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Method for determining content of rhodium in water-soluble rhodium-phosphine complex

A method of determination and complex technology, applied in the direction of weighing by removing certain components

Active Publication Date: 2015-11-18
成都欣华源科技有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In the prior art, to the mensuration of constant rhodium, only see the mensuration report (National Standard of the People's Republic of China, platinum-rhodium alloy chemical analysis method, GB1485---79) about the mensuration report of rhodium content in the platinum-rhodium alloy, to above-mentioned water-soluble The mensuration of the constant rhodium in the rhodium phosphine complex catalyst has not been reported yet

Method used

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  • Method for determining content of rhodium in water-soluble rhodium-phosphine complex
  • Method for determining content of rhodium in water-soluble rhodium-phosphine complex
  • Method for determining content of rhodium in water-soluble rhodium-phosphine complex

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Embodiment 1

[0028] The mensuration of rhodium content in the water-soluble rhodium phosphine complex of embodiment 1

[0029] Required reagents, solutions and instruments:

[0030] Water-soluble rhodium-phosphine catalyst sample: vacuum-dried at 70° C. for 5 hours.

[0031] Sulfuric acid: analytically pure. Nitric acid: analytically pure. Hydrochloric acid: analytically pure. Sodium nitrite: superior grade. Absolute ethanol: analytically pure. Anhydrous ether: analytically pure.

[0032] G 4 Glass sand crucible. A small vacuum drying box with a vacuum pump. One electronic balance (d=0.1mg).

[0033] Hexammine cobalt nitrate lotion: 0.05% aqueous solution.

[0034] Saturated hexaammine cobalt nitrate solution (precipitant solution): Weigh 17 grams of crystalline hexaammine cobalt nitrate, heat and dissolve with 300 mL deionized water, filter through fast filter paper, and dilute to 1000 mL with high-purity water.

[0035] The rhodium content determination process and the result ...

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Abstract

The invention discloses a method for determining the content of rhodium in a water-soluble rhodium-phosphine complex. The method is easy to operate, and the determination result can be taken as the commercial evaluation on the content of rhodium in a finished catalyst product. The method includes the steps of: (1) taking a sample, adding concentrated sulfuric acid to conduct digestion; (2) adding concentrated nitric acid dropwise to drive out excess sulfuric acid; (3) adding hydrochloric acid dropwise to drive out nitric acid; (4) conducting dilution; (5) adding sodium nitrite; (6) adding a saturated solution of nitrate cobaltic hexamine dropwise till no precipitation of yellow sediment; (7) ageing the sediment for 10-30min; (8) washing the sediment with a 0.05% nitrate cobaltic hexamine solution twice, with anhydrous ethanol 3 times, and with ethyl ether once in order; (9) performing weighing; and (10) calculating the content of rhodium according to the formula as shown in the specification, wherein w1 is the sediment weight, w2 is the crucible weight, w is the sample weight, and 0.19054 is the conversion factor of a rhodium double salt to rhodium.

Description

technical field [0001] The invention relates to a method for determining rhodium content in a water-soluble rhodium-phosphine complex. Background technique [0002] Currently, water-soluble rhodium-phosphine complex catalysts, including [tris[tris(m-sodium phenylsulfonate)]phosphinecarbonyl rhodium hydride [molecular formula HRh(CO)(TPPTS) 3 , TPPTS molecular formula: P(m-C 6 h 4 SO 3 Na) 3 ·3H 2 O], [two [three (m-sulfonate sodium phenyl)] phosphine carbonyl rhodium chloride [molecular formula is RhCl (CO) (TPPTS) 2 ], and [tris[tris(m-sodium phenyl sulfonate)phosphine]]rhodium chloride [molecular formula RhCl(TPPTS) 3 ], has been used in industrial production to prepare aldehydes by hydroformylation of olefins, wherein the content of rhodium in the catalyst is to control the initial substrate amount (alkenes) and ligand three (sodium sulfonate phenyl) of the hydroformylation reaction Phosphine (referred to as TPPTS) amount and catalyst [HRh (CO) (TPPTS) 3 ) or RhCl...

Claims

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Application Information

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IPC IPC(8): G01N5/04
Inventor 胡家元陈华向进李贤均
Owner 成都欣华源科技有限责任公司