A kind of preparation method of chlorophyll copper acid and copper sodium salt

A technology of chlorophyll cupric acid and copper sodium salt, applied in chemical instruments and methods, azo dyes, organic dyes, etc., can solve the problems of many recovery and storage equipment, time, and large amount of organic reagents.

Active Publication Date: 2015-08-12
YANTAI INST OF COASTAL ZONE RES CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The traditional technology has some disadvantages, such as long production cycle, the traditional technology uses organic solvents to repeatedly extract and remove impurities after the saponification step, and it takes a long time for the separation of the two liquids in the extraction to separate into layers, so it takes up equipment and consumes a lot time; the amount of organic reagents is large, the recovery is difficult, and a large amount of organic solvents are used to extract and remove impurities, and the required recovery and storage equipment are many, so the consumption is large and the cost is high; the yield is low, and the chlorophyll itself is easy to decompose. There is also a certain amount of loss in addition to organic solvent extraction, which results in a lower final yield

Method used

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  • A kind of preparation method of chlorophyll copper acid and copper sodium salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Example 1 Preparation of chlorophyll cupric acid and copper sodium salt from fresh Rumex.

[0029] Weigh 10kg fresh Rumex stems and leaves, add 20g CaCO 3 , add 40L of 90% ethanol solution, beating, and the extraction temperature is controlled at 50°C. Squeeze the slurry with a belt press, collect 47.5L of juice, and remove waste residue. After the juice is roughly filtered with a 180-mesh filter cloth, it is centrifuged at a high speed at a speed of 4000 rpm to remove waste residue. Adjust the pH to 11 with 5% NaOH solution, control the temperature at 45° C. and concentrate under reduced pressure while performing saponification to obtain 11.5 L of concentrated saponified liquid. The saponified solution was adjusted to pH 2 with hydrochloric acid, and 10% CuSO was added 4 The solution was 230ml, and the temperature was controlled at 75°C for 1.0h. After filtration under reduced pressure, the precipitate was washed three times with deionized water at a temperature of...

Embodiment 2

[0030] Example 2 Preparation of chlorophyll cupric acid and copper sodium salt from fresh spinach.

[0031] Weigh 10kg fresh spinach stems and leaves, add 40g CaCO 3 , add 60L of 95% ethanol solution, make a slurry, and control the extraction temperature at 55°C. The slurry is squeezed by a belt press, and 67L of juice is collected to remove waste residue. After the juice is coarsely filtered with a 250-mesh filter cloth, it is centrifuged at a high speed at a speed of 6000 rpm to remove waste residue. Adjust the pH to 12 with 5% NaOH solution, control the temperature at 50° C. and concentrate under reduced pressure while performing saponification to obtain 13.3 L of concentrated saponified liquid. The saponified solution was adjusted to pH 2.7 with hydrochloric acid, and 10% CuSO was added 4 The solution was 300ml, and the temperature was controlled at 70°C for 1.5h. After filtration under reduced pressure, the precipitate was washed three times with deionized water at a ...

Embodiment 3

[0032] Example 3 Preparation of chlorophyll cupric acid and copper sodium salt from fresh spinach.

[0033] Weigh 10kg fresh spinach stems and leaves, add 50g CaCO 3 , add 50L of 95% ethanol solution, make a slurry, and control the extraction temperature at 60°C. Squeeze the slurry with a belt press, collect 55L of juice, and remove waste residue. After the juice is coarsely filtered with a 300-mesh filter cloth, it is centrifuged at a high speed at a speed of 5000 rpm to remove waste residue. Adjust the pH to 12 with 5% NaOH solution, control the temperature at 60° C. and concentrate under reduced pressure while performing saponification to obtain 12 L of concentrated saponified liquid. The saponified solution was adjusted to pH 3 with hydrochloric acid, and 10% CuSO was added 4 The solution was 400ml, and the temperature was controlled at 60°C for 1.5h. After filtration under reduced pressure, the precipitate was washed three times with deionized water at a temperature o...

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Abstract

The invention discloses a method for preparing chlorophyll cuprate and sodium copper chlorophyll. The method comprises the following steps: taking fresh plant stem leaves, adding 90-95% of ethanol, pulping and extracting, and pressing and juicing; roughly filtering the juice by using a gauze of 180-300 meshes, and subsequently carrying out high-speed centrifugation with the speed of 4,000-6,000rpm; adding 5% of a NaOH solution and adjusting the pH value to be 11-12, saponifying, carrying out vacuum concentration and recycling the ethanol; adjusting the pH value to be 2-3, adding 10% of CuSO4 solution for copper substitution; subsequently sequentially washing sediment obtained from suction filtration in warm water for three times and washing the sediment in a low-degree ethanol solution for three times; directly drying the obtained sediment so as to obtain chlorophyll cuprate solid powder; dissolving the washed sediment by using acetone; adding 5% of a NaOH ethanol solution to adjust the pH value to be 10-12, washing the sediment, and drying the sediment after suction filtration so as to obtain sodium copper chlorophyll solid powder. The recycling rate of the method is 0.7-1.0%, and the prepared sodium copper chlorophyll meets various requirements of the GB36406-2011 standard. According to the method, as two time-consumption steps of concentration and saponification are combined together, the time is greatly shortened, the step of organic solvent extraction is eliminated, the process is simplified, and the cost is lowered.

Description

technical field [0001] The invention relates to a preparation process of cupric acid and copper sodium salt, in particular to a preparation process for producing chlorophyll cupric acid and copper sodium salt. Background technique [0002] Chlorophyll is commonly found in plants in nature. It is a green pigment developed earlier and one of the most widely distributed natural pigments on the earth. Chlorophyll is natural, non-toxic and edible, and can be widely used as colorant and deodorant in food and cosmetics. However, free chlorophyll is unstable, and it will change color instantly when it encounters light, oxygen, acid and alkali, etc., and chlorophyll is extremely difficult to dissolve in water, which limits the use of chlorophyll. Therefore, the development and utilization of chlorophyll is mainly to make chlorophyll copper sodium salt for use. [0003] Chlorophyll copper sodium salt is obtained through a series of changes in chlorophyll. The chlorophyll salt is de...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D487/22C09B61/00
CPCC07D487/22C09B61/00
Inventor 衣悦涛靳志明冯大伟刘胜一
Owner YANTAI INST OF COASTAL ZONE RES CHINESE ACAD OF SCI
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