CN107866089B - Device for extracting pharmaceutical-grade fulvic acid from weathered coal and extraction process thereof - Google Patents
Device for extracting pharmaceutical-grade fulvic acid from weathered coal and extraction process thereof Download PDFInfo
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- CN107866089B CN107866089B CN201711435375.0A CN201711435375A CN107866089B CN 107866089 B CN107866089 B CN 107866089B CN 201711435375 A CN201711435375 A CN 201711435375A CN 107866089 B CN107866089 B CN 107866089B
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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
Abstract
The invention relates to a device for extracting pharmaceutical-grade fulvic acid from weathered coal, which comprises a pure water preparation unit, a mixed extraction unit, a fulvic acid refining unit and a separation regeneration unit; the extraction process for extracting the pharmaceutical fulvic acid from the weathered coal comprises the following steps of: preparing pure water, mixing and extracting, refining fulvic acid, separating and regenerating to obtain the medical fulvic acid with high purity. The device for extracting the pharmaceutical fulvic acid from the weathered coal has the advantages of simple structure and convenience in operation, and is suitable for large-scale production and use; the method selects pure water as an extracting agent, is not easy to volatilize, is non-toxic, is easy to recycle, has the characteristics of simple extraction process operation, strong reliability, energy conservation and environmental protection, adopts the composite ion exchange resin, and has the advantages of low cost, short fulvic acid extraction time, high extraction rate, high purity of the extracted fulvic acid, strong physiological activity and stable performance.
Description
Technical Field
The invention belongs to the technical field of fulvic acid extraction, and particularly relates to a device and an extraction process for extracting pharmaceutical fulvic acid from weathered coal.
Background
Fulvic acid is one of the components of soil humus, is a low-molecular-weight yellow substance with bioactivity, is the ultimate after decomposition of all active organisms, has a microstructure form, has strong solubility, is suitable for different acid-base components, and can be decomposed in all pH values. Fulvic acid is a highly diverse and complex association, possessing an extremely complex molecular structure, formed by the association of microbial secretions with phytochemicals, formed by successive structural and reorganization during humification (decomposition), with unusual characteristics and abilities to alter and transform molecular combinations, containing almost all organic and inorganic substances, while possessing the characteristics of fusion molecules. Fulvic acid is a natural organic substance, has weak acidity, water absorbability, colloid property, adsorbability, ion exchange property, comprehensive property, oxidation reduction property, physiological activity and the like, and has the characteristics of small molecular weight, more acidic genes, capability of being dissolved in acid, alkali and water, easiness in plant absorption and the like. The fulvic acid product has wide application in the fields of agriculture, industry, animal husbandry, medicine and the like. The fertilizer has the functions of improving soil quality, promoting plant growth, resisting drought and diseases, improving fertilizer utilization rate, repairing heavy metal and organic polluted soil and the like in the aspect of agriculture; the industrial method is mainly used for treating heavy metal sewage, and can be used as an adsorbent of metal ions to remove harmful metal ions in the sewage; the fulvic acid additive can promote animals to grow and develop apricot, prevent and treat common diseases of livestock and poultry and the like in the aspect of animal husbandry; the fulvic acid has been clinically applied in the medical field, has the functions of improving the immunity of organisms, promoting the growth of fiber cells, stopping bleeding, treating burns and scalds, inhibiting the growth of cancer cells and the like.
In 2006, the Jiao Yuangang university of Beijing traffic 5363 Master academic paper "the fulvic acid extraction from weathered coal" researches the extraction effects of four methods, namely, a sulfuric acid method, an alkali-dissolution acid-separation method, an ion exchange resin method and a sulfuric acid acetone method. The influence of four factors, namely reaction time, liquid-solid ratio, acid-coal ratio and ultrasonic wave, on the extraction effect of the sulfuric acid method is researched, and under the optimal condition, the extraction rate is less than 8%; changing the pH value at the end of the reaction, researching the extraction effect of an alkali-soluble acid-separating method, wherein the extraction rate is less than 10% under the optimal condition; changing the weight ratio of resin to coal, researching the extraction effect of the ion exchange resin method, wherein under the optimal condition, the extraction rate is less than 7 percent; the influence of four factors of reaction time, liquid-solid ratio, acid-coal ratio and water content of the extracting solution on the extraction effect of the sulfuric acid acetone method is researched, the obtained optimal reaction conditions are that the extracting solution is acetone with 10% of water, the acid-coal ratio is 0.05, the liquid-solid ratio is 7.5, the reaction time is 30min, and the fulvic acid extraction rate can reach 41%. The method used in the thesis only researches the influence of various experimental factors on the process, the various processes are not modified, and all the processes are laboratory tests and do not have large-scale devices.
A new fulvic acid extraction method, namely a sulfuric acid ethanol method, is proposed in a text of a Wen Pengli university of Shanxi 5363 university Master degree paper research on fulvic acid extraction key technology in weathered coal in 2012, the method has the advantage of low energy consumption when the fulvic acid extraction rate in the inner Mongolian weathered coal is up to 32.28% under the most experimental conditions, but the method is limited to laboratory experiments and does not evaluate the environmental benefit and the economic benefit of the method.
Furic acid is used as a multipurpose fine organic additive, and the preparation method mainly comprises three types of extraction method, fermentation method and electrodialysis method. Wherein the extraction method comprises alkali dissolution and acid precipitation, ion exchange resin method, acetone sulfate method, strong acid extraction method, etc.
(1) Alkali dissolution and acid precipitation: carboxyl and phenolic hydroxyl contained in the weathered coal have weak acidity and can form salt with alkali, the salt is combined with potassium, sodium, calcium, magnesium, ammonium and other ions to generate corresponding humate, after inorganic acid is added, macromolecular black humic acid and brown humic acid in the humic acid are changed into insoluble substances, and the rest soluble substances are fulvic acid. The method has the disadvantages of low fulvic acid extraction rate and long extraction time.
(2) Ion exchange resin method: the hydrogen ions in the strong-acid cation exchange resin are used for replacing metal ions such as calcium, magnesium and the like in the fulvic acid to release the fulvic acid. The process has the disadvantages of complex extraction process, high energy consumption in the process and high production cost.
(3) Acetone sulfate method: by H of sulfuric acid + The metal ions of the calcium magnesium fulvate are replaced to enable the fulvic acid to be in a free state, the free fulvic acid can be dissolved by acetone containing a small amount of water (10-20%), the formed coal dust residue and the generated calcium sulfate salt are not dissolved, the generated fulvic acid can be extracted, and the low-ash fulvic acid can be obtained after the solvent is evaporated. The method has the defects of easy volatilization of acetone, toxicity, difficult recycling and high production cost.
(4) Strong acid extraction method: the combination of calcium, magnesium and carboxyl in the fulvic acid salt is destroyed by strong acid, and metal ions contained in the fulvic acid salt are replaced by hydrogen ions, so that the fulvic acid is released finally. The method has the defects of easy introduction of more soluble salts, low product purity and the like.
(5) A fermentation method: compared with coal fulvic acid, biochemical fulvic acid prepared by the fermentation method has higher physiological activity, but the method has strict requirements on fermentation conditions, the fermentation period is relatively long, and the purity of fulvic acid in a fermentation product is not high.
(6) An electrodialysis method: under the action of an electric field, metal ions combined with the fulvic acid in a complexing state are removed, so that the fulvic acid macromolecules and inorganic salt ash are separated, and the purification of the fulvic acid is realized. The method has the advantages of complex operation, high process cost and unsuitability for industrial production.
Disclosure of Invention
The invention aims to provide a device for extracting pharmaceutical fulvic acid from weathered coal and an extraction process thereof, so as to solve the problems.
In order to achieve the purpose, the invention adopts the technical scheme that:
the invention relates to a device for extracting pharmaceutical fulvic acid from weathered coal, which comprises a pure water preparation unit, a mixed extraction unit, a fulvic acid refining unit and a separation regeneration unit;
a pure water preparation unit: the system comprises a raw water storage tank, a pressure pump, a quartz sand filter, an activated carbon filter, an automatic softener, a precision filter, a reverse osmosis device, a pure water storage tank and a pure water delivery pump, wherein the raw water storage tank and the quartz sand filter are connected through the pressure pump;
a mixing extraction unit: the device comprises a composite ion exchange resin cyclone extraction tower, a weathered coal hopper, a composite ion exchange resin hopper, a weathered coal feeder, a composite ion exchange resin feeder and a static mixer, wherein the composite ion exchange resin cyclone extraction tower is connected with a pure water delivery pump, the weathered coal hopper is connected with the weathered coal feeder, the composite ion exchange resin hopper is connected with the composite ion exchange resin feeder, the weathered coal feeder and the composite ion exchange resin feeder are both connected with the static mixer, and the static mixer is connected with a feed inlet of the composite ion exchange resin cyclone extraction tower; a filter screen and a cyclone column are arranged in the composite ion exchange resin cyclone extraction tower, and the cyclone column is connected with a fan;
a fulvic acid refining unit: the device comprises a pipeline pump, a tubular centrifuge and a nanofiltration machine, wherein one end of the pipeline pump is connected with a discharge port I of the composite ion exchange resin cyclone extraction tower, the other end of the pipeline pump is connected with the tubular centrifuge, the tubular centrifuge is connected with the nanofiltration machine, and the nanofiltration machine is connected with a fulvic acid storage tank;
a separation and regeneration unit: the device comprises a liquid caustic soda storage tank, an alkaline washing pump, an alkaline washing tower, a hydrochloric acid storage tank, an acid washing pump, an acid washing tower and a composite ion exchange resin regeneration tower, wherein the alkaline washing tower is connected with a discharge port II of the composite ion exchange resin cyclone extraction tower, the alkaline washing tower is connected with the acid washing tower through a pipeline with a flow valve, the acid washing tower is connected with the composite ion exchange resin regeneration tower, the composite ion exchange resin regeneration tower is connected with a pure water delivery pump, the alkaline storage tank is connected with the alkaline washing tower through the alkaline washing pump, and the hydrochloric acid storage tank is connected with the acid washing tower through the acid washing pump.
The cyclone column is provided with a plurality of circles of cyclone small holes, the opening direction of the cyclone small holes is inclined upwards, and the air is ensured to be clockwise inclined upwards in the rotating direction from the cyclone holes, so that the materials can be further uniformly mixed, the ion exchange among the weathered coal, the composite ion exchange resin and the pure water is strengthened, and the extraction time of the fulvic acid is shortened.
The extraction process for extracting the pharmaceutical fulvic acid from the weathered coal comprises the following steps of:
1) Preparing pure water: raw water sequentially enters a quartz sand filter, an activated carbon filter, an automatic softener, a precision filter and a reverse osmosis device from a raw water storage tank through a pipeline by a pressure pump to prepare required pure water, and the pure water is stored in a pure water storage tank for later use;
2) Mixing and extracting: starting a fan and adjusting the air quantity until the raw materials cannot enter the swirl holes, allowing the weathered coal and the composite ion exchange resin to enter a static mixer through a weathered coal feeder and a composite ion exchange resin feeder respectively, mixing and then entering a composite ion exchange resin swirl extraction tower, feeding pure water serving as an extractant into the composite ion exchange resin swirl extraction tower from a pure water storage tank by a pure water delivery pump, gradually increasing the air quantity of the fan, injecting air clockwise through the swirl holes in the swirl column along the tangential direction, and adsorbing by resin to obtain a crude fulvic acid aqueous solution;
3) Refining fulvic acid: separating the crude fulvic acid aqueous solution from the composite ion exchange resin through a filter screen at the bottom of the composite ion exchange resin cyclone extraction tower, conveying the separated crude fulvic acid aqueous solution to a tubular centrifuge through a pipeline pump for solid-liquid separation, taking a centrifuged heavy phase as a humic acid organic fertilizer raw material, allowing a light phase to enter a nanofiltration machine through a pipeline for fulvic acid refining and concentration, and conveying a concentrated and refined medical-grade fulvic acid solution to a fulvic acid storage tank;
4) Separation and regeneration: the composite ion exchange resin flows to an alkaline tower automatically under the action of dead weight, liquid caustic soda is sprayed into the alkaline tower through an alkaline pump, and wastewater is discharged through a bottom drain valve to be subjected to sewage treatment; after alkaline washing, the composite ion exchange resin automatically flows to an acid washing tower, hydrochloric acid is sprayed into the acid washing tower through an acid washing pump, and wastewater is discharged through a bottom blow-down valve to be subjected to sewage treatment; the composite ion exchange resin automatically flows to a composite ion exchange resin regeneration tower after acid washing, pure water conveyed by a pure water conveying pump is discharged from the bottom after being cleaned, and the pure water circularly enters a composite ion exchange resin cyclone extraction tower for utilization.
The composite ion exchange resin is composed of strong-acid styrene cation exchange resin and macroporous styrene chelating resin, and the mass ratio of the strong-acid styrene cation exchange resin to the macroporous styrene chelating resin is 1:1.
The filling height of the quartz sand in the quartz sand filter is 1.0m, the particle size of the quartz sand is 1mm-2mm, and the filtering precision is 0.005-0.01m.
The liquid caustic soda adopts NaOH alkaline solution, the mass of the NaOH alkaline solution sprayed into the alkaline tower is 30-45 times of that of the composite ion exchange resin, and the mass of the hydrochloric acid sprayed into the acid tower is 30-45 times of that of the composite ion exchange resin.
The mass concentration of the liquid caustic soda is 2-10%, and the mass concentration of the hydrochloric acid is 2-10%.
The amount of the extractant pure water in the step 2) is 40-55 times of the mass of the weathered coal.
The absorption time of the weathered coal in the composite ion exchange resin cyclone extraction tower is 2-4h.
According to the method, the fulvic acid is extracted by adopting weathered coal as a principle, exchangeable hydrogen ions contained in the composite ion exchange resin exchange with metal ions of fulvic acid salt in weathered coal, and a fulvic acid crude solution and residues are released; because the composite ion exchange resin and the residue are not easy to dissolve in water, the device selects pure water as the extractant of the fulvic acid; the crude fulvic acid liquid is centrifugally separated, concentrated and refined to obtain high-purity fulvic acid, and the composite ion exchange resin is separated by a filter screen and regenerated for reuse.
The invention has the beneficial effects that:
(1) The device for extracting the pharmaceutical fulvic acid from the weathered coal has the advantages of simple structure and convenience in operation, and is suitable for large-scale production and use;
(2) The invention selects pure water as the extractant, which is not easy to volatilize, nontoxic and easy to recycle, and can solve the technical problems of easy volatilization, toxicity and difficult recycling of the traditional extractant;
(3) The extraction process has the characteristics of simplicity in operation, high reliability, energy conservation and environmental friendliness, and can solve the technical problem of complex operation of the traditional extraction method;
(4) The extraction process adopts the composite ion exchange resin, has low cost, short fulvic acid extraction time and high extraction rate, and can solve the technical problems of high cost, long extraction time and low extraction rate of the traditional extraction method;
(5) The fulvic acid extracted by the method has high purity, strong physiological activity and stable performance, and can solve the technical problem of low purity of fulvic acid in the traditional extraction method.
Drawings
FIG. 1 is a schematic structural view of a device for extracting pharmaceutical-grade fulvic acid from weathered coal according to the present invention;
FIG. 2 is a schematic structural view of a cyclone column;
in the figure: 1. raw water storage tank, 2, pressure pump, 3, quartz sand filter, 4, activated carbon filter, 5, automatic softener, 6, precision filter, 7, reverse osmosis device, 8, pure water storage tank, 9, pure water delivery pump, 10, composite ion exchange resin cyclone extraction tower, 101, cyclone column, 102, filter screen, 11, weathered coal hopper, 12, composite ion exchange resin hopper, 13, weathered coal feeder, 14, composite ion exchange resin feeder, 15, static mixer, 16, liquid caustic soda storage tank, 17, caustic wash pump, 18, caustic wash tower, 19, hydrochloric acid storage tank, 20, acid wash pump, 21, acid wash tower, 22, composite ion exchange resin regenerator, 23, fan, 24, pipeline pump, 25, humic acid organic fertilizer, 26, tubular centrifuge, 27, nanofiltration machine, 28, fulvic acid storage tank, 29, discharge port I, 30 and discharge port II.
Detailed Description
The following description of preferred embodiments of the invention will be made in further detail with reference to the accompanying drawings.
The invention relates to a device for extracting pharmaceutical fulvic acid from weathered coal, which comprises a pure water preparation unit, a mixed extraction unit, a fulvic acid refining unit and a separation regeneration unit;
a pure water preparation unit: the system comprises a raw water storage tank 1, a pressure pump 2, a quartz sand filter 3, an activated carbon filter 4, an automatic softener 5, a precision filter 6, a reverse osmosis device 7, a pure water storage tank 8 and a pure water delivery pump 9, wherein the raw water storage tank 1 and the quartz sand filter 3 are connected through the pressure pump 2, and the quartz sand filter 3, the activated carbon filter 4, the automatic softener 5, the precision filter 6, the reverse osmosis device 7 and the pure water storage tank 8 are connected through pipelines;
a mixing extraction unit: the device comprises a composite ion exchange resin cyclone extraction tower 10, a weathered coal hopper 11, a composite ion exchange resin hopper 12, a weathered coal feeder 13, a composite ion exchange resin feeder 14 and a static mixer 15, wherein the composite ion exchange resin cyclone extraction tower 10 is connected with a pure water delivery pump 9, the weathered coal hopper 11 is connected with the weathered coal feeder 13, the composite ion exchange resin hopper 12 is connected with the composite ion exchange resin feeder 14, the weathered coal feeder 13 and the composite ion exchange resin feeder 14 are both connected with the static mixer 15, and the static mixer 15 is connected with a feed inlet of the composite ion exchange resin cyclone extraction tower 10; a filter screen 102 and a cyclone column 101 are arranged in the composite ion exchange resin cyclone extraction tower 10, and the cyclone column 101 is connected with a fan 23;
a fulvic acid refining unit: the device comprises a pipeline pump 24, a tubular centrifuge 26 and a nanofiltration machine 27, wherein one end of the pipeline pump 24 is connected with a discharge port I29 of the composite ion exchange resin cyclone extraction tower 10, the other end of the pipeline pump is connected with the tubular centrifuge 26, the tubular centrifuge 26 is connected with the nanofiltration machine 27, and the nanofiltration machine 27 is connected with a fulvic acid storage tank 28;
a separation and regeneration unit: the device comprises a liquid caustic soda storage tank 16, a caustic washing pump 17, a caustic washing tower 18, a hydrochloric acid storage tank 19, an acid washing pump 20, an acid washing tower 21 and a composite ion exchange resin regeneration tower 22, wherein the caustic washing tower 18 is connected with a discharge hole II 30 of the composite ion exchange resin cyclone extraction tower 10, the caustic washing tower 18 is connected with the acid washing tower 21 through a pipeline with a flow valve, the acid washing tower 21 is connected with the composite ion exchange resin regeneration tower 22, the composite ion exchange resin regeneration tower 22 is connected with a pure water delivery pump 9, the liquid caustic soda storage tank 16 is connected with the caustic washing tower 18 through the caustic washing pump 17, and the hydrochloric acid storage tank 19 is connected with the acid washing tower 21 through the acid washing pump 20.
The swirling flow column 101 is provided with a plurality of rings of swirling flow small holes, and the hole opening directions of the swirling flow small holes are inclined upwards.
The extraction process for extracting the pharmaceutical fulvic acid from the weathered coal comprises the following steps of:
1) Preparing pure water: raw water sequentially enters a quartz sand filter, an activated carbon filter, an automatic softener, a precision filter and a reverse osmosis device from a raw water storage tank through a pipeline by a pressure pump to prepare required pure water, and the pure water is stored in a pure water storage tank for later use;
2) Mixing and extracting: starting a fan and adjusting the air quantity until the raw materials cannot enter the swirl small holes, allowing the weathered coal and the composite ion exchange resin to respectively enter a static mixer through a weathered coal feeder and a composite ion exchange resin feeder, mixing and then entering a composite ion exchange resin swirl extraction tower, feeding pure water serving as an extracting agent into the composite ion exchange resin swirl extraction tower from a pure water storage tank by using a pure water delivery pump, gradually increasing the air quantity of the fan, injecting air clockwise through the swirl small holes in the swirl column along the tangential direction, and adsorbing by using resin to obtain a crude fulvic acid aqueous solution;
3) Refining fulvic acid: separating the crude fulvic acid aqueous solution from the composite ion exchange resin through a filter screen at the bottom of the composite ion exchange resin cyclone extraction tower, conveying the separated crude fulvic acid aqueous solution to a tubular centrifuge through a pipeline pump for solid-liquid separation, taking a centrifuged heavy phase as a humic acid organic fertilizer raw material, allowing a light phase to enter a nanofiltration machine through a pipeline for fulvic acid refining and concentration, and conveying a concentrated and refined medical-grade fulvic acid solution to a fulvic acid storage tank;
4) Separation and regeneration: the composite ion exchange resin flows to an alkaline washing tower automatically under the action of dead weight, liquid caustic soda is sprayed into the alkaline washing tower through an alkaline washing pump, and wastewater is discharged through a bottom blow-down valve to be subjected to sewage treatment; after alkaline washing, the composite ion exchange resin automatically flows to an acid washing tower, hydrochloric acid is sprayed into the acid washing tower through an acid washing pump, and wastewater is discharged through a bottom blow-down valve to be subjected to sewage treatment; the composite ion exchange resin automatically flows to a composite ion exchange resin regeneration tower after acid washing, pure water conveyed by a pure water conveying pump is discharged from the bottom after being cleaned, and the pure water circularly enters a composite ion exchange resin cyclone extraction tower for utilization.
The composite ion exchange resin is composed of strong-acid styrene cation exchange resin and macroporous styrene chelating resin, and the mass ratio of the strong-acid styrene cation exchange resin to the macroporous styrene chelating resin is 1:1.
The filling height of the quartz sand in the quartz sand filter is 1.0m, the particle size of the quartz sand is 1mm-2mm, and the filtering precision is 0.005-0.01m.
The liquid caustic soda adopts NaOH alkaline solution, the mass of the NaOH alkaline solution sprayed into the alkaline tower is 30-45 times of that of the composite ion exchange resin, and the mass of the hydrochloric acid sprayed into the acid tower is 30-45 times of that of the composite ion exchange resin.
The mass concentration of the liquid caustic soda is 2-10%, and the mass concentration of the hydrochloric acid is 2-10%.
The amount of the extractant pure water in the step 2) is 40 to 55 times of the mass of the weathered coal.
The absorption time of the weathered coal in the composite ion exchange resin cyclone extraction tower is 2-4h.
By adopting the device and the extraction process for extracting the medical-grade fulvic acid from the weathered coal, the fulvic acid entering the nano filter is concentrated to the mass concentration of 3% in the refining process, the purity of the obtained fulvic acid is 98.5%, and the extraction rate of the fulvic acid is 80%.
Claims (9)
1. A device for extracting pharmaceutical-grade fulvic acid from weathered coal is characterized by comprising a pure water preparation unit, a mixed extraction unit, a fulvic acid refining unit and a separation and regeneration unit;
a pure water preparation unit: the device comprises a raw water storage tank (1), a pressure pump (2), a quartz sand filter (3), an activated carbon filter (4), an automatic softener (5), a precision filter (6), a reverse osmosis device (7), a pure water storage tank (8) and a pure water delivery pump (9), wherein the raw water storage tank (1) and the quartz sand filter (3) are connected through the pressure pump (2), and the quartz sand filter (3), the activated carbon filter (4), the automatic softener (5), the precision filter (6), the reverse osmosis device (7) and the pure water storage tank (8) are connected with each other through pipelines;
a mixed extraction unit: the device comprises a composite ion exchange resin cyclone extraction tower (10), a weathered coal hopper (11), a composite ion exchange resin hopper (12), a weathered coal feeder (13), a composite ion exchange resin feeder (14) and a static mixer (15), wherein the composite ion exchange resin cyclone extraction tower (10) is connected with a pure water delivery pump (9), the weathered coal hopper (11) is connected with the weathered coal feeder (13), the composite ion exchange resin hopper (12) is connected with the composite ion exchange resin feeder (14), the weathered coal feeder (13) and the composite ion exchange resin feeder (14) are both connected with the static mixer (15), and the static mixer (15) is connected with a feed inlet of the composite ion exchange resin cyclone extraction tower (10); a filter screen (102) and a cyclone column (101) are arranged in the composite ion exchange resin cyclone extraction tower (10), and the cyclone column (101) is connected with a fan (23);
a fulvic acid refining unit: the device comprises a pipeline pump (24), a tubular centrifugal machine (26) and a nanofiltration machine (27), wherein one end of the pipeline pump (24) is connected with a discharge port I (29) of the composite ion exchange resin cyclone extraction tower (10), the other end of the pipeline pump is connected with the tubular centrifugal machine (26), the tubular centrifugal machine (26) is connected with the nanofiltration machine (27), and the nanofiltration machine (27) is connected with a fulvic acid storage tank (28);
a separation and regeneration unit: the device comprises a liquid caustic soda storage tank (16), a caustic wash pump (17), a caustic wash tower (18), a hydrochloric acid storage tank (19), an acid washing pump (20), an acid washing tower (21) and a composite ion exchange resin regeneration tower (22), wherein the caustic wash tower (18) is connected with a discharge port II (30) of the composite ion exchange resin cyclone extraction tower (10), the caustic wash tower (18) is connected with the acid washing tower (21) through a pipeline with a flow valve, the acid washing tower (21) is connected with the composite ion exchange resin regeneration tower (22), the composite ion exchange resin regeneration tower (22) is connected with a pure water delivery pump (9), the liquid caustic soda storage tank (16) is connected with the caustic wash tower (18) through the caustic wash pump (17), and the hydrochloric acid storage tank (19) is connected with the acid washing tower (21) through the acid washing pump (20).
2. The device for extracting pharmaceutical grade fulvic acid from weathered coal according to claim 1, wherein the swirl column (101) is provided with a plurality of circles of swirl holes, and the holes of the swirl holes are inclined upwards.
3. An extraction process for extracting pharmaceutical-grade fulvic acid from weathered coal is characterized by comprising the following steps of:
1) Preparing pure water: raw water sequentially enters a quartz sand filter, an activated carbon filter, an automatic softener, a precision filter and a reverse osmosis device from a raw water storage tank through a pipeline by a pressure pump to prepare required pure water, and the pure water is stored in a pure water storage tank for later use;
2) Mixing and extracting: starting a fan and adjusting the air quantity until the raw materials cannot enter the swirl holes, allowing the weathered coal and the composite ion exchange resin to enter a static mixer through a weathered coal feeder and a composite ion exchange resin feeder respectively, mixing and then entering a composite ion exchange resin swirl extraction tower, feeding pure water serving as an extractant into the composite ion exchange resin swirl extraction tower from a pure water storage tank by a pure water delivery pump, gradually increasing the air quantity of the fan, injecting air clockwise through the swirl holes in the swirl column along the tangential direction, and adsorbing by resin to obtain a crude fulvic acid aqueous solution;
3) Refining fulvic acid: separating the crude fulvic acid aqueous solution from the composite ion exchange resin through a filter screen at the bottom of the composite ion exchange resin cyclone extraction tower, conveying the separated crude fulvic acid aqueous solution to a tubular centrifuge through a pipeline pump for solid-liquid separation, taking a centrifuged heavy phase as a humic acid organic fertilizer raw material, allowing a light phase to enter a nanofiltration machine through a pipeline for fulvic acid refining and concentration, and conveying a concentrated and refined medical-grade fulvic acid solution to a fulvic acid storage tank;
4) Separation and regeneration: the composite ion exchange resin flows to an alkaline washing tower automatically under the action of dead weight, liquid caustic soda is sprayed into the alkaline washing tower through an alkaline washing pump, and wastewater is discharged through a bottom blow-down valve to be subjected to sewage treatment; after alkaline washing, the composite ion exchange resin flows to an acid washing tower automatically, hydrochloric acid is sprayed into the acid washing tower through an acid washing pump, and wastewater is discharged through a bottom blow-down valve to be subjected to sewage treatment; the acid-washed composite ion exchange resin automatically flows to a composite ion exchange resin regeneration tower, and pure water conveyed by a pure water conveying pump is discharged from the bottom after being washed and circularly enters a composite ion exchange resin cyclone extraction tower for utilization.
4. The extraction process for extracting pharmaceutical fulvic acid from weathered coal according to claim 3, wherein the composite ion exchange resin is composed of a strongly acidic styrene cation exchange resin and a macroporous styrene chelating resin, and the mass ratio of the strongly acidic styrene cation exchange resin to the macroporous styrene chelating resin is 1:1.
5. The process for extracting pharmaceutical fulvic acid from weathered coal according to claim 3, wherein the filling height of the quartz sand in the quartz sand filter is 1.0m, the particle size of the quartz sand is 1-2mm, and the filtration accuracy is 0.005-0.01m.
6. The extraction process for extracting pharmaceutical fulvic acid from weathered coal according to claim 3, wherein the liquid caustic is NaOH alkaline solution, the NaOH alkaline solution sprayed into the caustic tower is 30-45 times the mass of the composite ion exchange resin, and the hydrochloric acid sprayed into the acid tower is 30-45 times the mass of the composite ion exchange resin.
7. The extraction process for extracting pharmaceutical-grade fulvic acid from weathered coal according to claim 3 or 6, wherein the mass concentration of the liquid caustic soda is 2% -10%, and the mass concentration of the hydrochloric acid is 2% -10%.
8. The extraction process for extracting pharmaceutical fulvic acid from weathered coal according to claim 3, wherein the amount of pure water used as the extractant in step 2) is 40-55 times the mass of weathered coal.
9. The extraction process for extracting pharmaceutical fulvic acid from weathered coal according to claim 3, wherein the adsorption time of weathered coal in the composite ion exchange resin cyclone extraction tower is 2-4h.
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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 |
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| MA19999A1 (en) * | 1983-01-25 | 1984-10-01 | Anlad N V | Process for the production of humic and fluvic acids and by-products from peat from peat soils and from humified organic matter |
| JP2004269484A (en) * | 2003-03-06 | 2004-09-30 | Fumihiko Yazaki | Method for producing fulvic acid from low-grade coal using high-temperature water under pressure |
| RU2434048C2 (en) * | 2010-01-19 | 2011-11-20 | Учреждение Российской академии наук Институт угля и углехимии Сибирского отделения РАН (ИУУ СО РАН) | Procedure for preparation of hydroxi-methyl derivatives of brown coal fulvic acids |
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