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Method for preparing humic acid and salt thereof by oxidation and degradation of brown coal

A technology of oxidative degradation and humate, applied in the direction of organic chemistry, can solve the problems of difficult large-scale production, increased extraction rate, environmental pollution, etc., and achieve the effect of increasing yield, improving utilization rate, and simple production process

Inactive Publication Date: 2009-05-06
KUNMING UNIV OF SCI & TECH +4
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Problems solved by technology

Some researchers first use oxidants (commonly used nitric acid, potassium permanganate) to oxidize and degrade lignite, and then use solvent method or alkali-soluble acid precipitation method to extract humic acid. Using this method to extract humic acid, the extraction rate increases. However, nitric acid, potassium permanganate, etc. will pollute the environment
In addition to using chemical oxidants to degrade lignite to increase the extraction rate of humic acid, some scientists also use bio-oxidative degradation to increase the extraction rate of humic acid. Although bio-oxidative degradation has little pollution to the environment, it takes a long time. In addition, a strain of bacteria can only degrade lignite in a certain place, so this method is difficult to be used in large-scale production

Method used

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  • Method for preparing humic acid and salt thereof by oxidation and degradation of brown coal

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Example 1: 100kg120 mesh lignite was added to the reactor, 0.10kg sucrose ester was added, and 250 liters of hydrogen peroxide with a mass fraction of 15% was added in 5 times at 30°C under stirring conditions, and fully stirred at a constant temperature until no large amount of hydrogen peroxide was produced. Until the foam is formed, let it react at room temperature for 12 hours. After the reaction was completed, it was centrifuged, the supernatant was filtered, and the filtrate was concentrated and dried to obtain 19.5 kg of water-soluble fulvic acid crude product. Add concentration of 0.25mol L to the precipitate obtained by centrifugation -1 2,000 liters of NaOH, reacted at 25°C for 20 hours, centrifuged after the reaction was completed, and the concentration of the supernatant was 1mol L -1 neutralized hydrochloric acid to a pH value of 1.5, centrifuged, precipitated and dried to obtain 35.02kg of brown humic acid.

Embodiment 2

[0036] Example 2: 100kg of 70-mesh lignite is added to the reactor, 0.12kg of sucrose ester is added, and 215 liters of hydrogen peroxide with a mass fraction of 17.5% is added in 5 times at 35°C under stirring conditions, and fully stirred at a constant temperature of 35°C until no longer It was allowed to react for 5 hours under the same conditions until a large amount of foam was generated. After the reaction was completed, it was centrifuged, the supernatant was suction filtered, and the filtrate was concentrated and dried to obtain 19.9 kg of crude water-soluble fulvic acid. Add concentration of 1.0mol L to the precipitate obtained by centrifugation -1 500 liters of NaOH, reacted at 25°C for 15 hours, centrifuged after the reaction was completed, and the concentration of the supernatant was 1mol L -1 The hydrochloric acid was neutralized to a pH value of 1.7, centrifuged, precipitated and dried to obtain 34.08kg of brown humic acid.

Embodiment 3

[0037] Example 3: 100kg of 80-mesh lignite was added to the reactor, 0.20kg of sucrose ester was added, and 200 liters of hydrogen peroxide with a mass fraction of 15% was added in 5 times at 40°C under stirring conditions, and fully stirred at a constant temperature of 40°C until no longer It was allowed to react for 40 minutes under the same conditions until foaming occurred. After the reaction was completed, it was centrifuged, the supernatant was filtered, and the filtrate was concentrated and dried to obtain 20.86 kg of crude water-soluble fulvic acid. The concentration of 0.25mol L was added to the residue precipitate after the production of fulvic acid -1 2000 liters of NaOH, reacted at 25°C for 15 hours, centrifuged after the completion of the reaction, and the concentration of the supernatant was 1mol L -1 The hydrochloric acid was neutralized to a pH value of 1.7, centrifuged, precipitated and dried to obtain 33.53kg of brown humic acid.

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Abstract

The invention discloses a method for producing humic acid and salt thereof through the oxidative degradation of young lignite. The method comprises the following steps: carrying out the oxidation reaction of the lignite containing the humic acid and aqueous hydrogen peroxide solution; after the reaction, obtaining water soluble fulvic acid through centrifugal separation, supernatant filtration, concentration and drying; adding alkali into the fulvic acid to prepare a fulvic acid salt product; carrying out the alkaline extraction and centrifugal separation of the residue deposit of the production of the fulvic acid, adding acid into the supernatant till the pH value is 1 to 2, carrying out a reaction at an increased temperature or room temperature, carrying out centrifugal separation after the reaction is finished, and obtaining purified ulmic acid after precipitation and drying; and directly concentrating and drying the supernatant in the previous step to obtain the humate. The method can improve the yield of the fulvic acid and total humic acid in the young lignite, and simultaneously increase the active group in the humic acid. The method can be used for producing fulvic acid, fulvic acid salt, ulmic acid and ulmic acid salt products. In particular, the method puts an end to the environmental pollution caused by the nitric acid which is taken as an oxidation degradation agent. In addition, the method has a short technological line, low cost, simple requirements on equipment, and moderate conditions. The method which can be applied to the industrialized production has good application prospect.

Description

technical field [0001] The invention belongs to the technical field of coal chemical industry, and relates to the production of fulvic acid and its salt, brown humic acid and its salt by taking lignite (young coal) as the basic raw material, carrying out oxidative degradation reaction with oxidizing agent and defoaming agent at a certain temperature method. Background technique [0002] In addition to being used for the production of montan wax, thermal processing, coking, etc., lignite is also a good humic acid raw material. The humic acid content of young lignite with a shallow degree of coalification is generally about 40%, and the yellow humic acid with higher biological activity The acid content is lower. At present, the methods for extracting humic acid and yellow humic acid from lignite include: solvent extraction method and alkali-soluble acid precipitation extraction method. If the above two methods are used to extract humic acid directly from lignite, the extracti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07G99/00
Inventor 李宝才张水花张惠芬角仕云何静戴伟锋刘建珍毕艳艳杨宏博黄昆
Owner KUNMING UNIV OF SCI & TECH
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