Method for preparing NiB non-crystalline alloy catalyst with the aid of microwave

A technology of amorphous alloys and catalysts, applied in catalyst carriers, chemical instruments and methods, catalyst activation/preparation, etc.

Inactive Publication Date: 2006-06-28
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The dispersion of active components also exists in the preparation of NiB amorphous alloy catalysts by electroless plating.

Method used

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  • Method for preparing NiB non-crystalline alloy catalyst with the aid of microwave
  • Method for preparing NiB non-crystalline alloy catalyst with the aid of microwave
  • Method for preparing NiB non-crystalline alloy catalyst with the aid of microwave

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～6

[0061] These examples illustrate the preparation of unsupported NiB amorphous alloy catalysts.

[0062] Configure 0.1mol / L nickel sulfate solution and 1.0mol / L KBH 4 solution (0.01mol / L NaOH to adjust pH=10, B / Ni=2:1, atomic ratio). At 0°C, air or N 2 atmosphere, under ultrasonic vibration, the KBH 4 The solution was added dropwise to the nickel sulfate solution, reacted until no gas was generated, washed with deionized water until neutral, then washed with absolute ethanol, and stored in absolute ethanol, coded as A-C. The samples were washed with water until neutral, then washed with absolute ethanol, and stored in ethanol.

[0063] During the reaction, catalyst A is obtained by using water as a solvent; catalyst B is obtained by using ethylene glycol as a solvent; and catalyst C is obtained by using N,N-dimethylamide as a solvent. The composition of the catalyst is shown in Table 1. The XRD of catalysts A-C have figure 1 a feature.

[0064] The non-supported NiB amor...

Embodiment 7～12

[0087] These examples illustrate the process of ultrasonically assisted preparation of NiB amorphous alloy catalysts using different main salts and co-salts.

[0088] Same as the preparation process of catalyst A, change the main salt nickel sulfate to nickel nitrate, nickel chloride and nickel acetate and keep the metal salt concentration constant to obtain catalyst G-I.

[0089] Using nickel sulfate as the main salt, using iron sulfate as the auxiliary salt, changing the atomic ratio of Ni and Fe (1:1, 2:1, 4:1), and keeping the total concentration of metal ions at 0.1mol / L, prepared according to catalyst A Methods to obtain catalyst K-L.

[0090] The composition of G-L is shown in Table 1.

Embodiment 13～14

[0092] These examples illustrate the preparation of supported NiB amorphous alloy catalysts.

[0093] Chemical reduction method: the carrier used is titanium oxide (Nanjing Titanium Dioxide Co., Ltd.), and the BET specific surface area is 11.5m 2 / g, average pore volume 0.47cm 3 / g, the average pore diameter is 16.2nm. Weigh 200gTiO 2 Powder, baked at 450°C for 4 hours, weighed 5g carrier in 11ml 1.3mol / LNiSO 4 The solution was soaked for 4 hours. The obtained carrier is suction filtered or centrifuged, dried in the air, oven-dried and roasted. At 0°C, under ultrasonic conditions, nitrogen protection, and vigorous stirring, the KBH 4 solution (2mol / L) with the above TiO 2 React until no gas is produced, filter, wash until neutral, and protect with absolute ethanol. The catalyst number is A1. Ni accounts for 20% by weight in the catalyst.

[0094] Electroless plating method:

[0095] The process of electroless plating supported NiB amorphous alloy: AgNO with a concent...

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Abstract

A microwave aided process for preparing the catalyst of non-crystalline NiB alloy suitable for catalytic hydro-reaction with high catalytic active features that the chemical reduction and chemical plating in microwave field is used, KBH4 is used as reducer, its primary salt is chosen from nickel sulfate, nickel acetate, etc, its secondary salt is chosen from cobalt chloride, iron chloride, etc, its carrier is chosen from oxide, molecular sieve, etc, its solvent is chosen from water, tetrahydrofuran, etc and the complex agent, stabilizer and additive is used.

Description

technical field [0001] The invention relates to a method for preparing a NiB amorphous alloy catalyst, more specifically a method for preparing an NiB amorphous alloy catalyst assisted by ultrasonic waves. Background technique [0002] In the 1940s, Brown adopted KBH 4 The NiB catalyst was prepared by reducing nickel salt. In 1980, Smith proposed the use of amorphous alloys as catalysts for the first time at the Seventh International Conference on Catalysis. So far, NiB amorphous alloy catalyst is still the focus and hotspot of catalytic researchers, and it is expected to replace traditional framework nickel and noble metal catalysts. [0003] CN1196975A discloses an amorphous alloy catalyst of nickel and boron, which consists of NiB amorphous alloy accounting for 0.1-30.0% by weight, porous carrier material accounting for 70.0-99.9% by weight, wherein the atomic ratio of nickel and boron is 0.5-10.0 ; The porous carrier material refers to a non-oxidizing porous body mate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/755B01J21/02B01J23/89B01J32/00B01J37/02B01J37/34C07C5/03
Inventor 张明慧李伟葛少辉吴志杰陶克毅
Owner NANKAI UNIV
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