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Batch-preparation and quick-separation method of iron-based coal-liquefaction nano catalyst

A nano-catalyst and coal liquefaction technology, applied in chemical instruments and methods, preparation of liquid hydrocarbon mixtures, physical/chemical process catalysts, etc., can solve the problems of difficult scale-up of preparation methods, difficulty in batch preparation, and high cost of waste treatment. Achieve the effect of low raw material price, high direct liquefaction activity and uniform shape

Inactive Publication Date: 2013-02-06
XINJIANG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of ordinary iron-based catalysts is that their catalytic activity is not high. Studies have shown that the smaller the particle size of the catalyst, the better the dispersion in the direct coal liquefaction system, and the higher its catalytic activity.
Although a variety of iron-based catalysts with small particle sizes have been prepared, and iron-based catalysts with high activity have been obtained, there are still some shortcomings, such as expensive preparation of raw materials (such as organometallic compounds, organic solvents), and difficult preparation methods. Scale-up (such as laser pyrolysis), complex production process, and high cost of waste treatment
[0004] At present, the ideal preparation method is to synthesize iron-based catalysts through aqueous precipitation, which has low raw material cost and simple production process, but it is difficult to obtain catalysts with smaller particle sizes by direct precipitation.
In addition, nanoscale catalyst products are difficult to separate from the catalyst preparation system, making it difficult to achieve batch production, and improper separation will cause particle agglomeration, greatly reducing its catalytic activity

Method used

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  • Batch-preparation and quick-separation method of iron-based coal-liquefaction nano catalyst
  • Batch-preparation and quick-separation method of iron-based coal-liquefaction nano catalyst
  • Batch-preparation and quick-separation method of iron-based coal-liquefaction nano catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] with FeCl 3 ·6H 2 O was used as raw material to prepare iron oxyhydroxide nanoparticles. Prepare 0.02 mol·L -1 FeCl 3 ·6H 2 O solution 2 L, at 76 o C and stirred for 10 hours to obtain a yellow opaque homogeneous liquid containing ferric oxyhydroxide nanoparticles, and the mixed liquid was not coagulated. Weigh 0.07 g ferric fulvic acid and prepare it into 10 ml aqueous solution. Add the prepared ferric fulvic acid solution into the reaction liquid after the reaction is completed under the condition of stirring, resulting in a large amount of precipitation. Leave to separate layers and remove the supernatant. The precipitate was filtered, washed three times with distilled water and three times with ethanol. The product was dried at room temperature to obtain iron oxyhydroxide nanoparticles.

Embodiment 2

[0026] with FeCl 3 ·6H 2 O as a raw material to prepare iron oxyhydroxide nanoparticles in large quantities. Prepare 0.04 mol·L -1 FeCl 3 ·6H 2 O solution 150 L, at 76 o C and stirred for 10 hours to obtain a yellow opaque homogeneous liquid of ferric oxyhydroxide nanoparticles, and the mixed liquid was not coagulated. Weigh 10 g of ferric fulvic acid and prepare 600 ml of aqueous solution. Add the prepared ferric fulvic acid solution into the reaction liquid after the reaction is completed under the condition of stirring, resulting in a large amount of precipitation. Leave to separate layers and remove the supernatant. The precipitate was filtered, washed three times with distilled water and three times with ethanol. The product was dried at room temperature to obtain 422 g of iron oxyhydroxide nanoparticles.

Embodiment 3

[0028] The direct liquefaction of Xinjiang Yili coal and Xinjiang Jiangjunmiao coal was catalyzed by nano-iron oxyhydroxide prepared in large quantities. Load the reaction materials in the high-pressure reactor according to the following material ratio: 30 g dry basis coal, 0.3 g elemental sulfur, 60 g hydrogen-donating solvent tetrahydronaphthalene, and the amount of catalyst input is 3% of the dry basis coal weight in which the iron content is % meter, pass hydrogen to make the initial pressure of the reactor 6.5MPa; react according to the following reaction conditions: the reaction temperature is 420 o C, the reaction time is 75 min; after the reaction is over, the product is extracted with n-hexane, toluene, and tetrahydrofuran through a Soxhlet extractor to obtain oil soluble in n-hexane, bitumen insoluble in n-hexane but soluble in toluene Pre-asphaltenes and tetrahydrofuran-insoluble liquefaction residues that are insoluble in alkene and toluene but soluble in tetrahydr...

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Abstract

The invention provides a batch-preparation and quick-separation method of an iron-based coal-liquefaction nano catalyst. The batch-preparation and quick-separation method includes utilizing 0.01-0.1mol L-1 of FeCl3 solution as a raw material, hydrolyzing the FeCl3 solution within the temperature ranging from 70 DEG C to 80 DEG C for 6-12 hours to obtain nano FeOOH colloidal solution; utilizing fulvic acid iron and sodium humate and the like as flocculant, simply separating nano particles by the aid of the flocculant and accordingly realizing batch preparation of the nano FeOOH. The batch-preparation and quick-separation method is low in cost, simple to operate, pollution-free and capable of preparing in batch. The catalyst prepared is small in particle diameter which is within nano range and uniform in particle diameter distribution, direct liquefaction activity of coal catalyzing is high, conversion rate ranging from 83-95% and oil yield rate ranging from 70-82 can be realized by direct liquefaction of Xinjiang Yili coal catalyzing, and conversion rate ranging from 85-97% and oil yield rate ranging from 65-85% can be realized by direct liquefaction of catalyzing of coal of General Temple of Xinjiang.

Description

technical field [0001] The invention relates to a method for preparing a catalyst for direct liquefaction of coal, in particular to a method for preparing an ultrafine and highly active nano-iron-based direct liquefaction catalyst for coal in an aqueous phase system, and using humate to separate nanoparticles to achieve batch preparation, which belongs to inorganic materials field. Background technique [0002] Coal direct liquefaction is a technology that hydrogenates coal macromolecules under the action of certain temperature, pressure and catalyst to crack them into small molecule gaseous hydrocarbons with high H / C ratio. [0003] After nearly a century of development, scientists from various countries have developed a variety of direct liquefaction processes to achieve industrial production, mainly including the IGOR process in Germany, the NEDOL process in Japan, the HIT process in the United States, and the Shenhua coal direct liquefaction process in my country. As on...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/745C10G1/06
Inventor 宿新泰饶雪辉李怡招马凤云钟梅樊金龙蔡泽宇孙好文冯春全
Owner XINJIANG UNIVERSITY
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