Method for producing sodium copper chlorophyllin through supercritical purification
A sodium copper chlorophyllin and supercritical technology, which is applied in the production of bulk chemicals, chemical instruments and methods, azo dyes, etc., can solve problems such as inability to use supercritical purification, and improve product quality, food and medicine safety, and poor selectivity , highly selective effect
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Embodiment 1
[0033] A method for producing sodium copper chlorophyllin by supercritical purification, comprising the following steps:
[0034] (1) Saponification: First, 1 part by weight of pasty chlorophyll is dissolved by adding 2 to 6 parts by weight of ethanol solvent, wherein the mass fraction of chlorophyll in the pasty chlorophyll is 12%, and the water content is 23%; Then add the liquid caustic soda that is 0.3~0.8 parts by weight and keep saponification reaction at 60 DEG C for 1 hour;
[0035] (2) Washing: extract and wash the saponified chlorophyll with gasoline for 3 times;
[0036] (3) Copperization: Add 0.1 parts by weight of copper chloride to the saponified chlorophyll after washing and keep it warm at 33°C.
[0037] 3 hours;
[0038] (4) Purification: Use supercritical carbon dioxide to purify and remove impurities for 2 hours at a pressure of 15MPa and a temperature of 36°C;
[0039] (5) Finished product: 0.01 part by weight of sodium hydroxide with a mass fraction of ...
Embodiment 2
[0042] A method for producing sodium copper chlorophyllin by supercritical purification, comprising the following steps:
[0043] (1) Saponification: First, add 4 to 12 parts of methanol solvent to 2 parts by weight of pasty chlorophyll for dissolution, wherein the mass fraction of chlorophyll in pasty chlorophyll is 10%, and the water content is 20%; then add 0.6 ~1.6 parts of liquid caustic soda are kept saponified at 60°C for 1 hour;
[0044] (2) Washing: extract and wash the saponified chlorophyll with gasoline for 3 times;
[0045] (3) Copperization: Add 0.2 parts by weight of copper chloride to the saponified chlorophyll after washing and keep it warm at 48°C.
[0046] 3 hours;
[0047] (4) Purification: Use supercritical carbon dioxide to purify and remove impurities for 2 hours at a pressure of 27MPa and a temperature of 48°C;
[0048] (5) Finished product: 0.02 part by weight of sodium hydroxide with a mass fraction of 97.5% is added to the purified copperized chlo...
Embodiment 3
[0051] A method for producing sodium copper chlorophyllin by supercritical purification, comprising the following steps:
[0052] (1) Saponification: First, add 3.2 to 9.6 parts of acetone solvent to 1.6 parts by weight of pasty chlorophyll for dissolution, wherein the mass fraction of chlorophyll in pasty chlorophyll is 14.3%, and the water content is 23.7%; then add 0.48 ~1.28 parts of liquid caustic soda are incubated and saponified at 60°C for 1 hour;
[0053] (2) Washing: extract and wash the saponified chlorophyll with gasoline for 3 times;
[0054] (3) Copperization: Add 0.16 parts by weight of copper chloride to the saponified chlorophyll after washing and keep it warm at 37°C.
[0055] 3 hours;
[0056] (4) Purification: Use supercritical carbon dioxide to purify and remove impurities for 2 hours at a pressure of 35MPa and a temperature of 65°C;
[0057] (5) Finished product: add 0.016 parts by weight of sodium hydroxide with a mass fraction of 95.9% to the purified ...
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