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Determination method of rhodium content in water-soluble rhodium-phosphine complexes

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

Active Publication Date: 2018-03-13
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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  • Determination method of rhodium content in water-soluble rhodium-phosphine complexes
  • Determination method of rhodium content in water-soluble rhodium-phosphine complexes
  • Determination method of rhodium content in water-soluble rhodium-phosphine complexes

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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 measuring the rhodium content in a water-soluble rhodium-phosphine complex, which is easy to operate, and the measurement result can be used as a commercial judgment of the rhodium content in a finished catalyst, comprising the following steps: (1) taking a sample, adding concentrated sulfuric acid to carry out Digest; (2) add concentrated nitric acid dropwise to drive away excess sulfuric acid; (3) add dropwise hydrochloric acid to drive away nitric acid; (4) dilute; (5) add sodium nitrite; (7) The precipitate was aged for 10-30 minutes; (8) The precipitate was washed twice with 0.05% hexaammine cobalt nitrate solution, washed three times with absolute ethanol, and washed once with ether (9) weigh; (10) calculate the content of rhodium according to the following formula: in the formula, w1--precipitation weight; w2--the weight of crucible; w--sample weight; conversion factor.

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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Patent Type & Authority Patents(China)
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