRP
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