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Method for preparing copper chlorophyll acid from silkworm litter

A technology of chlorophyll cupric acid and silkworm sand, which is applied in organic chemistry and other directions, can solve the problems of long production process and achieve the effects of reducing dosage, shortening process, reducing material consumption and energy consumption

Inactive Publication Date: 2013-08-07
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to overcome the defect of long production process of chlorophyll cupric acid at present, and provide a preparation method of chlorophyll cupric acid with simpler process flow

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0018] A method for preparing chlorophyll cupric acid, using silkworm excrement as raw material, comprising the following steps:

[0019] (1) Dilute the concentration to 0.40 g·mL -1 The aqueous sodium hydroxide solution and ethanol were mixed at a volume ratio of 6:4 to prepare an ethanol-sodium hydroxide two-phase aqueous system with a total volume of 1 L.

[0020] (2) Add 10 g of silkworm excrement into the ethanol-sodium hydroxide two-phase aqueous system in step (1), shake and mix, stir and react at 60°C for 2 h, then stand still for phase separation, and separate the upper phase.

[0021] (3) Adjust the pH value of the upper phase to 2 with hydrochloric acid, then add 20% CuSO 4 Solution 4mL, reacted at 60 °C for 2 h, filtered with suction, and dried the filter residue to obtain crude chlorophyll cupric acid.

[0022] (4) The crude chlorophyll cupric acid was washed once with 10 mL of distilled water, 10 mL of petroleum ether, and 10 mL of 40% ethanol, filtered, and t...

Embodiment 2

[0024] A method for preparing chlorophyll cupric acid, using silkworm excrement as raw material, comprising the following steps:

[0025] (1) Dilute the concentration to 0.40 g·mL -1 The aqueous sodium hydroxide solution and ethanol were mixed at a volume ratio of 3:7 to prepare an ethanol-sodium hydroxide two-phase aqueous system with a total volume of 1 L.

[0026] (2) Add 10 g of silkworm excrement into the ethanol-sodium hydroxide two-phase aqueous system in step (1), shake and mix, stir and react at 60°C for 2 h, then stand still for phase separation, and separate the upper phase.

[0027] (3) Adjust the pH value of the upper phase to 2 with hydrochloric acid, then add 20% CuSO 4 Solution 4mL, reacted at 60 °C for 2 h, filtered with suction, and dried the filter residue to obtain crude chlorophyll cupric acid.

[0028] (4) The crude chlorophyll cupric acid was washed once with 10 mL of distilled water, 10 mL of petroleum ether, and 10 mL of 40% ethanol, filtered, and t...

Embodiment 3

[0030] A method for preparing chlorophyll cupric acid, using silkworm excrement as raw material, comprising the following steps:

[0031] (1) Dilute the concentration to 0.40 g·mL -1 The aqueous sodium hydroxide solution and ethanol were mixed at a volume ratio of 3:7 to prepare an ethanol-sodium hydroxide two-phase aqueous system with a total volume of 1 L.

[0032] (2) Add 20 g of silkworm excrement into the ethanol-sodium hydroxide two-phase aqueous system in step (1), shake and mix, stir and react at 60°C for 2 h, then stand still for phase separation, and separate the upper phase.

[0033] (3) Adjust the pH value of the upper phase to 2 with hydrochloric acid, then add 20% CuSO 4 Solution 4mL, reacted at 60 °C for 2 h, filtered with suction, and dried the filter residue to obtain crude chlorophyll cupric acid.

[0034] (4) The crude chlorophyll cupric acid was washed once with 10 mL of distilled water, 10 mL of petroleum ether, and 10 mL of 40% ethanol, filtered, and t...

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PUM

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Abstract

The invention provides a method for preparing copper chlorophyll acid from silkworm litter, relating to the technical field of preparation of copper chlorophyll acid. The method comprises the following steps: directly saponifying chlorophyll in silkworm litter in an ethanol-sodium hydroxide dual-water-phase system, and meanwhile, extracting generated saponified chlorophyll to the upper phase of the dual-water-phase system; separating out the upper phase of the dual-water-phase system, and acidifying to replace copper to obtain a copper chlorophyll acid crude product; and washing with distilled water, petroleum ether and 40-50% ethanol to obtain the refined copper chlorophyll acid. Compared with the traditional technique, the invention shortens the technical process, reduces the consumption of organic solvents, and lowers the material consumption and energy consumption. The invention overcomes the defects of long technical process, high consumption of organic solvents, high material consumption and high energy consumption.

Description

technical field [0001] The invention relates to the technical field of preparation of chlorophyll cupric acid, in particular to a method for preparing chlorophyll cupric acid from silkworm excrement. Background technique [0002] Sodium copper chlorophyllin is a natural food coloring approved by the Food and Agriculture Organization of the United Nations, the World Health Organization and my country’s Food Additives Standards Committee. Compared with chlorophyll, sodium copper chlorophyllin is stable and resistant to processing, and is widely used in the food and pharmaceutical industries. . Chlorophyll cupric acid is an important intermediate for preparing sodium copper chlorophyllin. The traditional method of preparing chlorophyll cupric acid mainly includes the following processes: ① Preparation of paste chlorophyll by organic solvent extraction; ② Preparation of sodium chlorophyllin by saponification of pasty chlorophyll; ③ Preparation of crude chlorophyll cuprate by aci...

Claims

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Application Information

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IPC IPC(8): C07D487/22
Inventor 王赟韩娟马晶晶吴迎春胡钰涛倪良
Owner JIANGSU UNIV
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