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Preparation method of rhodium caprylate

A technology of octanoic rhodium and octanoic acid, which is applied in the field of homogeneous rhodium catalyst synthesis, can solve the problems of cumbersome purification and preparation of rhodium chloride, low overall yield, and many steps, and achieve high yield, fast reaction speed, and high purity.

Inactive Publication Date: 2012-11-21
陕西瑞科新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Method 1 starts from rhodium chloride, first prepares rhodium acetate, and then prepares rhodium octanoate by ligand exchange. Although the yield in the latter step exceeds 90%, the yield of rhodium acetate is only 75%, so the total yield is low and there are many steps. It takes a long time; numerous toxic organic solvents have been used in the method described in CN101353301A
Method 2 also starts from rhodium chloride. Although the problem of long reaction time is solved, the purification and preparation of rhodium chloride is also very complicated.

Method used

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Examples

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Effect test

Embodiment 1

[0009] Example 1: Add 200ml of pure water to a 500ml reaction flask at room temperature, add 57mmol of n-octanoic acid, adjust Ph to 6 with NaOH to obtain a buffered aqueous solution of octanoic acid-sodium octanoate. Continue to add 19mmol of sodium chlororhodium to the reaction flask, use an oil bath to heat up to 100°C, reflux and keep the reaction for 3 hours. Then it was cooled to room temperature, and 22% NaOH solution was added dropwise to adjust the pH to 13. Suction filtration, washing with deionized water to obtain rhodium octoate. The obtained rhodium octanoate was vacuum dried at 100°C and -0.05MPa to a water content of less than 0.1%. Obtain 7.02 g rhodium octanoate emerald green crystals with a yield of 97.3%.

Embodiment 2

[0010] Example 2: Add 20L of pure water to a 50L reaction flask at room temperature, add 7.6mol of n-octanoic acid, and adjust Ph to 5.5 with NaOH to obtain a buffered aqueous solution of caprylic acid-sodium caprylate. Continue to add 1.9 mol of sodium chlororhodium into the reaction flask, heat up to 90° C. with an oil bath, and reflux for 3.5 hours to keep warm. Then it was cooled to room temperature, and 22% NaOH solution was added dropwise to adjust the pH to 12. Suction filtration, washing with deionized water to obtain rhodium octoate. The resulting rhodium octanoate was vacuum dried at 90°C and -0.04MPa to a moisture content of less than 0.1%. 712 g of emerald green crystals were obtained with a yield of 98.87%.

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Abstract

The invention discloses a preparation method of rhodium caprylate. The preparation method comprises the following steps of: adding rhodium sodium chloride into excess caprylic acid-sodium caprylate buffer aqueous solution with pH value of 4.5-7.0; heating to 80-100 DEG C; reacting for 2-5 hours; cooling; neutralizing; filtering; washing; and performing vacuum drying to obtain rhodium caprylate emerald crystal. According to the preparation method, the rhodium sodium chloride is used as a rhodium source in place of rhodium chloride, the reaction speed is high, the yield is high (greater than 95 percent), the purity is high (greater than 99 percent), and large-scale production is facilitated.

Description

Technical field [0001] The invention belongs to the technical field of homogeneous rhodium catalyst synthesis, and specifically relates to a preparation method of rhodium octoate. Background technique [0002] Rhodium caprylate C 32 H 60 O 8 Rh 2 It is a noble metal organic compound catalyst developed in recent years. Like other rhodium carboxylates, rhodium octanoate is also a divalent dinuclear rhodium complex, usually called rhodium dimer. One of the main applications of rhodium octoate is a homogeneous catalyst used in the synthesis of carbapenem antibiotic products. Carbapenem antibiotics are substitutes for penicillin, and their efficacy is 200 times that of penicillin. [0003] The main preparation methods of rhodium octanoate include: 1) rhodium acetate-caprylic acid ligand exchange method (J Phys Chem, 1986, 90:5502-5503; Inorg Chem, 1996, 35, 3643-3658; CN101353301A); 2) rhodium chloride -Caprylic acid direct method (CN101891606A). Method 1 starts with rhodium chloride...

Claims

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Application Information

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IPC IPC(8): C07C53/126C07C51/41
Inventor 蔡万煜秦磊
Owner 陕西瑞科新材料股份有限公司
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