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Method for extracting high-purity humic acid from low-rank coal

A humic acid, high-purity technology, applied in organic chemistry and other directions, can solve the problems of high processing cost, complex process operation, long process, etc., and achieve the effect of low impurity element content, simple process operation, and easy industrial production.

Active Publication Date: 2012-07-11
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, patent CN1718615A (2006), although high-purity humic acid can be extracted by using this patent, it is humic acid extracted from soil, and the extraction steps are cumbersome and the process is long
Patent CN101033241A (2007) discloses "a method for the preparation of high-purity humic acid". In this method, raw coal is subjected to alkali dissolution in sequence, centrifuged to remove slag after adding a coagulant, and a complexing agent is added to remove high-valent cations under acidic conditions. After acidification, electrodialysis to remove inorganic salts in the colloidal system can obtain humic acid products with a purity higher than 95%, but more complexing agents and coagulants are used in the extraction process, and electrodialysis is used. The desalination purification process of the dialyzer complicates the process and significantly increases the processing cost. At the same time, the added complexing agent itself is a kind of organic matter, which will eventually enter the product and affect the quality of humic acid.
[0006] Therefore, in order to effectively solve the existing problems of low humic acid content, high impurity content, or high processing cost in the existing method for preparing humic acid from low-rank coal, the present invention is proposed

Method used

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  • Method for extracting high-purity humic acid from low-rank coal
  • Method for extracting high-purity humic acid from low-rank coal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The air-dried lignite (humic acid content 38%) is crushed and ground to a particle size of not more than 1.0mm in advance, and then the ground coal sample is mixed with 0.15mol / L sodium pyrophosphate solution (the mass ratio of coal sample to sodium pyrophosphate solution 1:8), heated in a water bath at 95°C for 1.0 h, nitrogen gas was introduced and stirred during the heating process; after the extraction process was completed, the mixed solution was poured out and centrifuged at a speed of 3000 r / min, and the centrifugation time was 30 min. The supernatant and precipitate were collected separately. Repeat the above water bath stirring extraction and centrifugation process for the precipitate once. Combine the supernatant obtained twice, add 6mol / L HCl to it to adjust the pH to 2.0, after standing still, use a siphon to absorb most of the supernatant, discard it, and centrifuge again at a speed of 3000r / min, and the centrifugation time is 30min , to collect the precip...

Embodiment 2

[0032]The mixture of air-dried lignite and weathered coal (humic acid content 35%) is crushed and ground to a particle size not greater than 1.0mm, and then the ground coal sample is mixed with 0.05mol / L sodium hydroxide solution (coal sample and hydroxide After the mass ratio of the sodium solution is 1:9), heat in a water bath at a temperature of 80°C for 1.5h, feed nitrogen and stir during the heating process; after the extraction process is completed, pour out the mixed solution and centrifuge at a speed of 5000r / min, The separation time was 20minmin, and the supernatant liquid and precipitate were collected respectively. Repeat the above water bath stirring extraction and centrifugation process for the precipitate once. Combine the supernatant obtained twice, add 6mol / L HCl to it to adjust the pH to 2.0, after standing still, use a siphon to absorb most of the supernatant, discard it, and centrifuge again at a speed of 5000r / min, and the centrifugation time is 20min , to...

Embodiment 3

[0034] The mixture of air-dried lignite and peat (44.7% humic acid content) was crushed and ground to a particle size not greater than 1.0mm, and then the ground coal sample was mixed with 0.25mol / L sodium carbonate solution (the ratio of coal sample to sodium carbonate solution After the mass ratio is 1:10), heat in a water bath at a temperature of 50°C for 2.0h, feed nitrogen gas and stir during the heating process; after the extraction process is completed, pour out the mixed solution for centrifugation at a speed of 10000r / min, and the centrifugation time is 10minmin, collect the supernatant and precipitate respectively. Repeat the above water bath stirring extraction and centrifugation process for the precipitate once. Combine the supernatant obtained twice, add 6mol / L HCl to it to adjust the pH to 2.0, and after standing still, use a siphon to absorb most of the supernatant, discard it, and centrifuge again at a speed of 10000r / min, and the centrifugation time is 10min ...

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Abstract

The invention discloses a method for extracting high-purity humic acid from low-rank coal. In the invention, abundant low-quality peat, lignite, weathered coal and the like in china are used as raw materials; and processes such as repeated base-dissolving acidification, centrifugal separation, mixed acid treatment, semi-permeable membrane dialysis, freeze drying and the like are carried out to separate and obtain a high-purity humic acid product with a humic acid content not lower than 97%. Compared with the traditional base-dissolving acidification method and the existing high-purity humic acid preparation method, the method has the advantages of low processing cost, simplicity and convenience in technological operation, high product purity, low impurity element content and the like. The high-purity humic acid prepared by the method can be applied to cathode plate expanding agents of lead storage batteries, medical products and the like, and can be used as a chemical reagent for related basic researches of humic acid substances and an important raw material for synthesis of organic polymers.

Description

technical field [0001] The invention discloses a method for extracting high-purity humic acid from low-grade coal, in particular to a method for separating and extracting high-purity humic acid (Humic Acid, code-named HA) from low-grade coal; it belongs to the technical field of coal processing and chemical industry , the obtained product belongs to the category of fine chemicals. Background technique [0002] my country is rich in low-quality coal resources (including peat, lignite, weathered coal, etc.), but because such resources contain a lot of inorganic minerals, it is difficult to separate and remove them by simple physical separation methods, so it has not yet been widely used. scale development and utilization. [0003] Humic acid is mainly divided into three categories: soil humic acid, coal humic acid and water humic acid. According to the solubility in acid and alkali solution, humic acid can be further divided into fulvic acid (FA), humic acid (HA) and humin (h...

Claims

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Application Information

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IPC IPC(8): C08H99/00C07G99/00
Inventor 张元波姜涛李光辉范晓慧李鹏周友连韩桂洪郭宇峰杨永斌黄柱成许斌李骞陈许玲游志雄段道显黄艳芳苏子健罗伟吴玉东
Owner CENT SOUTH UNIV
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