Method for purifying ruthenium complex crude product through recrystallization method

A technology for ruthenium complexes and crude products, which is applied in the field of purification of ruthenium complex crude products, can solve the problems of unfavorable industrial production, high cost, and low output, and achieve the effects of low cost, short cycle, and high output

Active Publication Date: 2013-04-03
江苏先进无机材料研究院
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AI Technical Summary

Problems solved by technology

[0012] The present invention solves the technical problems unfavorable for industrialized production such as low yield, small output, high cost and long cycle caused by the Sephadex LH-20 column chromatography method in the prior art, and its purpose is to provide a A method for purifying crude ruthenium complex products by crystallization, the method can obtain ruthenium complex products in large quantities, with low cost, high yield and high purity

Method used

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  • Method for purifying ruthenium complex crude product through recrystallization method
  • Method for purifying ruthenium complex crude product through recrystallization method
  • Method for purifying ruthenium complex crude product through recrystallization method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1Z907-1

[0039] Get 5g of the Z907 crude product obtained in Comparative Example, 250mL of methanol, and 75mL of 10% tetrabutylammonium hydroxide aqueous solution into a 500mL beaker, and stir at room temperature for 1 hour with a magnetic stirrer; The solids are discarded. Add 50mL 0.1M HNO to the filtrate 3 The acid solution was acidified, and the pH value was adjusted to 5. During this process, a large amount of black solids were gradually precipitated, and the solution gradually became clear. Then filter with a filter membrane with a pore size of 10 μm to obtain a black solid, which is washed 3 times with 50 mL of water. The obtained solid was dried under vacuum at 50° C. for 10 hours to obtain 4.6 g of product Z907-1 with a yield of 92% and a purity of 62.5%. Its HPLC spectrum is as figure 2 shown.

Embodiment 2Z907-2

[0041] Take 5g of Z907-1 product, 250mL of methanol, and 75mL of 10% tetrabutylammonium hydroxide aqueous solution into a 500mL beaker, and stir for 1 hour at room temperature with a magnetic stirrer; the solution is filtered with a filter membrane with a pore size of 1um, and the solid on the filter membrane is discarded. Add 50mL 0.1M HNO to the filtrate 3 The acid solution was acidified, and the pH value was adjusted to 5. During this process, a large amount of black solids were gradually precipitated, and the solution gradually became clear. Then filter with a pore diameter of 10um to obtain a black solid, which was washed 3 times with 50mL of water. The obtained solid was dried under vacuum at 50° C. for 10 hours to obtain 4.8 g of product Z907-2 with a yield of 96% and a purity of 67.0%. Its HPLC spectrum is as image 3 shown.

Embodiment 3Z907-3

[0043] Take 5g of Z907-2, 250mL of methanol, and 75mL of 10% tetrabutylammonium hydroxide aqueous solution into a 500mL beaker, and stir for 1 hour at room temperature with a magnetic stirrer; the solution is filtered with a filter membrane with a pore size of 1um, and the solid on the filter membrane is discarded. Add 50mL 0.1M HNO to the filtrate 3 The acid solution was acidified, and the pH value was adjusted to 5. During this process, a large amount of black solids were gradually precipitated, and the solution gradually became clear. Then filter with a filter membrane with a pore size of 10 μm to obtain a black solid, which is washed 3 times with 50 mL of water. The obtained solid was dried under vacuum at 50° C. for 10 hours to obtain 4.87 g of product Z907-3 with a yield of 97.4% and a purity of 70.25%. Its HPLC spectrum is as Figure 4 shown.

[0044] Embodiment 4~7 purify ruthenium complex crude product with different amounts of lye

[0045] The Z907 crude product ...

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Abstract

The invention discloses a method for purifying a ruthenium complex crude product through a recrystallization method, which comprises the following steps: A) dissolving 1g of ruthenium complex crude product and 10-20mL of alkali liquor in organic solvent while stirring, and filtering to remove insoluble impurities; B) acidifying the filtrate with dilute acid until the pH value is 3-6, thus precipitating a large amount of solids; C) filtering; D) washing; E) drying; and F) repeating the steps A)-C), or the steps A)-D), or the steps A)-E) 2-5 times, thus obtaining the ruthenium complex product. Through simple acid-base titration and pH value regulation recrystallization, the purity of the ruthenium complex dye can be effectively increased; and the purity of the dye is increased from 52.1% to 70.25% and is increased by 34.8%.

Description

technical field [0001] The invention relates to a method for purifying crude ruthenium complex products. Background technique [0002] A solar cell utilizing sunlight has attracted attention as an energy source to replace fossil fuels, and various researches have been conducted on it. A solar cell is a photoelectric conversion device that converts light energy into electrical energy. Since it uses sunlight as an energy source, it has minimal impact on the earth's environment and can be widely used. Dye-sensitized solar cells (hereinafter referred to as Dye-Sensitized Solar Cell, DSSC) that are sensitized by dyes to induce electron movement do not require expensive manufacturing devices such as vacuum devices due to their high photoelectric conversion efficiency. Moreover, it can be easily manufactured with extremely high productivity using cheap semiconductor materials such as titanium oxide, so it has the potential to become a next-generation solar cell. In recent years, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B67/54C09B57/10
Inventor 詹文海杨松旺李勇明刘岩
Owner 江苏先进无机材料研究院
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