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Non-crystalline alloy catalyst of uniform grain size and its preparing method

An amorphous alloy with uniform size technology, applied in catalyst activation/preparation, chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problem of catalyst inactivity, rapid reduction reaction, partial Problems such as excessive concentration

Inactive Publication Date: 2006-08-23
SHANGHAI NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Because the amorphous alloy catalyst prepared by the traditional quenching method has the following disadvantages: (1) the requirements for the reaction device are relatively high, and the investment is large; (2) the synthesized catalyst is not active and must be activated before use; (3) ) Since the amorphous structure is a thermodynamic metastable state, a crystallization reaction will occur when heated, and the thermal stability is poor; (4) The specific surface area of ​​the catalyst is small, generally 0.1-1m 2 / g
However, this method has the following problems: (1) the reduction reaction is rapid and violently exothermic, causing local overheating, resulting in agglomeration and / or crystallization of the generated alloy particles; (2) the process of dropping the reducing agent has a problem of excessive local concentration , making this process an unbalanced process
Even if a very high stirring speed is used, the particle size of the prepared amorphous alloy catalyst is still very uneven, and the particle size distribution range is very wide, resulting in large differences in catalytic performance, poor thermal stability and possible increase in pressure drop in fixed bed reactions. (3) Rapid nucleation and rapid growth cause the prepared particles to wrap a large number of unreduced metal oxides and decomposed boron oxide species. These impurities, which are difficult to completely remove by physical and chemical methods, cover part of the active sites and cause catalytic activity. decline
The above factors have become the bottleneck for the industrial application of amorphous alloy catalysts

Method used

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  • Non-crystalline alloy catalyst of uniform grain size and its preparing method
  • Non-crystalline alloy catalyst of uniform grain size and its preparing method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Step 1: Quantitative CoCl 2 Dissolve in distilled water, add quantitative ammonia solution, stir and mix thoroughly to obtain a clear and transparent green solution, CoCl 2 The molar ratio with ammonia water is: 1:1.

[0022] Step 2: Add quantitative KBH to the above solution 4 , stir well to mix. Raw material molar ratio: Co 2+ / BH 4 - =1:4.

[0023] Step 3: The above solution was heated to 5° C., and an ultrasonic probe with a frequency of 20 kHz and a power of 50 W was directly inserted into the mixed solution for ultrasonic treatment. Black particles gradually and slowly formed in the solution, and gas came out.

[0024] Step 4: Wash the prepared black particles repeatedly with water and absolute ethanol to obtain a Co-B amorphous alloy with a particle size of 200 nm.

Embodiment 2

[0026] Step 1: Quantitative NiCl 2 Dissolve in distilled water, add quantitative ethylenediamine solution, stir and mix thoroughly to obtain a clear and transparent blue solution, NiCl 2 The molar ratio with ethylenediamine is: 1:5.

[0027] Step 2: Add quantitative NaBH to the above solution 4 , stir well to mix. Raw material molar ratio: Ni 2+ / BH 4 - =1:4.

[0028] Step 3: The above solution was heated to 20° C., and an ultrasonic probe with a frequency of 10 kHz and a power of 50 W was directly inserted into the mixed solution for ultrasonic treatment. Black particles gradually and slowly formed in the solution, and gas came out.

[0029] Step 4: Wash the prepared black particles repeatedly with water and absolute ethanol to obtain a Ni-B amorphous alloy with a particle size of 100 nm.

Embodiment 3

[0031] Step 1: Quantitative PdCl 2 Dissolve in distilled water, add quantitative oxalic acid solution, stir and mix thoroughly to obtain a clear and transparent pink solution, PdCl 2 The molar ratio with oxalic acid is: 1:0.5.

[0032] Step 2: Add quantitative KBH to the above solution 4 , stir well to mix. Raw material molar ratio: Pd 2+ / BH 4 - =1:3.

[0033] Step 3: The above solution was heated to 20°C, and an ultrasonic probe with a frequency of 70 kHz and a power of 50 W was directly inserted into the mixed solution for ultrasonic treatment. Black particles gradually and slowly formed in the solution, and gas came out.

[0034] Step 4: Wash the prepared black particles repeatedly with water and absolute ethanol to obtain a Pd-B amorphous alloy with a particle size of 10 nm.

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Abstract

The present invention discloses non-crystalline alloy catalyst of uniform grain size and its preparation process. The catalyst is spherical grains of size in 10-500 nm. The preparation process includes: mixing metal salt solution and ligand solution well to form stable metal complex, adding reductant to obtain homogeneously mixed solution, ultrasonic initiation of reduction in the solution to obtain black solid, and washing separately with deionized water and absolute ethyl alcohol to obtain the non-crystalline alloy catalyst of uniform grain size. The said preparation process can maintain the high homogeneity and dispersion of the metal salt and reductant components, so as to prepare high performance non-crystalline alloy with uniform grain size. The catalyst may be used in hydrogenating various compounds with unsaturated functional radical and has hydrogenating performance superior to non-crystalline alloy prepared through conventional chemical reduction process.

Description

technical field [0001] The invention relates to an amorphous alloy catalyst with uniform particle size, in particular to a narrow distribution amorphous alloy catalyst and a preparation method thereof. Background technique [0002] Amorphous alloy means that the atoms or their mixed arrangement that make up the alloy are completely disordered, and there is no periodicity and translation in space. Therefore, amorphous alloys are a type of long-range disorder and short-range order in structure. Its unique structural characteristics endow it with excellent catalytic activity, selectivity, anti-poisoning and corrosion resistance, and it is also environmentally friendly. [0003] Because the amorphous alloy catalyst prepared by the traditional quenching method has the following disadvantages: (1) the requirements for the reaction device are relatively high, and the investment is large; (2) the synthesized catalyst is not active and must be activated before use; (3) ) Since the a...

Claims

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Application Information

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IPC IPC(8): B01J35/08B01J23/75B01J23/755B01J23/44B01J23/46B01J37/16B01J37/34
Inventor 李和兴李辉张静
Owner SHANGHAI NORMAL UNIVERSITY
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