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A method for degrading black humic acid and brown humic acid to prepare fulvic acid

A technology of brown humic acid and black humic acid, applied in the direction of organic chemistry, can solve the problems of long extraction time, environmental hazards of nitric acid, complicated process, etc., and achieve the effect of improving the extraction rate

Active Publication Date: 2021-12-07
SHANGHAI INST OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The existing fulvic acid extraction methods each have their advantages and disadvantages: (1) the alkali-dissolved acid analysis method is widely used, but the extraction rate of fulvic acid is low, only about 8%, and the extraction time needs about 90 minutes, which is relatively long. (2) Catalyzed oxygen hydrolysis is now mainly carried out by nitric acid to improve the extraction rate of fulvic acid, but nitric acid causes great harm to the environment, and the reaction time is long. In this regard, some researchers use hydrogen peroxide instead of nitric acid oxygen solution, which reduces the pollution to the environment; (3) for organic solvent extractant electrodialysis, ion exchange method, etc., it is mainly used for the extraction of high-purity fulvic acid, such as medical fulvic acid
It is made by extraction, separation, acidification, crystallization, and drying, but the patented process is relatively complicated, and more reagents and drugs need to be added, which reduces the purity of the prepared product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] A method for degrading fulvic acid and black humic acid to prepare fulvic acid, the specific steps are as follows:

[0034] (1) Preparation of black humic acid and brown humic acid powder: fully pulverize black humic acid and brown humic acid into powders with a particle size of 60 mesh respectively with a pulverizer;

[0035](2) Preparation of degradable material: first mix black humic acid and brown humic acid powder prepared in step (1) evenly in a weight ratio of 2:1, dilute with water to a solution state, and then place in a water bath at 50°C While preheating, use microwave pretreatment with a frequency of 200MHz, put the pretreated black humic acid and brown humic acid powder into the autoclave, add ferrous sulfate Fenton (Fenton) reagent and catalyst to the autoclave, set The autoclave pressure was degraded, and the degradation time was 50 minutes to obtain the degraded material;

[0036] Wherein, the ratio of water addition to brown black humic acid is 40:1; ...

Embodiment 2

[0046] A method for degrading fulvic acid and black humic acid to prepare fulvic acid, the specific steps are as follows:

[0047] (1) Preparation of black humic acid and brown humic acid powder: fully pulverize black humic acid and brown humic acid with a pulverizer into powders with a particle size of 70 mesh;

[0048] (2) Preparation of degraded material: first mix black humic acid and brown humic acid powder prepared in step (1) evenly in a weight ratio of 3:1, add water to dilute to a solution state, and then place it in a water bath at 55°C While preheating, use microwave pretreatment with a frequency of 100MHz, put the pretreated black humic acid and brown humic acid powder into the autoclave, add ferrous sulfate Fenton (Fenton) reagent and catalyst into the autoclave, set The autoclave pressure was degraded, and the degradation time was 55 minutes to obtain the degraded material;

[0049] Wherein, the ratio of water addition to brown black humic acid is 30:1;

[0050...

Embodiment 3

[0059] A method for degrading fulvic acid and black humic acid to prepare fulvic acid, the specific steps are as follows:

[0060] (1) Preparation of black humic acid and brown humic acid powder: fully pulverize black humic acid and brown humic acid with a pulverizer into powders with a particle size of 70 mesh;

[0061] (2) Preparation of degraded material: first mix black humic acid and brown humic acid powder prepared in step (1) evenly in a weight ratio of 1:1, add water to dilute to a solution state, and then place it in a water bath at 52°C While preheating, use microwave pretreatment with a frequency of 150MHz, put the pretreated black humic acid and brown humic acid powder into the autoclave, add ferrous sulfate Fenton (Fenton) reagent and catalyst to the autoclave, set The autoclave pressure is degraded, and the degradation time is 40-60 minutes, and the degraded material is obtained;

[0062] Wherein, the ratio of water addition to brown black humic acid is 40:1;

...

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Abstract

The invention relates to a method for degrading black humic acid and brown humic acid to prepare fulvic acid. The black humic acid and brown humic acid are fully pulverized into powder by a pulverizer, and then the degraded slurry is prepared by oxidation. Ultrasonic treatment is used to treat the slurry, and finally the ultrasonically treated slurry is centrifuged to obtain filter residue and supernatant, the filter residue is washed with hot water for several times, and the obtained washing water is mixed with the above supernatant for treatment, and the supernatant is sequentially passed through Concentrate, dry, cool and grind to obtain fulvic acid products. Compared with the prior art, the invention can significantly increase the extraction rate and shorten the extraction time.

Description

technical field [0001] The invention relates to the technical field of utilization of natural source humic substances, in particular to a method for degrading black humic acid and brown humic acid to prepare fulvic acid. Background technique [0002] Humic acid (HA for short) is a natural organic mixture composed of C, H, O, N, S and other elements, among which brown humic acid, black humic acid and fulvic acid are the main ones. Brown humic acid and black humic acid are a kind of humic substances that can be dissolved in alkali solution and precipitated by acid solution. Their molecular weight is larger than that of fulvic acid. The percentages of each element in the molecular composition are: C50~60, H2 .8~6.6, O 31~40, N2.6~6.0. Brown humic acid and black humic acid have lower acidity than fulvic acid, are slightly acidic, and have a higher absorption capacity. Its monovalent salts are soluble in water, and divalent and trivalent salts are insoluble in water, which affec...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07G99/00
CPCC07G99/00
Inventor 张祥郑义陈明良袁宸
Owner SHANGHAI INST OF TECH
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