Production method of sodium copper chlorophyllin

A copper chlorophyllin sodium salt and a production method technology are applied in the fine chemical industry to prepare natural pigments, which can solve the problems of large solvent consumption, multiple equipment, and lower yields, and reduce equipment investment, increase product yields, and save energy. clear effect

Active Publication Date: 2014-02-26
四川通世达生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the saponification reaction, ethanol (or acetone) and gasoline (or petroleum ether) are used to dissolve the saponification reactants to form a liquid-liquid separation, and the two liquids need to stand for a long time before they can be layered and separated, so Takes up too much equipment and consumes a lot of time
[0005] 2. Large solvent consumption and high energy consumption
Due to the need for large doses of gasoline (or petroleum ether) to dissolve the unsaponifiable matter many times, the consumption is large (more than 30 times), and the recovery temperature is high, resulting in large consumption, high energy consumption and high cost
[0006] 3. Low yield
Due to liquid-liquid separation, there is always a transition zone between the two liquids, the interface is not easy to control, and it is easy to cause losses and reduce the yield.

Method used

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  • Production method of sodium copper chlorophyllin

Examples

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Effect test

Embodiment 1

[0021] Such as figure 1 As shown, Example 1: A method for producing sodium copper chlorophyllin, using pasty chlorophyll as a raw material, including the following steps:

[0022] a. Saponification separation: directly add NaOH solution to the paste chlorophyll and stir to PH=12~14, control the temperature at 50℃, react for 60 minutes, control the stirring speed to 80 r / min, add paste to the reactant after the saponification reaction Dissolve 3 times the weight of chlorophyll in acetone, the temperature is controlled at 40℃, the stirring speed is controlled at 100 r / min to form a solid and liquid phase. The saponified solid is obtained by solid-liquid filtration, and then 1 to 2 times the acetone is added to repeatedly wash 2~4 times;

[0023] b. Copper crystals: Add 4 times the weight of pure water to the saponified solid obtained after saponification and separation to dissolve, and then add 3% CuSO by weight of paste chlorophyll 4 , Control the temperature to 50°C, and place the...

Embodiment 2

[0027] Example 2: A method for producing sodium copper chlorophyllin, using pasty chlorophyll as a raw material, including the following steps:

[0028] a. Saponification separation: directly add NaOH solution to the paste chlorophyll and stir to PH=12~14, control the temperature at 40℃, react for 90 minutes, control the stirring speed to 120 r / min, add the paste to the reactant after the saponification reaction Dissolve 5 times the weight of chlorophyll in acetone, the temperature is controlled at 45℃, and the stirring speed is controlled at 160 r / min to form a solid and liquid phase. The saponified solid is obtained through solid-liquid filtration, and then 1 to 2 times of acetone is added to repeatedly wash 2~4 times;

[0029] b. Set copper crystals: add 5 times the weight of pure water to dissolve the saponified solid obtained after saponification and separation, and then add 4% CuSO by weight of paste chlorophyll 4 , Control the temperature to 60°C, and set the copper for 30 m...

Embodiment 3

[0032] Example 3: A method for producing sodium copper chlorophyllin, using pasty chlorophyll as a raw material, including the following steps:

[0033] a. Saponification separation: directly add NaOH solution to the paste chlorophyll and stir to PH=12~14, control the temperature at 60℃, react for 70 minutes, control the stirring speed to 60 r / min, add paste to the reactant after the saponification reaction Dissolve 4 times the weight of chlorophyll in acetone, the temperature is controlled at 35℃, the stirring speed is controlled at 80 r / min to form a solid and liquid phase, the saponified solid is obtained by solid-liquid filtration, and then 1 to 2 times of acetone is added to repeatedly wash 2~4 times;

[0034] b. Copper crystals: Add 4 times the weight of pure water to the saponified solid obtained after saponification and separation to dissolve, and then add 3% CuSO by weight of paste chlorophyll 4 , Control the temperature to 55°C, set the copper for 30 minutes, after the co...

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Abstract

The invention discloses a production method of sodium copper chlorophyllin. With chlorophyll paste as the raw material, the method comprises the steps of: adding a NaOH solution into the chlorophyll paste for a saponification reaction, then conducting saponification and separation, adding copper for crystallization, precipitation and purification, salt formation and drying, thus obtaining a sodium copper chlorophyllin finished product. The solid and liquid are separated during the whole production course. The production method of the invention thoroughly solves various disadvantages of liquid-liquid separation in prior art, eradicates labour-consuming and time-consuming liquid-liquid separation difficult to control in production, and realizes solid-liquid separation in the whole course, thus reducing equipment investment by 30%, saving energy and reducing consumption by 40%, enhancing product yield by over 5%. The production method provided in the invention has the characteristics of high production efficiency, less solvent kind, obvious energy saving and emission reduction effect, as well as low production cost, etc.

Description

Technical field [0001] The invention relates to a method for preparing natural pigments from fine chemicals, in particular to a method for producing sodium copper chlorophyllin. Background technique [0002] The traditional process of using pasty chlorophyll to produce sodium copper chlorophyll is: paste chlorophyll is added to two solvents to dissolve and saponify, and then separated → ethanol is added to adjust the saponification solution, and then copper sulfate is added to set copper → washed with water, ethanol, petroleum ether and purified → The refined copper acid is placed in sodium to form a salt, filtered and dried to obtain sodium copper chlorophyllin. The invention patent "Patent No. ZL200710061547.2", the invention patent "Patent No. ZL01128942.2" and other processes are mostly used for saponification of ethanol (or acetone) and gasoline (or petroleum ether) two solvents to repeatedly dissolve, wash, stand for stratification, liquid-liquid Separate the saponifiable ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D487/22C09B61/00
Inventor 周定志樊平原朱万岭
Owner 四川通世达生物科技有限公司
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