High-activity iron-based catalysts for coal direct liquefaction and preparation methods for high-activity iron-based catalysts

A technology of direct coal liquefaction and catalyst, which is applied in the direction of physical/chemical process catalysts, chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, etc. It can solve the problem that the oil yield needs to be further improved and the requirements for catalyst conditions are high , limited catalyst dispersion, etc.

Inactive Publication Date: 2012-07-04
XINJIANG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the iron-based catalysts provided by the above-mentioned existing technologies still have the following problems: the smallest particle size of the catalyst is more than tens of nanometers, the dispersion of the catalyst is limited, and the conditions for preparing the catalyst are relatively high. The catalyst is used for direct coal liquefaction The oil yield in the reaction needs to be further improved

Method used

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  • High-activity iron-based catalysts for coal direct liquefaction and preparation methods for high-activity iron-based catalysts
  • High-activity iron-based catalysts for coal direct liquefaction and preparation methods for high-activity iron-based catalysts

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Experimental program
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Effect test

Embodiment 1

[0035] 36.5g sodium oleate (C 18 H 33 O 2 Na) and 10.8g iron chloride (FeCl 3 ·6H 2 O) Add to the solvent system composed of 140mL n-hexane, 60mL water and 80mL ethanol, stir to make it fully mixed; heat the system to 70℃ for 4h; after that, transfer the solution system to the separatory funnel to make the upper layer oily Add 30 mL of water to the phase, let it stand, and separate the lower water phase, repeat 3 times; dry the oil phase liquid containing iron oleate at 70° C. for 12 hours; finally obtain an oil-soluble iron oleate coal direct liquefaction catalyst.

[0036] Using Xinjiang Jiangjunmiao coal for direct coal liquefaction reaction, mixing 7 parts by weight of the above-mentioned iron oleate catalyst with 30 parts by weight of coal sample, adding 0.3 parts by weight of elemental sulfur and 60 parts by weight of tetralin, passing H 2 , At a temperature of 420°C and a pressure of 6.5MPa, react for 75 minutes; after the reaction, the products are extracted with n-hexane, ...

Embodiment 2

[0038] Add 36 g of naphthenic acid with an average molar mass of 300 and 4.8 g of sodium hydroxide (NaOH) to a solvent system consisting of 140 mL of n-hexane, 60 mL of water, and 80 mL of ethanol, and stir to mix thoroughly; heat the system to 70°C 2h to obtain sodium naphthenate solution; 10.8g ferric chloride (FeCl 3 ·6H 2 O) Add to the sodium naphthenate solution and keep it at 70°C for 4 hours; then, transfer the solution system to a separatory funnel, add 30 mL of water to the upper oil phase, let it stand, and separate the lower water phase. Repeat 3 Second; the oil phase liquid containing iron naphthenate is vacuum dried at 70°C for 12 hours; finally an oil-soluble iron naphthenate coal direct liquefaction catalyst is obtained.

[0039] Using Xinjiang Jiangjunmiao coal for direct coal liquefaction reaction, mixing 14 parts by weight of the above iron naphthenate catalyst with 30 parts by weight of coal sample, adding 0.3 parts by weight of elemental sulfur and 60 parts by ...

Embodiment 3

[0041] Mix 70mL of tetrahydronaphthalene and 1mL of oleylamine, stir well for 30min; 2 Under protection, slowly heat the system to 180℃; use a syringe to add 2.4mL Fe(CO) 5 Slowly inject into the system, react at 180℃ for 20min; finally get oil-soluble Fe 3 O 4 Hollow nanospheres are uniformly dispersed in the tetralin solvent system.

[0042] Xinjiang Jiangjunmiao coal is used for direct coal liquefaction reaction. 1 part by weight of the iron-based coal direct liquefaction catalyst is mixed with 25 parts by weight of coal sample, 0.25 parts by weight of elemental sulfur and 50 parts by weight of tetralin are added, and H 2 , At a temperature of 420°C and a pressure of 6.5MPa, react for 75 minutes; after the reaction, the products are extracted with n-hexane, toluene, and tetrahydrofuran through a Soxhlet extractor to obtain oil and n-hexane that are soluble in n-hexane. Asphaltene insoluble in alkanes but soluble in toluene, pre-asphaltene insoluble in toluene but soluble in tetr...

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Abstract

The invention provides three high-activity iron-based catalysts for coal direct liquefaction and preparation methods for the three high-activity iron-based catalysts. The three catalysts are iron oleate, iron naphthenate and Fe3O4 hollow nanospheres respectively. The series of catalysts are oil-soluble, can contact with coal samples well and can react completely. A solvent tetrahydronaphthalene used in the process of preparing the Fe3O4 hollow nanospheres is the solvent used in coal direct liquefaction reaction; by adoption of the 'in-situ' synthesis technology, the catalysts can be directly used in the coal direct liquefaction reaction without aftertreatment; and the catalysts have high contact surface area and high activity in a reaction system. The catalysts are low in preparation cost and simple in preparation and are not required to be recycled. A small quantity of the catalyst is used in the coal direct liquefaction process, but the catalysts have high activity, so temperature and pressure required during the coal direct liquefaction are reduced, conversion ratio of the coal and the yield of oil are obviously increased, and industrial amplified application is realized.

Description

Technical field [0001] The invention belongs to the technical field of direct coal liquefaction, and specifically relates to a high-activity iron-based coal direct liquefaction catalyst and a preparation method thereof. Background technique [0002] With the rapid economic development, my country's oil consumption is increasing year by year. As of December 2009, China's oil dependence on foreign countries has exceeded 50%, which will seriously affect my country's oil supply security. Direct coal liquefaction, as one of the main technologies of "coal instead of oil", can make full use of my country's rich coal resources to produce highly efficient liquid fuels, thereby effectively solving the problem of oil supply security. In addition, coal liquefaction can also solve the environmental pollution caused by coal burning, so that coal resources can be fully and cleanly used. [0003] Direct coal liquefaction is the process of hydrocracking the three-dimensional network composite stru...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/04B01J23/745C10G1/06
Inventor 宿新泰李怡招马凤云孙超任书通刘建超王吉德
Owner XINJIANG UNIVERSITY
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