Method for preparing copper chlorophyll and sodium salt thereof from silkworm excrement

A technology of copper chlorophyll and silkworm sand, applied in organic chemistry and other directions, can solve the problems of high explosion-proof requirements in production workshops, affecting the content of finished products, damage, etc., to increase production safety, reduce extraction costs, and simplify the operation process. Effect

Inactive Publication Date: 2013-04-03
INST OF BOTANY JIANGSU PROVINCE & CHINESE ACADEMY OF SCI
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  • Abstract
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  • Application Information

AI Technical Summary

Problems solved by technology

Since underivatized chlorophyll is unstable to light and heat, it is easy to cause damage to chlorophyll during the extraction process and affect the content of the finished product
In addition, the impurity removal process after saponification often uses flammable and toxic organic solvents such as benzene, gasoline, and petroleum ether for extraction, which is prone to environmental pollution during the production process and has high requirements for the explosion-proof performance of the production workshop

Method used

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  • Method for preparing copper chlorophyll and sodium salt thereof from silkworm excrement
  • Method for preparing copper chlorophyll and sodium salt thereof from silkworm excrement
  • Method for preparing copper chlorophyll and sodium salt thereof from silkworm excrement

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preparation example Construction

[0033] 2.1 Preparation of silkworm excrement chlorophyll extract

[0034] Weigh 100g silkworm excrement, add water to moisten it, add 800ml of 90% ethanol, add 12mL of 10% CuSO 4 solution, adjusted to pH 2-3 with hydrochloric acid, and extracted by heating at reflux at 80°C for 6 hours. After filtering, the extract was refrigerated and left standing, and then filtered again to obtain the extract.

[0035] 2.2 Determination of desorption rate of different solvents

[0036] Accurately weigh 6 parts of 0.1 g of NaOH, add 50%, 60%, 70%, 80%, and 95% ethanol respectively to dissolve, and configure alkaline ethanol solutions with different alcohol concentrations.

[0037] Weigh 6 g of pretreated D101 dry resin, put it in a conical flask, and pipette 150.00 mL of chlorophyll extract precisely, 120r min -1 Shake for 24h, filter after full adsorption. Weigh 6 parts of the saturated adsorption resin, each 1.000g, and put them into 6 Erlenmeyer flasks, and add 50%, 60%, 70%, 80%, 95%...

Embodiment 2

[0046] Take 1.0kg of silkworm excrement, wash it with water, remove the sediment, add 4L of 95% ethanol, add hydrochloric acid to adjust pH1, add 10g of CuSO 4 Dissolved in a small amount of water and added to the extract, heated to reflux at 70°C for 4 hours, filtered to obtain the extract. The extract was refrigerated for 24 hours, filtered to obtain the sample solution. Take 330g of HPD-100 macroporous resin and add the chlorophyll extract of silkworm excrement as a sample, first elute with water and 30% ethanol to remove impurities until the eluate is basically colorless, then discard the eluate. Another 70% ethanol was taken, and NaOH was added to adjust the pH to 10 to become alkaline ethanol, which was eluted with 3.3Kg alkaline ethanol, and the eluate was collected. The eluate was concentrated to an alcohol concentration of 20-30%, and the insoluble matter was filtered. Add acid to adjust the pH to 2-3, filter the precipitated precipitate, wash with water until the p...

Embodiment 3

[0048] Take 1.0kg of silkworm excrement, wash it with water, remove the sediment, add 10L of ethanol with a concentration of 80%, add hydrochloric acid to adjust pH4, add 30g of CuSO 4 Dissolve it in a small amount of water and add it to the extract, heat and reflux at 80°C for 6 hours, and filter to obtain the extract. The extract was refrigerated and allowed to stand for 12 hours, then filtered to obtain the sample solution. Take 1000g of NKA macroporous resin and sample the chlorophyll extract from silkworm excrement, first elute with water and 50% ethanol to remove impurities until the eluate is basically colorless, then discard the eluate. Another 60% ethanol was taken, and NaOH was added to adjust the pH to 11 to become alkaline ethanol, which was eluted with 3Kg alkaline ethanol, and the eluate was collected. The eluate was concentrated to an alcohol concentration of 10-20%, and the insoluble matter was filtered. Add acid to adjust the pH to 2-3, filter the precipitat...

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Abstract

The invention discloses a method for preparing copper chlorophyll and a sodium salt thereof from silkworm excrement. The method comprises the following steps of (1) washing the silkworm excrement with water; (2) extracting the silkworm excrement by using acidic ethanol containing CuSO4, standing an extracting solution in cold and filtering; (3) taking a macroporous resin, loading the extracting solution obtained from the step (2), eluting firstly with water and low concentration ethanol and then with an alkaline ethanol solution and collecting the alkaline ethanol eluant; (4) concentrating the alkaline ethanol eluant obtained from the step (3) to a low ethanol concentration, filtering insoluble substances, adjusting a pH value to an acidic state, filtering precipitated precipitate, washing with water until the pH value is in a neutral state, so that the copper chlorophyll is obtained; and (5) adjusting a pH value of the copper chlorophyll obtained from the step (4) to 10-11 by using a NaOH solution, stirring, filtering, and drying the filtrate by concentrating under a reduced pressure or spray drying to obtain the sodium copper chlorophyll. A finished product prepared by the method has high purity, and the method is simple in process and low in cost.

Description

technical field [0001] The invention specifically relates to a method for preparing copper chlorophyllin and its sodium salt from silkworm excrement. Background technique [0002] Silkworm excrement contains a large amount of chlorophyll (chlorophyll). Chlorophyll belongs to the magnesium porphyrin ring complex, which is generally fat-soluble and not easily soluble in water. The magnesium ions in chlorophyll molecules are easily replaced by copper, iron, cobalt and other ions to form chlorophyll derivatives (CPD). Chlorophyll itself is extremely unstable to physical and chemical factors such as light, heat, acid, alkali, and enzymes, while its derivatives are relatively stable, so chlorophyll is generally made into derivatives. Chlorophyll keto acid and its sodium salt are the most widely used chlorophyll derivatives, which are widely used in chemical industry, medicine, food, health care and so on. [0003] There are several typical processes for the preparation of sodium...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D487/22
Inventor 吕寒李维林马丽陈剑任冰如刘艳
Owner INST OF BOTANY JIANGSU PROVINCE & CHINESE ACADEMY OF SCI
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