Preparation method of hierarchical porous material-loaded cobalt-based catalyst

A cobalt-based catalyst and multi-stage pore technology, which is applied in the direction of molecular sieve catalysts, chemical instruments and methods, and the preparation of liquid hydrocarbon mixtures, can solve the problems of non-interconnection, zeolite uniformity, loading, etc., to avoid diffusion limitations, high water Thermal stability, the effect of high thermal stability

Inactive Publication Date: 2015-04-29
华文蔚
3 Cites 8 Cited by

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Problems solved by technology

[0008] Tang Yi et al. (CN 01126842.5) used diatomite as a carrier, formed a zeolite film on its surface through the nano-zeolite seed crystal layer-by-layer assembly method, and then grew it secondary under an organic amine atmosphere, thus forming a zeolite film on the diatomite. Zeolite material with a certain strength and multi-level pore structure, but the pores of zeolized diatomite are not interconnected, which will limit the diffusion
[0009] Hiroko Shikata et al. used the sol-gel method to load Silicalit-1 on a multi-level channel through-flow silica gel material (Journal of Sol-G...
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Abstract

The invention discloses a preparation method of a hierarchical porous material-loaded cobalt-based catalyst. The method comprises the following steps: (1) evenly mixing a silicon source, an aluminum source, ethanol, NH3 and H2O at the ratio of 1 to (20-30) to (25-35) to (0.1-0.4) to (1-3), and adding a template agent at the mass ratio of the template agent to the aluminum source being (0.5-1) to 1; (2) putting the mixed liquid obtained from the step (1) into a crystallization kettle lined with polytetrafluoroethylene, filtering, washing, drying and removing the template agent through three-section temperature control roasting; (3) carrying out acid treatment on a carrier precursor to obtain a hierarchical porous carrier; and (4) dipping a saline solution dissolved with cobalt or a saline solution of cobalt and non-noble metal into the hierarchical porous material by adopting an equivalent-volume impregnation method for 10-48 hours, drying at 100-130 DEG C, and roasting at 300-600 DEG C for 4-10 hours, tabletting, and screening to prepare the hierarchical porous material-loaded cobalt-based catalyst.

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Examples

  • Experimental program(2)

Example Embodiment

[0022] Example 1
[0023] (1) According to the silicon source: aluminum source: ethanol: NH3: H2O = 1:20:25:0.1:1; the silicon source uses porous solid silica gel particles, and the aluminum source uses sodium aluminate. The above raw materials are mixed uniformly, and then the template is added The mass ratio of the added amount of the template agent to the aluminum source is 1:1; the template agent is porous carbon or porous polystyrene microspheres;
[0024] (2). The mixed solution obtained in step (1) is put into a crystallization kettle lined with polytetrafluoroethylene, crystallized at 120°C for 24 hours and at 200°C for 60 hours; filtered, washed, Dry, remove the template by three-stage temperature-controlled roasting, decompose the template at a low temperature of 200°C for 6.0 hours, decompose the template at a medium temperature of 250°C for 4.0 hours, and remove free carbon at a high temperature of 650°C for 20.0 hours; obtain a catalyst carrier precursor;
[0025] (3) Treat the carrier precursor acid with 1 mol/L sulfuric acid, a treatment temperature of 180°C, a treatment time of 1.01 hour, and a pressure of 0.5 MPa to obtain a multi-stage porous carrier;
[0026] (4) Using the equal volume dipping method, immerse the dissolved cobalt nitrate solution into the multi-stage porous material for 48 hours, then dry at 130°C, roast at 600°C for 10 hours, press tablets, and sieving. Class-pored zeolite particles support cobalt-based catalysts.

Example Embodiment

[0027] Example 2
[0028] (1) According to silicon source: aluminum source: ethanol: NH3: H2O = 1:30:35:0.4:3; silicon source uses porous solid silica gel particles, aluminum source uses sodium aluminate, the above raw materials are mixed uniformly, and then the template is added The mass ratio of the added amount of the template agent to the aluminum source is 0.5:1; the template agent is porous carbon or porous polystyrene microspheres;
[0029] (2). The mixed liquid obtained in step (1) is put into a crystallization kettle lined with polytetrafluoroethylene, crystallized at 80°C for 24 hours and at 130°C for 48 hours; filtered, washed, Dry, remove the template by three-stage temperature-controlled roasting, decompose the template at a low temperature of 200°C for 6.0 hours, decompose the template at a medium temperature of 350°C for 4.0 hours, and remove free carbon at a high temperature of 550°C for 20.0 hours; obtain a catalyst carrier precursor;
[0030] (3) Treat the carrier precursor acid with 0.1 mol/L hydrochloric acid, a treatment temperature of 20°C, a treatment time of 1.00 hours, and a pressure of 0.1 MPa to obtain a multi-stage porous carrier;
[0031] (4) Using the equal volume impregnation method, immerse the cobalt-dissolved salt solution or the salt solution of cobalt, precious metals and non-precious metals into the multi-stage porous support for 48 hours, then dry at 130°C and roast at 600°C After 40 hours, tableting and sieving to prepare multi-class pore zeolite particles supporting cobalt-based catalyst.
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