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Rhodium-tellurium intermetallic compound particle, method for producing the same, and use of the same

A technology for intermetallic compounds and manufacturing methods, which can be used in chemical instruments and methods, metal processing equipment, chemical/physical processes, etc., and can solve problems such as differences in the degree of reduction of metal salts, heterogeneous alloy particles, and difficulty in synthesizing intermetallic compounds. , to achieve the effect of less deterioration over time

Inactive Publication Date: 2009-08-26
MITSUBISHI CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in these methods, the reducing agent and the metal salt undergo a reduction reaction while mixing and diffusing, so there is a difference in the reduction degree of the metal salt, and as a result, only inhomogeneous alloy particles can be obtained
[0005] In order to improve this problem and reduce the influence of mixing and diffusion by increasing the reduction reaction speed, the following method is proposed in Patent Document 2: the first reducing agent with weak reducing ability is mixed into the metal salt solution in advance, and the mixed The final solution is added dropwise to the solution obtained after heating the solution containing the second reducing agent with strong reducing ability, but the effect of this method is not ideal
[0006] In addition, Non-Patent Document 2 describes using ethylenediaminetetraacetic acid (EDTA) as a complexing agent and bringing the complexing agent into contact with a reducing agent under neutral conditions. However, in this method, the complexed Rh salt Precipitation occurs, so it is difficult to synthesize an intermetallic compound even if a subsequent reduction operation is performed

Method used

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  • Rhodium-tellurium intermetallic compound particle, method for producing the same, and use of the same
  • Rhodium-tellurium intermetallic compound particle, method for producing the same, and use of the same
  • Rhodium-tellurium intermetallic compound particle, method for producing the same, and use of the same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0259] Add 0.15 mol of rhodium chloride and 0.30 mmol of 1,3-dihydroxy-4-(2-pyridyl azo)benzene (1,3-dihydroxy-4-(2-pyridylazo)benzene) in distilled water (referred to as PAR: Formula C 11 h 9 o 2 N 3 ), then add sodium hydroxide, the pH is adjusted to 13, rhodium chloride and PAR are dissolved thus, prepare 10ml rhodium-containing solution. Let this solution be A solution.

[0260] Further, after adding and dissolving 0.40 mmol of citric acid in distilled water, 0.10 mmol of telluric acid was added and dissolved therein to prepare 10 ml of a tellurium-containing solution. Let this solution be B solution.

[0261] Then, the A solution and the B solution were mixed, and distilled water and sodium hydroxide were added thereto, the pH was adjusted to 13, the total amount was 48ml, then mixed with enough time, and then 2ml of 80% hydrazine hydrate solution was added, Reduction was carried out at 70°C for 3 hours.

[0262] In a nitrogen atmosphere, the black powder obtained ...

Embodiment 2

[0267] After raising the temperature of the compound powder of Example 1 to 150° C. in a nitrogen gas stream, the flowing gas was switched from nitrogen to hydrogen, and the temperature was further raised to 400° C. and kept for 2 hours, thereby performing heat treatment. Thereafter, the flowing gas was switched to nitrogen gas again, and cooled to room temperature to obtain a compound powder (compound powder of Example 2).

[0268] The compound powder of Example 2 was subjected to powder X-ray diffraction measurement. The obtained powder X-ray diffraction pattern was compared with Rh 3 Te 2 The standard peaks together are shown in figure 1 . Depend on figure 1 It can be clearly seen that the powder X-ray diffraction pattern of the compound powder of Example 2 is basically consistent with the standard peak, thus it can be known that the compound powder of Example 2 is an intermetallic compound, and the compound powder is a high-purity Rh 3 Te 2 .

Embodiment 3

[0270] 0.15 mol of rhodium chloride and 0.45 mmol of thiosalicylic acid were added and dissolved in distilled water, and then sodium hydroxide was added to adjust the pH to 13, thereby preparing 10 ml of a rhodium-containing solution. Let this solution be A solution.

[0271] Separately, after adding and dissolving 0.15 mmol of sodium tellurite in distilled water, sodium hydroxide was added to adjust the pH to 13, thereby preparing 10 ml of a tellurium-containing solution. Let this solution be B solution.

[0272] Separately, after adding and dissolving 2 mmol of sodium borohydride in distilled water, sodium hydroxide was added to adjust the pH to 13, thereby preparing 10 ml of a solution containing sodium borohydride. This solution is referred to as C solution.

[0273] Then, mix solution A and solution B, add distilled water and sodium hydroxide to it, and adjust the pH to 13, the total amount is 48ml, then mix with sufficient time, then add solution C, and carry out at 70...

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Abstract

For the purpose of efficiently producing a high-purity rhodium-tellurium intermetallic compound particle, a solution containing a rhodium salt, a tellurium salt and a complexing agent is brought into contact with a reducing agent and an organic compound containing a sulfur atom and / or a nitrogen atom is used as the complexing agent.

Description

technical field [0001] The present invention relates to a method for producing rhodium-tellurium intermetallic compound particles, rhodium-tellurium intermetallic compound particles obtained by the production method, an oxidation catalyst using the rhodium-tellurium intermetallic compound particles, and production of oxidation addition products using the oxidation catalyst Methods. Background technique [0002] PdTe-based catalysts are industrially used as catalysts for oxidative acyloxylation of conjugated dienes. [0003] In view of this, RhTe-based catalysts have extremely high selectivity compared with PdTe-based catalysts, and if RhTe-based catalysts can be used, it will be extremely cost-effective, so the development of RhTe-based catalysts is of great significance. However, since a large amount of Rh in the RhTe-based catalyst is dissolved in acetic acid as a solvent during the reaction, the activity of the RhTe-based catalyst decreases in a very short time, so the R...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/057B22F1/00B22F9/24C22C5/04B22F1/054
CPCB22F9/24B01J27/0576C22C1/0491C22C5/04B22F1/0018B82Y30/00B22F1/054C22C1/047
Inventor 村松淳司高桥英志大野博信高桥和成
Owner MITSUBISHI CHEM CORP
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