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Fixing method for bimetal salt

A bimetallic salt, metal salt technology, applied in chemical instruments and methods, chemical/physical processes, catalyst activation/preparation, etc., can solve problems such as bimetallic salts that have not yet been seen, and achieve stable activity, not easy to leak, and catalyst loading. high volume effect

Inactive Publication Date: 2008-08-06
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, there has been no report on the use of microcapsule technology to form an emulsion to immobilize bimetallic salts through water-in-oil

Method used

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  • Fixing method for bimetal salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Weigh 0.6g CuCl 2 and 0.15g MnCl 2 Dissolve in 10mL water to form solution A; weigh 6.0g toluene 2,4-diisocyanate and 3.5g sorbitan monooleate (Span-80) and dissolve in 40mL cyclohexane to prepare solution B; 25°C Add solution A to solution B under mechanical stirring, continue to stir for 20 minutes, add 0.5mL triethylamine (TEA), react for 5h, then add 0.8mL TEA, react for 24h, and the reaction system is centrifuged to obtain the required microcapsules. The microcapsules were washed and filtered with acetone, 95% ethanol, deionized water and acetone successively, and dried at room temperature to obtain bimetallic copper chloride and manganese chloride microcapsules, abbreviated as (CuCl 2 +MnCl 2 ) EnCat. The morphology of the microcapsules and the distribution of metal salts on the walls of the microcapsules were characterized by scanning electron microscopy and transmission electron microscopy. The scanning electron microscope picture shown in Figure 1 shows tha...

Embodiment 2

[0026] Weigh 0.15g MnCl 2 and 1.2g CoCl 2 Dissolve in 30mL water to form solution A; weigh isophor diisocyanate (15g) and 7g Span-80 and dissolve in 60mL cyclohexane to prepare solution B; add solution A to solution B under mechanical stirring at 25°C, continue Stir for 20min, add 0.7mL TEA, react for 5h, then add 1.3mL TEA, react for 24h, the reaction system is centrifuged to obtain the required microcapsules, and the obtained microcapsules are successively washed with acetone, 95% ethanol, deionized water and acetone. filter, and dry at room temperature to obtain bimetallic cobalt chloride and manganese chloride microcapsules, abbreviated as (MnCl 2 +CoCl 2 ) EnCat. Transmission electron microscope pictures show that the metal in the prepared microcapsules is distributed in nanometer state on the microcapsules.

Embodiment 3

[0028] Weigh 0.2g CuCl 2 and 0.6MnCl 2 Dissolve in 10mL water to form solution A; weigh toluene 2,4-diisocyanate (6.0g) and Span-80 (3.5g) and dissolve in 40mL cyclohexane to obtain solution B; add solution A under mechanical stirring at 25°C Add TEA (0.5mL) to solvent B, continue to stir for 20min, add TEA (0.8mL) after 5h of reaction, react for 24h, and obtain the desired microcapsules through centrifugation of the reaction system. % ethanol, deionized water and acetone washing and suction filtration, drying at room temperature to obtain bimetallic palladium chloride and nickel chloride microcapsules, abbreviated as (CuCl 2 +NiCl 2 ) EnCat. Transmission electron microscope pictures show that the metal in the prepared microcapsules is distributed in nanometer state on the microcapsules.

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Abstract

The invention discloses a bimetal salt immobilization method, which comprises: adding 0.1 to 4 weight parts of metal salt I and 0.1 to 4 weight parts of metal salt II into 10 to 50 volume parts of deionized water and then forming solution A; adding 6 to 15 weight parts of diisocyanate and 1 to 10 parts of surfactant into 40 to 80 volume parts of cyclohexane and then forming solution B; adding the solution A into the solution B under strong stirring and then forming stable water - in - oil emulsion C; adding 1 to 6 volume parts of tertiary amine catalyst into the emulsion C; after reacting for 24h, adding cyclohexane to dilute and centrifugally separating out microcapsule; washing the microcapsule with ethanol of 95 percent, deionized water and acetone respectively and natural drying, thus achieving the microcapsule loading bimetal salts. The method has the advantages of simple operation, low cost, high stability of the microcapsule loading bimetal salts and wide application range.

Description

technical field [0001] The invention relates to a method for immobilizing bimetallic salts, in particular to a method for immobilizing bimetallic salts using microcapsule technology. Background technique [0002] Bimetallic salts are widely used in the synthesis of pharmaceutical intermediates and fine chemicals because of their high catalytic activity shown by their synergistic effects. As a homogeneous catalyst, the bimetallic salt is in the same system as the reactants and products during the reaction process, and there are problems such as difficult catalyst separation and recovery, environmental pollution, and residual catalyst pollution products. very important. [0003] There are two types of commonly used methods for the immobilization of bimetallic salts: one is to immobilize metal salts on porous inorganic carriers (such as SiO 2 , activated carbon, molecular sieve, etc.). Although this method is simple to prepare, there are problems such as poor catalyst stabil...

Claims

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Application Information

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IPC IPC(8): B01J13/16B01J37/00B01J35/02
Inventor 纪红兵李俊丽裴丽霞
Owner SOUTH CHINA UNIV OF TECH
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