Method for producing sodium copper chlorophyllin through supercritical purification
A sodium copper chlorophyllin, supercritical technology, applied in the production of bulk chemicals, organic chemistry, etc., can solve the problems of inability to use supercritical purification, improve product quality and food and medicine safety, high selectivity, and increase yield Effect
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Embodiment 1
[0034] A method for producing sodium copper chlorophyllin by supercritical purification, comprising the following steps:
[0035] (1) saponification: first adding 2 to 6 parts by weight of ethanol solvent in 1 part of pasty chlorophyll for dissolving, 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;
[0036] (2) Washing: the saponified chlorophyll is extracted and washed 3 times with gasoline;
[0037] (3) Copperization: add copper chloride that is 0.1 part by weight to the saponified chlorophyll after washing, insulate at 33° C., and copperize for 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 in 2 parts by weight of pasty chlorophyll to dissolve, wherein the mass fraction of chlorophyll in the 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: the saponified chlorophyll is extracted and washed 3 times with gasoline;
[0045] (3) Copperization: add copper chloride that is 0.2 parts by weight to the saponified chlorophyll after washing, insulate at 48° C., and copperize for 3 hours;
[0046] (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;
[0047] (5) Finished product: 0.02 part by weight of sodium hydroxide with a mass fraction of 97.5% is added to the purified coppe...
Embodiment 3
[0050] A method for producing sodium copper chlorophyllin by supercritical purification, comprising the following steps:
[0051] (1) Saponification: first add 3.2 to 9.6 parts of acetone solvent in the pasty chlorophyll of 1.6 parts by weight to dissolve, wherein the mass fraction of chlorophyll in the 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;
[0052] (2) Washing: the saponified chlorophyll is extracted and washed 3 times with gasoline;
[0053](3) Copperization: add copper chloride that is 0.16 parts by weight to the saponified chlorophyll after washing, insulate at 37° C., and copperize for 3 hours;
[0054] (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;
[0055] (5) Finished product: Add 0.016 parts by weight of sodium hydroxide with a mass fraction of 95.9% t...
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