CN107866089A - Weathered coal extracts the device and its extraction process of pharmaceutical grade fulvic acid - Google Patents
Weathered coal extracts the device and its extraction process of pharmaceutical grade fulvic acid Download PDFInfo
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- CN107866089A CN107866089A CN201711435375.0A CN201711435375A CN107866089A CN 107866089 A CN107866089 A CN 107866089A CN 201711435375 A CN201711435375 A CN 201711435375A CN 107866089 A CN107866089 A CN 107866089A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/028—Flow sheets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0292—Treatment of the solvent
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/441—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by reverse osmosis
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F5/00—Softening water; Preventing scale; Adding scale preventatives or scale removers to water, e.g. adding sequestering agents
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- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Chemistry (AREA)
- Treatment Of Water By Ion Exchange (AREA)
Abstract
The device of weathered coal extraction pharmaceutical grade fulvic acid of the present invention, including pure water preparation unit, hybrid extraction unit, fulvic acid refined unit and separation regeneration unit；The extraction process of weathered coal extraction pharmaceutical grade fulvic acid of the present invention, comprises the following steps：Pure water preparation, hybrid extraction, fulvic acid is refined and separation regenerates, and obtains the high medical grade fulvic acid of purity.The device of weathered coal extraction pharmaceutical grade fulvic acid of the present invention, it is simple in construction, it is easy to operate, suitable for use of large-scale production；Pure water selected by the present invention is not volatile, nontoxic and more easy to be recycled as extractant, extraction process is simple to operate, highly reliable, and there is the characteristics of energy-saving and environmental protection, using combination ion exchange resin, cost is low, fulvic acid extraction time is short, recovery rate is high, and fulvic acid purity height, the physiologically active of extraction are strong, stable performance.
Description
Technical field
The invention belongs to the extractive technique field of fulvic acid, and in particular to a kind of dress of weathered coal extraction pharmaceutical grade fulvic acid
Put and its extraction process.
Background technology
Fulvic acid is one of constituent of agron, has the low molecule amount yellow substance of bioactivity, is institute
It is ultimate after active biological decomposition, microstructure form, possess very strong solubility, suitable for different soda acid compositions, and can
Decomposed in all pH value.Fulvic acid is high diversity and complicated combination, and it possesses extremely complex molecular structure, by
Microorganism secretion thing and vegetalitas chemical substance are combined and formed, continuous structure, restructuring formation during humification (decomposition)
, there is uncommon speciality and ability, can change and convert molecular combinations, comprising almost all of organic and inorganic substances,
Possess the characteristic of fusion molecule simultaneously.Fulvic acid is a kind of natural organic substance, has faintly acid, water imbibition, colloidality, absorption
Property, ion exchangeable, comprehensive, oxidation-reduction quality and physiologically active etc., have that molecular weight is smaller, and acidic groups can be dissolved in because more
Acid, alkali and water, the characteristic such as easily it is absorbed by plants.Fulvic acid product all has in industry fields such as agricultural, industry, animal husbandry and medicine
It is widely used.Agriculture aspect have improve soil quality, promote plant growth, drought resisting, it is disease-resistant, improve utilization rate of fertilizer,
Heavy metal and the soil of organic contamination have the effect such as repair function；Industrial aspect is mainly used for heavy metal-polluted water process, can
The harmful metal ion in waste water is removed using the adsorbent as metal ion；Fulvic acid additive can promote in terms of animal husbandry
Growth of animal hair apricot, preventing and treating livestock and poultry common disease etc.；Had been applied to clinically in terms of medical science, fulvic acid, which has, improves immunity of organism
Function, promote the growth of fibrocyte, and can stop blooding, treat burn and scald, suppress the functions such as growth of cancer cells.
The burnt firm master thesis of member of Beijing Jiaotong University in 2006《Fulvic acid is extracted from weathered coal》Studied in one text
Sulfuric acid process, alkali-soluble acid analysis method, ion-exchange-resin process, the extraction effect of four kinds of methods of sulfuric acid acetone method.When have studied reaction
Between, liquid-solid ratio, sour coal than, influence of four factors of ultrasonic wave to sulfuric acid process extraction effect, at optimum conditions, recovery rate is less than
8%；Change the pH value at the end of reaction, study the extraction effect of alkali-soluble acid analysis method, at optimum conditions, recovery rate is less than
10%；Change the weight ratio of resin and coal, study the extraction effect of ion-exchange-resin process, at optimum conditions, recovery rate is small
In 7%；Study the shadow of reaction time, liquid-solid ratio, sour coal than, four factors of extract solution water content to sulfuric acid acetone method extraction effect
Ring, the optimum reaction condition drawn is the acetone that extract solution is aqueous 10%, and sour coal is than 0.05, liquid-solid ratio 7.5, the reaction time
30min, fulvic acid recovery rate can reach 41%.The paper method therefor simply have studied shadow of the various empirical factors to technique
Ring, various techniques are not modified, and each technique is laboratory lab scale, does not there is maximization device.
University Of Shanxi's Wen Pengli master thesis in 2012《Fulvic Acid From Weathered Coal extracts the research of key technology》One
A kind of new fulvic acid extracting method is proposed in text --- sulfuric acid Ethanol Method, this method extract Inner Mongol in the case where most there is experiment condition
Fulvic acid extraction rate reached 32.28% in weathered coal, this method has the advantages of energy consumption is low, but it is only limitted to laboratory lab scale,
The environmental benefit and economic benefit of this method are not evaluated.
Fulvic acid mainly has extraction method, fermentation method, electricity as a kind of multiduty fine organic additive, its preparation method
Dialysis three major types.Wherein, extraction method includes alkali-soluble acid analysis method, ion-exchange-resin process, sulfuric acid acetone method, strong acid extracting again
The methods of method.
(1) alkali-soluble acid analysis method：Using the carboxyl and phenolic hydroxyl group that contain in weathered coal have faintly acid can with alkali into salt, with
Potassium, sodium, calcium, magnesium and ammonium plasma, which combine, generates corresponding humate, after adding inorganic acid, the black corruption of macromolecular in humic acid
Acid and ulmic acid are changed into insoluble substance again, and remaining solable matter is fulvic acid.It is low fulvic acid recovery rate to be present in this method, carries
The shortcomings that taking the time longer.
(2) ion-exchange-resin process：Utilize the calcium in the hydrogen ion substitution fulvic acid in storng-acid cation exchange resin
The Metal ion releases such as magnesium go out fulvic acid.The shortcomings that extraction process is complicated, process power consumption is high and production cost is high be present in the technique.
(3) sulfuric acid acetone method：Utilize the H of sulfuric acid+Substitute the metal ion of fulvic acid calcium and magnesium salt, it is in free shape to make fulvic acid
State, free fulvic acid can be dissolved by the acetone containing a small amount of water (10~20%), the coal dust residue of formation and the sulfuric acid of generation
Calcium salt does not dissolve then, the fulvic acid of generation can thus be extracted, and after boiling off solvent, just obtains low ash content fulvic acid.
The method has that acetone is volatile, has toxicity, is not easily recycled utilization, the shortcomings that production cost is high.
(4) strong acid extraction process：The combination of the calcium, magnesium and the carboxyl that are destroyed using strong acid in fulvate, is replaced using hydrogen ion
Metal ion contained in fulvate is changed, finally discharges fulvic acid.The method process is easily introduced more soluble-salt, product
The shortcomings such as purity is low.
(5) fermentation method：Biochemical fulvic acid prepared by fermentation method has higher physiologically active compared to mineral fulvic acid, no
Cross the method and harsh required to fermentation condition, fermentation period is relatively long and tunning in fulvic acid purity it is not high.
(6) electroosmose process：The metal ion combined with fulvic acid with complex status is removed in the presence of electric field, makes richness
In sour macromolecular and inorganic salts ash content separated, realize the purification of fulvic acid.The method complex operation, the cost of technology be higher, no
It is applicable industrialized production.
The content of the invention
It is an object of the invention to provide the device and its extraction process of a kind of weathered coal extraction pharmaceutical grade fulvic acid, to solve
Above mentioned problem.
To achieve these goals, the technical solution adopted by the present invention is：
The device of weathered coal extraction pharmaceutical grade fulvic acid of the present invention, including pure water preparation unit, hybrid extraction unit, Fu Li
Acid treating unit and separation regeneration unit；
Pure water preparation unit：Including raw water storage tank, force (forcing) pump, quartz filter, active carbon filter, automatic softening
Device, accurate filter, reverse osmosis unit, pure water storage tank and pure water delivery pump, pass through between raw water storage tank and quartz filter
Force (forcing) pump connects, quartz filter, active carbon filter, automatic demineralizer, accurate filter, reverse osmosis unit, pure water storage
Connected between adjacent two equipment of tank by pipeline；
Hybrid extraction unit：Tree is exchanged including combination ion exchange resin eddy flow extraction tower, weathering coal hopper, compound ion
Fat hopper, weathered coal feeder, combination ion exchange resin feeder and static mixer, combination ion exchange resin eddy flow extraction
Tower is taken to be connected with pure water delivery pump, weathering coal hopper connection weathered coal feeder, combination ion exchange resin hopper connects compound
Ion exchange resin feeder, weathered coal feeder and combination ion exchange resin feeder are connected with static mixer, quiet
State blender is connected with the charging aperture of combination ion exchange resin eddy flow extraction tower；The combination ion exchange resin eddy flow extraction
Filter screen and eddy flow post are provided with tower, eddy flow post is connected with blower fan；
Fulvic acid refined unit：Including pipeline pump, tube centrifuge and collecting and filtering apparatus, pipeline pump one end exchanges with compound ion
The discharging opening I of resin eddy flow extraction tower is connected, and the other end and tube centrifuge, tube centrifuge are connected with collecting and filtering apparatus, collecting and filtering apparatus
It is connected with fulvic acid storage tank；
Separate regeneration unit：Including liquid caustic soda storage tank, alkali cleaning pump, caustic wash tower, hydrochloric acid tank, acid picking pump, pickling tower and compound
Ion exchange resin regeneration tower, caustic wash tower are connected with the discharging opening II of combination ion exchange resin eddy flow extraction tower, caustic wash tower with
Pickling tower is connected by the pipeline with flow valve, and pickling tower is connected with combination ion exchange resin regenerator, and compound ion exchanges
Resin regeneration tower is connected with pure water delivery pump, and alkali storage tank is connected with caustic wash tower by alkali cleaning pump, and hydrochloric acid tank passes through with pickling tower
Acid picking pump connects.
Eddy flow post is provided with some circle eddy flow apertures, and the opening direction of eddy flow aperture obliquely, ensures that air goes out from whirl hole
It being direction of rotation obliquely clockwise, can not only material is further well mixed, and enhance weathered coal, compound
Ion exchange between ion exchange resin and pure water, shorten the extraction time of fulvic acid.
The extraction process of weathered coal extraction pharmaceutical grade fulvic acid of the present invention, comprises the following steps：
1) pure water preparation：Raw water sequentially enters quartz sand filtration, activated carbon mistake from raw water storage tank by force (forcing) pump through pipeline
Filter, automatic demineralizer, accurate filter and reverse osmosis unit, required pure water is prepared, it is standby that pure water is stored in pure water storage tank；
2) hybrid extraction：Eddy flow aperture, weathered coal, compound ion can not be entered by opening blower fan and adjusting air quantity to raw material
Exchanger resin enters static mixer by weathered coal feeder, combination ion exchange resin feeder respectively, enters after mixing
Combination ion exchange resin eddy flow extraction tower, pure water are sent into compound ion from pure water storage tank by pure water delivery pump as extractant and handed over
Resin eddy flow extraction tower is changed, gradually tunes up fan delivery, air tangentially sprays clockwise in eddy flow post through eddy flow aperture
Penetrate, after resin adsorption, obtain the thick fulvic acid aqueous solution；
3) fulvic acid refines：The thick fulvic acid aqueous solution through combination ion exchange resin eddy flow extraction tower bottom screen with it is compound
Ion exchange resin is separated, and the thick fulvic acid aqueous solution after separation is delivered in tube centrifuge through pipeline by pipeline pump to be carried out
Solid and liquid separation, as humic acid organic fertilizer raw material, light phase enters collecting and filtering apparatus through pipeline and carries out fulvic acid the heavy phase after centrifuging
Refining and concentrating, the pharmaceutical grade fulvic acid solution after concentration is refined are sent into fulvic acid storage tank；
4) separation regeneration：From caustic wash tower is flow under Gravitative Loads, liquid caustic soda sprays into combination ion exchange resin through alkali cleaning pump
Caustic wash tower, waste water discharge sewage disposal through bottom blow-down valve；Combination ion exchange resin flow to pickling tower, salt certainly after alkali cleaning
Acid sprays into pickling tower through acid picking pump, and waste water discharges sewage disposal through bottom blow-down valve；The combination ion exchange resin after pickling
From flowing to combination ion exchange resin regenerator, discharged via after the pure water cleaning of pure water delivery pump conveying by bottom, circulate into
Enter the utilization of combination ion exchange resin eddy flow extraction tower.
The combination ion exchange resin is chelated by strongly acidic styrene type cation exchange resin and macropore polystyrene
Resin, the mass ratio of the two are 1:1.
Quartz sand filling height is 1.0m in quartz filter, quartz sand particle size 1mm-2mm, and filtering accuracy is
0.005-0.01m。
Liquid caustic soda uses NaOH aqueous slkalis, and the NaOH aqueous slkalis for spraying into caustic wash tower are the 30- of combination ion exchange resin quality
45 times, the hydrochloric acid for spraying into pickling tower is 30-45 times of combination ion exchange resin quality.
The mass concentration of liquid caustic soda is 2%-10%, and the mass concentration of hydrochloric acid is 2%-10%.
The amount of extractant pure water is 40-55 times of weathered coal quality in step 2).
Weathered coal adsorption time in combination ion exchange resin eddy flow extraction tower is 2-4h.
The present invention use weathered coal as principle extraction fulvic acid, the tradable hydrogen contained in combination ion exchange resin from
The metal ion of son and fulvate in weathered coal swaps, and discharges the thick solution of fulvic acid and residue；Due to compound ion
Exchanger resin and residue are all not readily dissolved in water, therefore the device selects extractant of the pure water as fulvic acid；The thick liquid warp of fulvic acid
Centrifuge and the refined proposition high-purity fulvic acid of concentration, combination ion exchange resin are separated by filter screen, regenerate reuse.
Beneficial effects of the present invention are：
(1) device of weathered coal extraction pharmaceutical grade fulvic acid of the present invention, it is simple in construction, it is easy to operate, suitable for extensive raw
Production uses；
(2) pure water selected by the present invention is not volatile, nontoxic and more easy to be recycled as extractant, can solve tradition
Extractant is volatile, it is toxic, be not easily recycled the technical problem utilized；
(3) extraction process of the present invention is simple to operate, highly reliable, and has the characteristics of energy-saving and environmental protection, can solve to pass
The technical problem for extraction method complex operation of uniting；
(4) extraction process of the present invention uses combination ion exchange resin, and cost is low, and fulvic acid extraction time is short, recovery rate
Height, can solve traditional extraction method cost height, the extraction time long technical problem low with recovery rate；
(5) the fulvic acid purity that the present invention extracts is high, physiologically active is strong, stable performance, it is rich can to solve traditional extraction method
In the low technical problem of sour purity.
Brief description of the drawings
Fig. 1 is the structural representation for the device that weathered coal of the present invention extracts pharmaceutical grade fulvic acid；
Fig. 2 is the structural representation of eddy flow post；
In figure：1st, raw water storage tank, 2, force (forcing) pump, 3, quartz filter, 4, active carbon filter, 5, automatic demineralizer,
6th, accurate filter, 7, reverse osmosis unit, 8, pure water storage tank, 9, pure water delivery pump, 10, the extraction of combination ion exchange resin eddy flow
Tower, 101, eddy flow post, 102, filter screen, 11, weathering coal hopper, 12, combination ion exchange resin hopper, 13, weathered coal feeder,
14th, combination ion exchange resin feeder, 15, static mixer, 16, liquid caustic soda storage tank, 17, alkali cleaning pump, 18, caustic wash tower, 19, salt
Acid storage tank, 20, acid picking pump, 21, pickling tower, 22, combination ion exchange resin regenerator, 23, blower fan, 24, pipeline pump, 25, rotten
Phytic acid organic fertilizer, 26, tube centrifuge, 27, collecting and filtering apparatus, 28, fulvic acid storage tank, 29, discharging opening I, 30, discharging opening II.
Embodiment
It is further detailed to the embodiment work of the present invention by the description to optimum embodiment below against accompanying drawing
Thin explanation.
The device of weathered coal extraction pharmaceutical grade fulvic acid of the present invention, including pure water preparation unit, hybrid extraction unit, Fu Li
Acid treating unit and separation regeneration unit；
Pure water preparation unit：Including raw water storage tank 1, force (forcing) pump 2, quartz filter 3, active carbon filter 4, automatic soft
Change device 5, accurate filter 6, reverse osmosis unit 7, pure water storage tank 8 and pure water delivery pump 9, raw water storage tank 1 and quartz filter 3
Between connected by force (forcing) pump 2, quartz filter 3, active carbon filter 4, automatic demineralizer 5, accurate filter 6, reverse osmosis
Connected thoroughly between device 7, adjacent two equipment of pure water storage tank 8 by pipeline；
Hybrid extraction unit：Handed over including combination ion exchange resin eddy flow extraction tower 10, weathering coal hopper 11, compound ion
Resin hopper 12, weathered coal feeder 13, combination ion exchange resin feeder 14 and static mixer 15 are changed, compound ion is handed over
Change resin eddy flow extraction tower 10 with pure water delivery pump 9 to be connected, weathering coal hopper 11 connects weathered coal feeder 13, and compound ion is handed over
Change resin hopper 12 and connect combination ion exchange resin feeder 14, weathered coal feeder 13 and combination ion exchange resin charging
Device 14 is connected with static mixer 15, the charging aperture phase of static mixer 15 and combination ion exchange resin eddy flow extraction tower 10
Even；Filter screen 102 and eddy flow post 101, eddy flow post 101 and the phase of blower fan 23 are provided with combination ion exchange resin eddy flow extraction tower 10
Even；
Fulvic acid refined unit：Including pipeline pump 24, tube centrifuge 26 and collecting and filtering apparatus 27, the one end of pipeline pump 24 with it is compound
The discharging opening I 29 of ion exchange resin eddy flow extraction tower 10 is connected, and the other end and tube centrifuge 26, tube centrifuge 26 is with receiving
Filter 27 is connected, and collecting and filtering apparatus 27 is connected with fulvic acid storage tank 28；
Separate regeneration unit：Including liquid caustic soda storage tank 16, alkali cleaning pump 17, caustic wash tower 18, hydrochloric acid tank 19, acid picking pump 20, acid
Wash tower 21 and combination ion exchange resin regenerator 20, the discharging of caustic wash tower 18 and combination ion exchange resin eddy flow extraction tower 10
Mouth II 30 is connected, and caustic wash tower 18 is connected with pickling tower 21 by the pipeline with flow valve, and pickling tower 21 exchanges tree with compound ion
Fat regenerator 20 is connected, and combination ion exchange resin regenerator 20 is connected with pure water delivery pump 9, and alkali storage tank 16 is logical with caustic wash tower 17
Cross alkali cleaning pump 20 to connect, hydrochloric acid tank 19 is connected with pickling tower 21 by acid picking pump 21.
Eddy flow post 101 is provided with some circle eddy flow apertures, and the opening direction of eddy flow aperture is obliquely.
The extraction process of weathered coal extraction pharmaceutical grade fulvic acid of the present invention, comprises the following steps：
1) pure water preparation：Raw water sequentially enters quartz sand filtration, activated carbon mistake from raw water storage tank by force (forcing) pump through pipeline
Filter, automatic demineralizer, accurate filter and reverse osmosis unit, required pure water is prepared, it is standby that pure water is stored in pure water storage tank；
2) hybrid extraction：Eddy flow aperture, weathered coal, compound ion can not be entered by opening blower fan and adjusting air quantity to raw material
Exchanger resin enters static mixer by weathered coal feeder, combination ion exchange resin feeder respectively, enters after mixing
Combination ion exchange resin eddy flow extraction tower, pure water are sent into compound ion from pure water storage tank by pure water delivery pump as extractant and handed over
Resin eddy flow extraction tower is changed, gradually tunes up fan delivery, air tangentially sprays clockwise in eddy flow post through eddy flow aperture
Penetrate, after resin adsorption, obtain the thick fulvic acid aqueous solution；
3) fulvic acid refines：The thick fulvic acid aqueous solution through combination ion exchange resin eddy flow extraction tower bottom screen with it is compound
Ion exchange resin is separated, and the thick fulvic acid aqueous solution after separation is delivered in tube centrifuge through pipeline by pipeline pump to be carried out
Solid and liquid separation, as humic acid organic fertilizer raw material, light phase enters collecting and filtering apparatus through pipeline and carries out fulvic acid the heavy phase after centrifuging
Refining and concentrating, the pharmaceutical grade fulvic acid solution after concentration is refined are sent into fulvic acid storage tank；
4) separation regeneration：From caustic wash tower is flow under Gravitative Loads, liquid caustic soda sprays into combination ion exchange resin through alkali cleaning pump
Caustic wash tower, waste water discharge sewage disposal through bottom blow-down valve；Combination ion exchange resin flow to pickling tower, salt certainly after alkali cleaning
Acid sprays into pickling tower through acid picking pump, and waste water discharges sewage disposal through bottom blow-down valve；The combination ion exchange resin after pickling
From flowing to combination ion exchange resin regenerator, discharged via after the pure water cleaning of pure water delivery pump conveying by bottom, circulate into
Enter the utilization of combination ion exchange resin eddy flow extraction tower.
Combination ion exchange resin by strongly acidic styrene type cation exchange resin and macropore polystyrene chelating resin,
The mass ratio of the two is 1:1.
Quartz sand filling height is 1.0m in quartz filter, quartz sand particle size 1mm-2mm, and filtering accuracy is
0.005-0.01m。
Liquid caustic soda uses NaOH aqueous slkalis, and the NaOH aqueous slkalis for spraying into caustic wash tower are the 30- of combination ion exchange resin quality
45 times, the hydrochloric acid for spraying into pickling tower is 30-45 times of combination ion exchange resin quality.
The mass concentration of liquid caustic soda is 2%-10%, and the mass concentration of hydrochloric acid is 2%-10%.
The amount of extractant pure water is 40-55 times of weathered coal quality in step 2).
Weathered coal adsorption time in combination ion exchange resin eddy flow extraction tower is 2-4h.
The device and extraction process for the weathered coal extraction pharmaceutical grade fulvic acid recorded using the present invention, fulvic acid were being refined
Cheng Zhong, the fulvic acid into collecting and filtering apparatus are concentrated into mass concentration as 3%, and the purity of gained fulvic acid is 98.5%, fulvic acid
Recovery rate is 80%.
Claims (9)
1. a kind of device of weathered coal extraction pharmaceutical grade fulvic acid, it is characterised in that including pure water preparation unit, hybrid extraction list
Member, fulvic acid refined unit and separation regeneration unit；
Pure water preparation unit：Including raw water storage tank (1), force (forcing) pump (2), quartz filter (3), active carbon filter (4), from
Dynamic demineralizer (5), accurate filter (6), reverse osmosis unit (7), pure water storage tank (8) and pure water delivery pump (9), raw water storage tank
(1) between quartz filter (3) by force (forcing) pump (2) connect, quartz filter (3), active carbon filter (4), from
Connected between dynamic demineralizer (5), accurate filter (6), reverse osmosis unit (7), adjacent two equipment of pure water storage tank (8) by pipeline
Connect；
Hybrid extraction unit：Handed over including combination ion exchange resin eddy flow extraction tower (10), weathering coal hopper (11), compound ion
Resin hopper (12), weathered coal feeder (13), combination ion exchange resin feeder (14) and static mixer (15) are changed, it is multiple
Close ion exchange resin eddy flow extraction tower (10) with pure water delivery pump (9) to be connected, weathering coal hopper (11) connection weathered coal charging
Device (13), combination ion exchange resin hopper (12) connection combination ion exchange resin feeder (14), weathered coal feeder
(13) be connected with combination ion exchange resin feeder (14) with static mixer (15), static mixer (15) with it is compound from
The charging aperture of sub-exchange resin eddy flow extraction tower (10) is connected；It is provided with the combination ion exchange resin eddy flow extraction tower (10)
Filter screen (102) and eddy flow post (101), eddy flow post (101) are connected with blower fan (23)；
Fulvic acid refined unit：Including pipeline pump (24), tube centrifuge (26) and collecting and filtering apparatus (27), pipeline pump (24) one end with
The discharging opening I (29) of combination ion exchange resin eddy flow extraction tower (10) is connected, the other end and tube centrifuge (26), tubular type from
Scheming (26) is connected with collecting and filtering apparatus (27), and collecting and filtering apparatus (27) is connected with fulvic acid storage tank (28)；
Separate regeneration unit：Including liquid caustic soda storage tank (16), alkali cleaning pump (17), caustic wash tower (18), hydrochloric acid tank (19), acid picking pump
(20), pickling tower (21) and combination ion exchange resin regenerator (20), caustic wash tower (18) and combination ion exchange resin eddy flow
The discharging opening II (30) of extraction tower (10) is connected, and caustic wash tower (18) is connected with pickling tower (21) by the pipeline with flow valve, acid
Wash tower (21) with combination ion exchange resin regenerator (20) to be connected, combination ion exchange resin regenerator (20) conveys with pure water
Pump (9) is connected, and alkali storage tank (16) is connected with caustic wash tower (17) by alkali cleaning pump (20), and hydrochloric acid tank (19) is logical with pickling tower (21)
Overpickling pump (21) connects.
2. the device of weathered coal extraction pharmaceutical grade fulvic acid according to claim 1, it is characterised in that eddy flow post (101)
Provided with some circle eddy flow apertures, the opening direction of eddy flow aperture is obliquely.
3. a kind of extraction process of weathered coal extraction pharmaceutical grade fulvic acid, it is characterised in that comprise the following steps：
1) pure water preparation：Raw water by force (forcing) pump from raw water storage tank through pipeline sequentially enter quartz sand filtration, active carbon filter,
Automatic demineralizer, accurate filter and reverse osmosis unit, prepare required pure water, it is standby that pure water is stored in pure water storage tank；
2) hybrid extraction：Eddy flow aperture can not be entered by opening blower fan and adjusting air quantity to raw material, and weathered coal, compound ion exchange
Resin enters static mixer by weathered coal feeder, combination ion exchange resin feeder respectively, enters after mixing compound
Ion exchange resin eddy flow extraction tower, pure water are sent into compound ion from pure water storage tank by pure water delivery pump as extractant and exchange tree
Fat eddy flow extraction tower, fan delivery is gradually tuned up, air tangentially sprays clockwise in eddy flow post through eddy flow aperture, warp
After resin adsorption, the thick fulvic acid aqueous solution is obtained；
3) fulvic acid refines：The thick fulvic acid aqueous solution is through combination ion exchange resin eddy flow extraction tower bottom screen and compound ion
Exchange resin is opened, the thick fulvic acid aqueous solution after separation be delivered to through pipeline by pipeline pump in tube centrifuge carry out it is solid,
Liquid separates, and the heavy phase after centrifuging enters the essence of collecting and filtering apparatus progress fulvic acid through pipeline as humic acid organic fertilizer raw material, light phase
System concentration, the pharmaceutical grade fulvic acid solution after concentration is refined are sent into fulvic acid storage tank；
4) separation regeneration：For combination ion exchange resin from caustic wash tower is flow under Gravitative Loads, liquid caustic soda sprays into alkali cleaning through alkali cleaning pump
Tower, waste water discharge sewage disposal through bottom blow-down valve；Combination ion exchange resin passes through from pickling tower, hydrochloric acid is flow to after alkali cleaning
Acid picking pump sprays into pickling tower, and waste water discharges sewage disposal through bottom blow-down valve；Combination ion exchange resin flows automatically after pickling
To combination ion exchange resin regenerator, discharged, be recycled into multiple by bottom via after the pure water cleaning of pure water delivery pump conveying
Ion exchange resin eddy flow extraction tower is closed to utilize.
4. the extraction process of weathered coal extraction pharmaceutical grade fulvic acid according to claim 3, it is characterised in that described compound
Ion exchange resin is by strongly acidic styrene type cation exchange resin and macropore polystyrene chelating resin, the mass ratio of the two
For 1:1.
5. the extraction process of weathered coal extraction pharmaceutical grade fulvic acid according to claim 3, it is characterised in that quartz sand mistake
Quartz sand filling height is 1.0m, quartz sand particle size 1-2mm, filtering accuracy 0.005-0.01m in filter.
6. the extraction process of weathered coal extraction pharmaceutical grade fulvic acid according to claim 3, it is characterised in that liquid caustic soda uses
NaOH aqueous slkalis, the NaOH aqueous slkalis for spraying into caustic wash tower are 30-45 times of combination ion exchange resin quality, spray into pickling tower
Hydrochloric acid is 30-45 times of combination ion exchange resin quality.
7. the extraction process of the weathered coal extraction pharmaceutical grade fulvic acid according to claim 3 or 6, it is characterised in that liquid caustic soda
Mass concentration be 2%-10%, the mass concentration of hydrochloric acid is 2%-10%.
8. the extraction process of weathered coal extraction pharmaceutical grade fulvic acid according to claim 3, it is characterised in that in step 2)
The amount of extractant pure water is 40-55 times of weathered coal quality.
9. the extraction process of weathered coal extraction pharmaceutical grade fulvic acid according to claim 3, it is characterised in that weathered coal exists
Adsorption time is 2-4h in combination ion exchange resin eddy flow extraction tower.
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| CN111196639A (en) * | 2020-01-16 | 2020-05-26 | 西藏华阳供热工程服务有限公司 | Reverse osmosis water purifier and operation method thereof |
| CN112029114A (en) * | 2020-09-23 | 2020-12-04 | 山东奥淼科技发展有限公司 | Method and device for extracting medical fulvic acid from biomass pyrolysis liquid |
| CN115991881A (en) * | 2022-05-05 | 2023-04-21 | 山东金科力电源科技有限公司 | Humic acid iron removing method |
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