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A kind of preparation method of chlorophyll copper sodium salt

A technology for chlorophyll copper sodium salt and paste chlorophyll is applied in the field of preparation of chlorophyll copper sodium salt, which can solve the problems of large loss of concentration and recovery, high cost of organic solvents, affecting production efficiency, etc., and achieves improvement of color value conversion rate and reduction of production. cost, health benefits

Active Publication Date: 2022-08-09
云南博瑞生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Traditional method has following shortcoming: 1, need to use a large amount of organic solvents (acetone, ethanol etc.) to carry out saponification separation, and carry out organic solvent (ethanol, acetone, ether, gasoline etc.) washing with copper chlorophyllin sodium salt behind the copper, The cost of organic solvent is high, the loss of concentration recovery is large, and the heat energy consumption is large
2. The use of organic solvents for washing and purification requires standing and settling, and the settling time is too long, which affects production efficiency
3. The conversion rate of color value is low. Due to solvent washing and purification, the critical point of washing is not easy to control. Sometimes a large amount of pigment is washed down as waste liquid, and sometimes the washing is not sufficient, and the color value after salt formation cannot meet the national standard requirements.
4. Due to the use of a large amount of organic solvents, there are high requirements for the operating environment (need to be equipped with corresponding organic solvent alarms, etc.), and the operators will be more or less exposed to organic solvents, which is not conducive to the health of the operators

Method used

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

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0020] A preparation method of copper chlorophyll sodium salt, comprising the steps:

[0021] (1) Weigh 344.8g of chlorophyll crude paste (E1%1CM: 22.7), add 3BV 3.5% NaOH aqueous solution, electric stirring (200RPM) 55 ℃ thermal insulation saponification for 6h, the net weight of saponification paste after saponification: 1209.52g, after saponification, E1%1CM ( 405+-3nm) is 40.0, w 1 : 4.63 (detection method is GB26406-2011).

[0022] (2) Separation of saponified matter: add 1BV pure water to the above saponified paste, and centrifuge with a centrifuge after electric stirring for 1 hour. Take the supernatant and put it into copper (5.0% anhydrous copper sulfate of the quality of the crude paste, add 5BV water to dilute and dissolve) , while adding copper sulfate solution and stirring (rotation speed: 250RPM), 55 ℃ water bath heating and placing copper for 2h, after placing copper solution E1% 1CM: 13.3, w 1 : 3.72, water content (detected by a rapid moisture meter): 90.39%...

Embodiment 2

[0052] In order to further verify the feasibility of the new process, it is verified by a larger amount. A preparation method of copper chlorophyll sodium salt, comprising the steps:

[0053] (1) Weigh 1kg of chlorophyll crude paste (E1% 1CM: 22.7), add 3BV 3.5% NaOH aqueous solution, electric stirring (200RPM) 55 ℃ insulation saponification for 6h, saponification paste net weight after saponification: 3.97kg, after saponification E1% 1CM (405 +-3nm) is 40.5, w 1 : 4.60 (detection method is GB26406-2011).

[0054] (2) Separation of saponified matter: add 1BV pure water to the above saponified paste, and centrifuge with a centrifuge after electric stirring for 1 hour. Take the supernatant and carry out copper substitution (3.2% anhydrous copper sulfate of the quality of the crude paste is added, and 5BV water is added to dilute and dissolve) , while adding copper sulfate solution and stirring (rotation speed: 250RPM), 55 ℃ copper substitution for 2h, copper substitution solut...

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Abstract

The invention belongs to the technical field of separation and extraction of active ingredients of natural products, and in particular relates to a preparation method of copper chlorophyll sodium salt; a preparation method of copper chlorophyll sodium salt, comprising the following steps: S1, saponification: taking viscous paste chlorophyll, adding NaOH aqueous solution, keep the constant temperature of 55 ℃ for saponification with electric stirring for 6h; S2, separation: after the saponification is completed, continue to add 1BV pure water and stir until the dissolution is uniform, and centrifuge with a high-speed centrifuge. liquid to set copper; S3, set copper: add CuSO with 5% mass of viscous paste 4 , dissolved in 5BV water, while adding CuSO 4 The aqueous solution is stirred at a constant temperature of 50 °C for 2.5 hours; S4, precipitation purification: take the filtrate and filter it with a hollow fiber membrane, then concentrate it, and test it; using this method has the advantages of high production efficiency, environmental protection, and no purification and purification with organic solvents. The chlorophyll copper sodium salt is prepared, and the production cost is greatly reduced.

Description

technical field [0001] The invention belongs to the technical field of separation and extraction of active ingredients of natural products, and particularly relates to a preparation method of copper chlorophyll sodium salt. Background technique [0002] The traditional process of using sticky chlorophyll to prepare copper chlorophyll sodium salt is as follows: sticky chlorophyll is saponified by adding alkali in acetone and ethanol, or first adding alkali saponification, then washing with acetone → adding copper sulfate and placing copper → using acid water, ethanol, Acetone, ether, gasoline, etc. are washed to remove impurities → concentrated and dried finished products. Among them, there are invention patents "Patent No. ZL200710061547.2" and "Patent No. ZL01128942.2", in the process of saponification, ethanol and acetone are used to repeatedly wash and remove impurities. After copper is placed, ethanol or (or acetone), gasoline, ether Wait for further washing and purific...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D487/22
CPCC07D487/22Y02P20/10
Inventor 鲁恒李丽梅祝涛王能昆白富庭
Owner 云南博瑞生物科技有限公司