Preparation method of high-activity and free-reduction Cu/ZnO catalyst

A catalyst and high-activity technology, applied in the direction of catalyst activation/preparation, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problems affecting the grain size of metal catalysts, the growth of metal Cu grains, and the remaining amorphous carbon

Inactive Publication Date: 2014-08-13
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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Problems solved by technology

With the deepening of research later, it was found that this method has two disadvantages: ①The combustion process is too violent, and a large amount of heat is released instantaneously, which easily leads to the growth of the reduced metal Cu grains; ②Because it is carried out under an inert atmosphere, many Carboxyl organic matter is incompletely decomposed, and there is a large amount of carbon-containing organic matter and amorphous carbon remaining
Therefore, the stage leading to the growth of metal grains is the process of solid-phase grinding. We found that during the process of solid-phase grinding of metal precursors and formic acid, the reaction is very violent, releasing a lot of heat, accompanied by a large release of nitrogen oxides. Directly lead to the agglomeration of the precursor, which significantly affects the grain size of the metal catalyst after calcination

Method used

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  • Preparation method of high-activity and free-reduction Cu/ZnO catalyst
  • Preparation method of high-activity and free-reduction Cu/ZnO catalyst
  • Preparation method of high-activity and free-reduction Cu/ZnO catalyst

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Experimental program
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Embodiment 1

[0025] Table 1 shows the characterization results and low-temperature methanol synthesis reaction data of the Cu / ZnO catalysts prepared by the citric acid-sol-gel method, the formic acid solid-phase grinding method and the acetic anhydride-alcoholic solution method of the present invention. As shown in Table 1, the specific surface area of ​​metal Cu / ZnO catalysts prepared by three methods and the use of N 2 The surface area of ​​metallic copper determined by O chemisorption was citric acid: BET, 27.7 m 2 / g,S Cu ,3.2 m 2 / g; formic acid: BET, 15.29 m 2 / g,S Cu ,4.42 m 2 / g; Acetic anhydride: BET, 41.54 m 2 / g,S Cu ,13.26 m 2 / g. The XRD characteristic peaks of the three prepared catalysts were all attributed to metal Cu and ZnO without any impurity peaks. The grain size of metal Cu and ZnO is calculated using the Scherrer formula, D = Kλ / (β cos θ). Among them, D represents the calculated grain size, K is the Scherrer constant 0.89, λ is the X-ray wavelength of coppe...

Embodiment 2

[0032] Example 2. Table 2 shows the characterization, reactivity and formazan selectivity of Cu / ZnO catalysts prepared by different molar ratios of acetic anhydride / copper nitrate. The characterization instruments and conditions are consistent with those in Example 1, and the catalyst evaluation conditions are still synchronized with those in Example 1. From Table 2, we can clearly see that with the increase of acetic anhydride content in the dissolution process, the smaller the crystal grains of Cu in the final prepared catalyst, the higher the reactivity and the higher the methanol selectivity. However, as the amount of acetic anhydride increases, the time required for the solution reduction process is longer, and the maximum reaction time can reach 50 hours before the reduction process can be completed. Because in the oxidation reaction process, with the increase of reducing agent dosage, the reduction process is slower.

[0033] Table 2 Characterization, reactivity and me...

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Abstract

The invention discloses a preparation method of a high-activity and free-reduction Cu / ZnO catalyst and relates to a preparation method of a catalyst. According to the preparation method, acetic anhydride is adopted for replacing original multi-carboxyl organic acid (such as citric acid, glycine and oxalic acid) or formic acid as a chelating agent and a reducing agent; in the stirring process after an alcohol solution with different moles of acetic anhydride is mixed with copper nitrate and zinc nitrate, small bubbles are generated in the solution slowly and are released slowly, brown-yellow oxynitride is released, and then sky-blue uniform precipitates are obtained; after the precipitates are roasted in an inert atmosphere at the temperature of 300 DEG C, the deep-red ultrafine metal Cu / ZnO catalyst can be directly obtained by one step. The Cu / ZnO catalyst is directly used for a synthetic reaction of methanol without any additional reducing process, and is excellent in reaction activity and methanol selectivity.

Description

technical field [0001] The invention relates to a catalyst preparation method, in particular to a high-activity, reduction-free Cu / ZnO catalyst preparation method. Background technique [0002] Metal catalysts are the most important class of catalysts in industrial catalysis, and they are also the most widely used catalysts. According to their functional classification, metal catalysts can be divided into functional catalysts such as hydrogenation, dehydrogenation, oxidation, isomerization, and cyclization. According to its own output and price classification, metal catalysts include base metal catalysts, such as: Ni, Cu, Co, Fe, etc.; and noble metal catalysts, such as: Pt, Pd, Ru, Rh, etc. At present, the preparation methods of metal catalysts mainly include chemical methods and physical methods. Among them, chemical methods mainly include impregnation method, co-precipitation method, homogeneous deposition method, sol-gel method and microemulsion method; physical metho...

Claims

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Application Information

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IPC IPC(8): B01J23/80B01J37/08C07C31/04C07C29/154
CPCY02P20/52
Inventor 石磊王玉鑫谭猗生
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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