CN107141321A - The method that fulvic acid is extracted from lignite - Google Patents
The method that fulvic acid is extracted from lignite Download PDFInfo
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- CN107141321A CN107141321A CN201710465617.4A CN201710465617A CN107141321A CN 107141321 A CN107141321 A CN 107141321A CN 201710465617 A CN201710465617 A CN 201710465617A CN 107141321 A CN107141321 A CN 107141321A
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- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
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Abstract
The present invention relates to a kind of extraction process of coal humic acid, a kind of method that fulvic acid is extracted from lignite is specifically disclosed, is comprised the following steps：A, lignite are crushed；B, oxidative degradation；C, while being carried out in ultrasonic cleaner ultrasonically treated after adding the water mixing of metering, it will be stirred while ultrasonically treated in degraded slurry injection ultrasonic cleaner；D, post processing.It is an advantage of the invention that：1) method using ultrasonic cleaner ultrasonic agitation processing lignite degraded slurry is proposed, the yield of fulvic acid is improved；2) propose after oxidative degradation completion, then the method that ultrasonic agitation is carried out to product degradation slurry, it is to avoid over oxidation.
Description
Technical field
The present invention relates to a kind of Coal dressing method, especially a kind of extraction process of coal humic acid.
Background technology
Humic acid is animal and plant body remains by producing one under biochemistry, physical chemistry and geochemistry collective effect
Plant complicated natural macromolecular organic monoacid.According to the size of solubility of the humic acid in different solvents, color and molecular weight,
Humic acid can be divided into humic acid, ulmic acid and fulvic acid.Fulvic acid can be dissolved in water, acid, alkali, ethanol and acetone etc., and divide
Son amount is smaller, is the larger class organic monoacid of bioactivity.
In summary, fulvic acid has the features such as molecular weight is smaller, active function groups are more and soluble in water, commonly used
In agricultural, animal husbandry.Apply in agricultural, fulvic acid energy improved soil, the utilization rate for improving nutrient (nitrogen, phosphorus, potassium), stimulation
Plant growth, the toxicity for promoting crop resistance, improvement agricultural product quality and reduction agricultural chemicals；Apply in animal husbandry, Xanthohumate
Used usually as feed addictive, can effectively improve yield and prevention disease.
At present, fulvic acid content intrinsic in mineral resources lignite is very low, directly using causing utilization rate low, causes resource wave
Expense is, it is necessary to which oxidative degradation is used after improving fulvic acid content.Oxidant used at this stage mainly has ozone, permanganic acid
Potassium, hydrogen peroxide and nitric acid, it is common in the majority using hydrogen peroxide and nitric acid as oxidizing degraded lignite production fulvic acid, but nitric acid
Oxidative degradation lignite production fulvic acid has substantial amounts of nitrogen oxides and produced, and causes environmental pollution.Current lignite oxidative extraction is yellow
The subject matter that the technique of rotten acid is present is that fulvic acid yield is not high, probe into how to improve fulvic acid yield be this area weight
Want problem.
The content of the invention
To improve the yield that oxidative degradation lignite produces fulvic acid, fulvic acid is extracted from lignite the invention provides one kind
Method.
The technical solution adopted in the present invention is：The method that fulvic acid is extracted from lignite, comprises the following steps：
A, crushing：Lignite is crushed and obtains brown coal powder；
B, oxidative degradation：Oxidant is added into brown coal powder oxidative degradation is carried out to brown coal powder, obtain slurry of degrading；
C, ultrasonic agitation：Degraded slurry is injected in ultrasonic cleaner, while adding after the water mixing measured in ultrasound
Carry out ultrasonically treated in ripple washer, be stirred while ultrasonically treated, obtain ultrasonically treated slurry；
D, post processing：Ultrasonically treated slurry is centrifuged obtaining filter residue and supernatant, and supernatant is concentrated successively, dry
Fulvic acid product is made in dry, cooling, grinding.
Inventor has found that ultrasonication can reduce the molecular weight of humic acid, in the present invention inventor under study for action
Proposition improves the imagination of fulvic acid recovery rate using ultrasonic wave.
Inventor is devised during oxidative degradation while ultrasonically treated method is carried out, to improve oxidation drop accordingly
Solve efficiency.Experiment is demonstrated, and ultrasonic wave can strengthen the oxidative degradation of lignite, and can destroy the macromolecular knot of humic acid
Structure, improves the ratio of fulvic acid.But inventor has found in an experiment, the raising of above-mentioned fulvic acid ratio, which does not have, brings final Huang
Rotten acid product yield is significantly improved, and inventor thinks that its reason is the ultrasonic wave stirring auxiliary in oxidizing process, can cause
Oxidative degradation is very violent, causes over oxidation, and the small molecule fulvic acid that early stage has been formed further aoxidizes generation dioxy
Change carbon and water.
Therefore inventor is proposed in this programme after oxidative degradation completion, then product degradation slurry is carried out
The method of ultrasonic agitation.Because oxidative degradation has been completed, a small amount of oxidant is only remained in degraded slurry, thus it is super
Will not occur violent oxidative degradation in sound whipping process, it is to avoid over oxidation.And the generation of ultrasonic agitation process is strong
Large impact ripple causes the particle diameter of the still undegradable cinder of a part after oxidation further to reduce, and improves specific surface area, then
The further oxidative degradation of small amounts agent under ultrasonic agitation effect with residual, improves the yield of fulvic acid.On the other hand, send out
Bright to find under study for action, another major reason of influence fulvic acid yield is cinder surface not degradable in degraded slurry
Coarse and with a large amount of tiny holes, the small molecule fulvic acid of generation is easily adsorbed on cinder surface, difficult in last handling process
To separate, so as to cause part fulvic acid not extract.The present invention is surpassed using ultrasonic cleaner to degraded slurry
Sonication can desorb the fulvic acid adsorbed on cinder surface, beneficial to extraction, so as to improve the yield of fulvic acid.
As a further improvement on the present invention, before oxidative degradation, the brown coal powder is first placed in 30~70 DEG C of water-baths
Relevant temperature is preheated in pot, and the purpose of preheating is chiefly to facilitate oxidative degradation, and there is provided activation energy.
As a further improvement on the present invention, the quality of the water added in step C is 8~12 times of brown coal powder quality.Water
Amount can excessively cause the later stage to be concentrated and dried cost increase, and water is very few, cause fulvic acid to extract incomplete, fulvic acid low yield.
As a further improvement on the present invention, in step C, the frequency of the ultrasonic wave of ultrasonic cleaner for 40~
60Hz, sonication treatment time is 5~60min, and ultrasonically treated temperature is 40~80 DEG C.The program is that inventor passes through many experiments
The preferable ultrasonic cleaning condition drawn, can effectively facilitate cinder and further aoxidize and maintain preferable fulvic acid desorption efficiency.More preferably
, step C stir speed (S.S.) is 100~200r/min, and the too slow slurry of rotating speed disperses insufficient, too fast to cause slurry to splash.
As a further improvement on the present invention, oxidant described in step B is hydrogen peroxide, and oxidant is used as using hydrogen peroxide
Great advantage be it is environmentally friendly, with economical and environmentally friendly double benefit.In addition to hydrogen peroxide, can also use ozone,
Potassium permanganate, nitric acid etc. are used as oxidant.More preferably, the mass concentration of the hydrogen peroxide is 15%~25%, hydrogen peroxide (with
H2O2Meter) mass ratio of consumption and brown coal powder is 0.1~0.5:1, oxidative degradation temperatures are 30~70 DEG C, and the oxidative degradation time is
30~120min.To ensure that it is abundant that oxidative degradation is carried out, while remaining oxidant is unlikely to excessive so that follow-up microwave is stirred
Middle generation over oxidation is mixed, and ensures certain reaction rate.
As a further improvement on the present invention, by the filter residue obtained in step D with after hot wash 3~5 times, by what is obtained
Wash water mixes progress subsequent treatment with the supernatant.Contain a small amount of fulvic acid in filter residue, fulvic acid can be made with hot water injection
It is dissolved in and the wash water containing fulvic acid is formed in hot water, then wash water mixes progress subsequent treatment with supernatant, is filtered with abundant reclaim
Fulvic acid in slag, further improves the recovery rate of fulvic acid.
The beneficial effects of the invention are as follows：1) side using ultrasonic cleaner ultrasonic agitation processing lignite degraded slurry is proposed
Method, the strong impact ripple that ultrasonic agitation process is produced causes the particle diameter of the still undegradable cinder of a part after oxidation further to subtract
It is small, specific surface area is improved, then the further oxidative degradation of small amounts agent under ultrasonic agitation effect with residual, improve yellow
The yield of rotten acid；On the other hand, it will be adsorbed using ultrasonic cleaner is ultrasonically treated to degraded slurry progress on cinder surface
Fulvic acid is desorbed, beneficial to extraction, so as to improve the yield of fulvic acid.2) propose after oxidative degradation completion,
The method for carrying out ultrasonic agitation to product degradation slurry again；Because oxidative degradation has been completed, only remained in degraded slurry
There is a small amount of oxidant, therefore violent oxidative degradation will not occur during ultrasonic agitation, it is to avoid over oxidation.
Embodiment
With reference to embodiment, the present invention is further described.
Embodiment one：
Fulvic acid is extracted from lignite in accordance with the following methods：
(1) after crushing lignite, drying, 120 mesh and the double sieves of 160 mesh is crossed, brown coal powder is obtained.
(2) 20g brown coal powders are weighed to add in 1000mL three-necked flasks, is placed in water-bath and is preheating to 50 DEG C.
(3) after after temperature stabilization, into three-necked flask, addition mass concentration carries out oxidative degradation for 20% hydrogen peroxide 40g
Continuous heating maintenance reaction temperature stabilization is at 50 DEG C or so in reaction, course of reaction, and question response stops heating, obtained after 100 minutes
To degraded slurry.
(4) degraded slurry is injected in ultrasonic cleaner, while 200g water is added at 60 DEG C, 50Hz ultrasonic cleaners
In ultrasonically treated 5min, while being stirred using agitator, stir speed (S.S.) 150r/min obtains ultrasonically treated slurry.
(5) ultrasonically treated slurry is centrifuged, centrifugation rate 2000r/min, centrifugation time 10min is filtered
Slag and supernatant, with 50 DEG C of hot wash filter residues 4 times, each amount of hot water 50mL, obtained wash water mixes laggard with supernatant
Row is concentrated and dried.
(6) sample after being concentrated and dried is ground after 4h, cooling room temperature are incubated in 70 DEG C of baking ovens, obtains fulvic acid powder,
Weighing quality is 3.4g, and it is 16.9% to calculate fulvic acid yield.
Embodiment two：
Fulvic acid is extracted from lignite in accordance with the following methods：
(1) after crushing lignite, drying, 120 mesh and the double sieves of 160 mesh is crossed, brown coal powder is obtained.
(2) 20g brown coal powders are weighed to add in 1000mL three-necked flasks, is placed in water-bath and is preheating to 50 DEG C.
(3) after after temperature stabilization, into three-necked flask, addition mass concentration carries out oxidative degradation for 20% hydrogen peroxide 40g
Continuous heating maintenance reaction temperature stabilization is at 50 DEG C or so in reaction, course of reaction, and question response stops heating, obtained after 100 minutes
To degraded slurry.
(4) degraded slurry is injected in ultrasonic cleaner, while 200g water is added at 60 DEG C, 50Hz ultrasonic cleaners
In ultrasonically treated 30min, while being stirred using agitator, stir speed (S.S.) 150r/min obtains ultrasonically treated slurry.
(5) ultrasonically treated slurry is centrifuged, centrifugation rate 2000r/min, centrifugation time 10min is filtered
Slag and supernatant, with 50 DEG C of hot wash filter residues 4 times, each amount of hot water 50mL, obtained wash water mixes laggard with supernatant
Row is concentrated and dried.
(6) sample after being concentrated and dried is ground after 4h, cooling room temperature are incubated in 70 DEG C of baking ovens, obtains fulvic acid powder,
Weighing quality is 4.1g, and it is 20.5% to calculate fulvic acid yield.
Embodiment three：
Fulvic acid is extracted from lignite in accordance with the following methods：
(1) after crushing lignite, drying, 120 mesh and the double sieves of 160 mesh is crossed, brown coal powder is obtained.
(2) 20g brown coal powders are weighed to add in 1000mL three-necked flasks, is placed in water-bath and is preheating to 50 DEG C.
(3) after after temperature stabilization, into three-necked flask, addition mass concentration carries out oxidative degradation for 20% hydrogen peroxide 40g
Continuous heating maintenance reaction temperature stabilization is at 40 DEG C or so in reaction, course of reaction, and question response stops heating, obtained after 100 minutes
To degraded slurry.
(4) degraded slurry is injected in ultrasonic cleaner, while 200g water is added at 60 DEG C, 50Hz ultrasonic cleaners
In ultrasonically treated 60min, while being stirred using agitator, stir speed (S.S.) 150r/min obtains ultrasonically treated slurry.
(5) ultrasonically treated slurry is centrifuged, centrifugation rate 2000r/min, centrifugation time 10min is filtered
Slag and supernatant, with 50 DEG C of hot wash filter residues 4 times, each amount of hot water 50mL, obtained wash water mixes laggard with supernatant
Row is concentrated and dried.
(6) sample after being concentrated and dried is ground after 4h, cooling room temperature are incubated in 70 DEG C of baking ovens, obtains fulvic acid powder,
Weighing quality is 3.6g, and it is 18.0% to calculate fulvic acid yield.
Note：Fulvic acid calculation of yield formula is as follows：
In formula,
MYield--- fulvic acid yield；
m2--- the quality of obtained fulvic acid product, unit is gram (g)；
M --- the quality of used raw material brown coal powder, unit is gram (g).
Claims (9)
1. extracting the method for fulvic acid from lignite, comprise the following steps：
A, crushing：Lignite is crushed and obtains brown coal powder；
B, oxidative degradation：Oxidant is added into brown coal powder oxidative degradation is carried out to brown coal powder, obtain slurry of degrading；
C, ultrasonic agitation：Degraded slurry is injected in ultrasonic cleaner, while adding clear in ultrasonic wave after the water mixing measured
Wash in device and carry out ultrasonically treated, be stirred while ultrasonically treated, obtain ultrasonically treated slurry；
D, post processing：Ultrasonically treated slurry is centrifuged obtaining filter residue and supernatant, and supernatant is concentrated successively, dry, cold
But, grind and fulvic acid product is made.
2. the method according to claim 1 that fulvic acid is extracted from lignite, it is characterised in that：Before oxidative degradation,
First the brown coal powder is placed in 30~70 DEG C of water-baths and is preheated to relevant temperature.
3. the method according to claim 1 that fulvic acid is extracted from lignite, it is characterised in that：The water added in step C
Quality be 8~12 times of brown coal powder quality.
4. the method according to claim 1 that fulvic acid is extracted from lignite, it is characterised in that：In step C, ultrasonic wave
The frequency of the ultrasonic wave of washer is 40~60Hz, and sonication treatment time is 5~60min, and ultrasonically treated temperature is 40~80 DEG C.
5. the method according to claim 4 that fulvic acid is extracted from lignite, it is characterised in that：Step C stir speed (S.S.)
For 100~200r/min.
6. the method that fulvic acid is extracted from lignite according to any claim in Claims 1 to 5, its feature exists
In：Oxidant described in step B is hydrogen peroxide.
7. the method according to claim 6 that fulvic acid is extracted from lignite, it is characterised in that：The quality of the hydrogen peroxide
Concentration is 15%~25%, and hydrogen peroxide is (with H2O2Meter) mass ratio of consumption and brown coal powder is 0.1~0.5:1.
8. the method according to claim 7 that fulvic acid is extracted from lignite, it is characterised in that：Oxidative degradation temperatures are 30
~70 DEG C, the oxidative degradation time is 30~120min.
9. the method that fulvic acid is extracted from lignite according to any claim in Claims 1 to 5, its feature exists
In：By the filter residue obtained in step D with after hot wash 3~5 times, obtained wash water is mixed into progress with the supernatant follow-up
Processing.
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Cited By (8)
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| CN107383390A (en) * | 2017-06-19 | 2017-11-24 | 龙蟒大地农业有限公司 | The method that hybrid oxidant oxidative degradation lignite produces fulvic acid |
| CN109553501A (en) * | 2019-01-21 | 2019-04-02 | 宁夏然尔特工业产业研究院（有限公司） | A method of activated silica@active humic acid compound fertilizer being prepared by colm and compound fertilizer that this method obtains |
| CN109762029A (en) * | 2019-03-01 | 2019-05-17 | 中国矿业大学 | A method of oxidation lignite extracts fulvic acid |
| CN109810150A (en) * | 2019-03-01 | 2019-05-28 | 中国矿业大学 | A method of fulvic acid in lignite is extracted using supersonic synergic catalysis oxidation |
| CN110105407A (en) * | 2019-04-17 | 2019-08-09 | 上海应用技术大学 | A method of degradation humic acid and ulmic acid are to prepare fulvic acid |
| CN112175625A (en) * | 2020-10-29 | 2021-01-05 | 中煤科工集团沈阳设计研究院有限公司 | Preparation and use methods of modifier for surface soil substitute material of opencast coal mine |
| CN113149792A (en) * | 2021-05-26 | 2021-07-23 | 重庆文理学院 | Special compound foliar fertilizer for rice and preparation method thereof |
| CN114561027A (en) * | 2022-03-02 | 2022-05-31 | 常州大学 | Preparation method of composite potassium fulvate |
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| CN109553501A (en) * | 2019-01-21 | 2019-04-02 | 宁夏然尔特工业产业研究院（有限公司） | A method of activated silica@active humic acid compound fertilizer being prepared by colm and compound fertilizer that this method obtains |
| CN109553501B (en) * | 2019-01-21 | 2021-09-21 | 宁夏然尔特工业产业研究院（有限公司） | Method for preparing active silicon-active humic acid compound fertilizer from low-grade coal and compound fertilizer obtained by method |
| CN109762029A (en) * | 2019-03-01 | 2019-05-17 | 中国矿业大学 | A method of oxidation lignite extracts fulvic acid |
| CN109810150A (en) * | 2019-03-01 | 2019-05-28 | 中国矿业大学 | A method of fulvic acid in lignite is extracted using supersonic synergic catalysis oxidation |
| CN110105407A (en) * | 2019-04-17 | 2019-08-09 | 上海应用技术大学 | A method of degradation humic acid and ulmic acid are to prepare fulvic acid |
| CN110105407B (en) * | 2019-04-17 | 2021-12-07 | 上海应用技术大学 | Method for preparing fulvic acid by degrading fulvic acid and ulmic acid |
| CN112175625A (en) * | 2020-10-29 | 2021-01-05 | 中煤科工集团沈阳设计研究院有限公司 | Preparation and use methods of modifier for surface soil substitute material of opencast coal mine |
| CN112175625B (en) * | 2020-10-29 | 2021-11-19 | 中煤科工集团沈阳设计研究院有限公司 | Preparation and use methods of modifier for surface soil substitute material of opencast coal mine |
| CN113149792A (en) * | 2021-05-26 | 2021-07-23 | 重庆文理学院 | Special compound foliar fertilizer for rice and preparation method thereof |
| CN114561027A (en) * | 2022-03-02 | 2022-05-31 | 常州大学 | Preparation method of composite potassium fulvate |
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