CN112029114A - Method and device for extracting medical fulvic acid from biomass pyrolysis liquid - Google Patents
Method and device for extracting medical fulvic acid from biomass pyrolysis liquid Download PDFInfo
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- CN112029114A CN112029114A CN202011006606.8A CN202011006606A CN112029114A CN 112029114 A CN112029114 A CN 112029114A CN 202011006606 A CN202011006606 A CN 202011006606A CN 112029114 A CN112029114 A CN 112029114A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
Abstract
The invention discloses a method for extracting medical fulvic acid from biomass pyrolysis liquid, which comprises the following steps: the biomass pyrolysis liquid is filtered in a biomass pyrolysis liquid pretreatment unit and then subjected to fraction splitting, and crude yellow humic acid liquid collected from the side line of a fractionating tower is stored for later use; preparing pure water from raw water through a pure water preparation unit, and storing the pure water in a pure water storage tank; adding the crude fulvic acid liquid, pure water and ion exchange resin into an extraction tower of an extraction unit, and blowing air into the extraction tower to enable the crude fulvic acid liquid, the pure water and the ion exchange resin to be in a boiling state for 3-6 hours; discharging the extracted fulvic acid solution from the bottom of the extraction tower to a fulvic acid concentration unit for concentration by evaporation, and obtaining fulvic acid solution after concentration, and feeding the fulvic acid solution into a fulvic acid storage tank; the ion exchange resin after adsorption flows to a regeneration unit from the extraction tower under the action of gravity to complete regeneration. The process provided by the invention is simple in flow, convenient to operate, low in energy consumption and suitable for industrialization.
Description
Technical Field
The invention relates to the technical field of fulvic acid extraction, in particular to a method and an extraction device for extracting medical fulvic acid from biomass pyrolysis liquid.
Background
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 in the aspect of animal husbandry can promote animals to grow apricot, prevent and treat common diseases of livestock and poultry and the like; 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.
The fulvic acid is used as a multipurpose fine organic additive, the extraction rate of the fulvic acid is low by an alkali-dissolution acidification method, and the extraction time is long; the ion exchange resin extraction process has the defects of complex extraction process, high process energy consumption and high production cost; the acetone sulfate method has the defects of easy volatilization, toxicity and difficult recycling of acetone; the strong acid extraction method has the defects of easy introduction of soluble salt, low product purity and the like; the fermentation method has strict requirements on conditions, the fermentation period is relatively long, and the purity of fulvic acid in the fermentation product is low; the electrodialysis method has complex operation and higher process cost, and is not suitable for industrial production.
A Chinese patent document, named as equipment for extracting water body fulvic acid, discloses equipment, which comprises a raw water supply unit, a pretreatment unit, a nanofiltration concentration unit, a pH value adjusting unit, a water tank, a master control system, a filtration and purification unit and a fulvic acid extraction unit, wherein the fulvic acid extraction unit comprises a leaching device, an alkali liquor medicament tank, an adsorption enrichment device and an ion exchange device; the filtration purification unit can separate fulvic acid from insoluble impurities, and the fulvic acid extraction unit can adsorb and purify fulvic acid to obtain high-concentration fulvic acid extract. The device has higher requirements on raw materials, is more complex and is not suitable for industrial production.
Disclosure of Invention
The invention provides a method and a device for extracting medical fulvic acid from biomass pyrolysis liquid to make up for the defects of the prior art.
The invention is realized by the following technical scheme:
a method for extracting medical fulvic acid from biomass pyrolysis liquid is characterized by comprising the following steps:
(1) pretreatment of biomass pyrolysis liquid: the biomass pyrolysis liquid is filtered in a biomass pyrolysis liquid pretreatment unit and then subjected to fraction splitting, and crude yellow humic acid liquid collected from the side line of a fractionating tower is stored for later use;
(2) preparing pure water: preparing pure water from raw water through a pure water preparation unit, and storing the pure water in a pure water storage tank;
(3) and (3) extraction: adding the crude fulvic acid liquid, pure water and ion exchange resin into an extraction tower of an extraction unit, and blowing air into the extraction tower to enable the crude fulvic acid liquid, the pure water and the ion exchange resin to be in a boiling state for 3-6 hours;
(4) concentrating: discharging the extracted fulvic acid solution from the bottom of the extraction tower to a fulvic acid concentration unit for concentration by evaporation, and obtaining fulvic acid solution after concentration, and feeding the fulvic acid solution into a fulvic acid storage tank;
(5) raw: the ion exchange resin after adsorption flows to a regeneration unit from the extraction tower under the action of gravity to complete regeneration.
In the step (1), the biomass pyrolysis liquid is filtered, thermally vaporized and then enters a fractionating tower for splitting fraction.
The proportion of the crude fulvic acid liquid, the pure water and the ion exchange resin added in the step (3) is that, by volume, 10-40 parts of the crude fulvic acid liquid, 10-40 parts of the extractant pure water and 20-80 parts of the ion exchange resin are added.
The temperature during heating and vaporization is 450-500 ℃.
The utility model provides an extraction element that medical fulvic acid was drawed to living beings pyrolysis liquid, includes pure water preparation unit, still includes living beings pyrolysis liquid pretreatment unit, extraction unit, fulvic acid concentration unit and regeneration unit, the extraction unit pass through the pipeline respectively in living beings pyrolysis liquid pretreatment unit, pure water preparation unit, fulvic acid concentration unit, regeneration unit lead to.
The extraction unit comprises a crude fulvic acid delivery pump, a pure water delivery pump, a fan and an extraction tower; the feeding end of the crude fulvic acid delivery pump is connected with the biomass pyrolysis liquid pretreatment unit through a pipeline, and the discharging end of the crude fulvic acid delivery pump is connected with the feeding port I of the extraction tower through a pipeline; the feed end of the pure water delivery pump is connected with the pure water preparation unit through a pipeline, the discharge end of the pure water delivery pump is connected with the feed inlet II of the extraction tower through a pipeline, and the discharge outlet I of the extraction tower is connected with the feed inlet of the regeneration unit through a pipeline; and a discharge hole of the regeneration unit is connected with a feed inlet IV of the extraction tower (17) through a pipeline.
The biomass thermal decomposition liquid pretreatment unit comprises a biomass thermal decomposition liquid storage tank, a basket type filter, a biomass thermal decomposition liquid delivery pump, a heating furnace, a fractionating tower and a crude fulvic acid storage tank which are sequentially connected through a pipeline, wherein the crude fulvic acid storage tank is connected with the feed end of the crude fulvic acid delivery pump through a pipeline.
The regeneration unit comprises a primary ion exchange resin washing tower and a secondary ion exchange resin washing tower which are connected in series through a pipeline with a flow valve, wherein a feed inlet of the primary ion exchange resin washing tower is connected with a discharge outlet I through a pipeline; the discharge hole of the secondary ion exchange resin washing tower is connected with the feed hole IV through a pipeline; and pure water inlets of the primary ion exchange resin washing tower and the secondary ion exchange resin washing tower are connected with the pure water delivery pump through pipelines.
The fulvic acid concentration unit comprises a three-effect evaporator and a steam condenser which are sequentially connected through a pipeline; the feed inlet of the triple-effect evaporator is connected with the discharge outlet II through a pipeline; the feed inlet of the triple-effect evaporator is connected with a medical fulvic acid storage tank through a pipeline.
An air distribution cap is arranged in the extraction tower, and the air distribution cap is conical and is fully distributed with small holes.
The invention has the following technical effects:
(1) the equipment provided by the invention has the advantages of simple structure, simple process flow, convenience in operation, lower energy consumption and suitability for industrialization.
(2) According to the invention, the medical fulvic acid with high added value is extracted by taking the biomass pyrolysis liquid with low cost as a raw material, so that the added value of the biomass pyrolysis liquid is greatly improved.
(3) The invention carries out ion exchange between the amphoteric ion exchange resin and the crude fulvic acid, and no acid-base waste liquid is generated in the regeneration process, thus having strong environmental friendliness.
(4) The method has the advantages of short fulvic acid extraction time, high extraction efficiency and high purity of the prepared fulvic acid, and reaches medical grade standard.
Drawings
The invention will be further described with reference to the accompanying drawings.
FIG. 1 is a schematic view of the structure of an extraction apparatus according to the present invention;
in the figure: 1-biomass pyrolysis liquid storage tank, 2-basket filter, 3-biomass pyrolysis liquid delivery pump, 4-heating furnace, 5-fractionating tower, 6-crude fulvic acid storage tank, 7-crude fulvic acid delivery pump, 8-raw water storage tank, 9-pressure pump, 10-quartz sand filter, 11-activated carbon filter, 12-softener, 13-reverse osmosis device, 14-pure water storage tank, 15-pure water delivery pump, 16-blower, 17-extraction tower, 171-feed inlet I, 172-feed inlet II, 173-feed inlet III, 174-feed inlet IV, 175-discharge outlet I, 176-discharge outlet II, 177-air distribution hood, 18-first evaporator, 19-first evaporator, 20-first evaporator, 21-condenser, 22-medical fulvic acid storage tank, 23-first-stage ion exchange resin water washing tower and 24-second-stage ion exchange resin water washing tower.
Detailed Description
The invention provides a method for extracting medical fulvic acid from biomass pyrolysis liquid and an extraction device, wherein the structure of the extraction device is shown in figure 1, and the extraction device comprises a biomass pyrolysis liquid pretreatment unit, a pure water preparation unit, an extraction unit, a fulvic acid concentration unit and a regeneration unit which are connected together through pipelines;
the biomass pyrolysis liquid pretreatment unit comprises a biomass pyrolysis liquid storage tank 1, a basket filter 2, a biomass pyrolysis liquid delivery pump 3, a heating furnace 4, a fractionating tower 5 and a crude fulvic acid storage tank 6 which are sequentially connected through pipelines; the heating furnace 4 is used for heating the biomass pyrolysis liquid to 450-500 ℃ and changing the biomass pyrolysis liquid from a liquid phase to a gas phase, and the biomass pyrolysis liquid finally enters the fractionating tower in a gas phase form, so that the fractionating tower does not need a reboiler, the equipment cost is reduced, and the energy consumption is saved.
The pure water preparation unit comprises a raw water storage tank 8, a pressure pump 9, a quartz sand filter 10, an activated carbon filter 11, a softener 12, a reverse osmosis device 13 and a pure water storage tank 14 which are sequentially connected through pipelines, wherein the raw water storage tank 8 is connected with the quartz sand filter 10 through the pressure pump 9, and the quartz sand filter 10, the activated carbon filter 11, the softener 12, the reverse osmosis device 13 and the pure water storage tank 14 are connected with each other through pipelines;
the extraction unit comprises a crude fulvic acid delivery pump 7, a pure water delivery pump 15, a fan 16 and an extraction tower 17, wherein the feed end of the crude fulvic acid delivery pump 7 is connected with the discharge hole of a crude fulvic acid storage tank 6 of the biomass pyrolysis liquid pretreatment unit through a pipeline, the discharge end of the crude fulvic acid delivery pump 7 is connected with a feed inlet I171 of the extraction tower 17, the discharge end of the pure water delivery pump 15 is communicated with a feed inlet II172 of the extraction tower 17 through a pipeline, and the feed end is connected with the discharge hole of a pure water storage tank 14 through a pipeline; the output end of the fan 16 is connected with a feed inlet III173 of the extraction tower 17 through a pipeline; an air distribution cap 177 is arranged inside the extraction tower 17, the air distribution cap 177 is connected with the feed port III173, the cap is conical, small holes are distributed in the cap, and air fed by the fan 17 is uniformly distributed in the extraction tower 17 through the air distribution cap 177.
The fulvic acid concentration unit comprises a triple-effect evaporator and a steam condenser 21 which are sequentially connected through a pipeline, and a discharge outlet II176 of the extraction tower 17 is connected with a feed inlet of the triple-effect evaporator through a pipeline; the discharge port of the triple-effect evaporator is connected with a medical fulvic acid storage tank 22 through a pipeline, and a steam outlet is connected with a steam condenser 21 through a pipeline. The triple-effect evaporator comprises a first evaporator 18, a second evaporator 19 and a third evaporator 20 which are sequentially connected in series, and a discharge hole II176 of the extraction tower 17 is connected with a feed inlet of the first evaporator 18 through a pipeline; the triple-effect evaporator is concentrated by adopting a downstream feeding mode.
The regeneration unit comprises a first-stage ion exchange resin washing tower (23) and a second-stage ion exchange resin washing tower (24), wherein the first-stage ion exchange resin washing tower (23) is connected with a discharge port I (175) of the extraction tower (17), the first-stage ion exchange resin washing tower (23) is connected with the second-stage ion exchange resin washing tower (24) through a pipeline with a flow valve, and the quantity entering the second-stage ion exchange resin washing tower (24) is controlled so as to better clean the ion exchange resin.
The method for extracting fulvic acid by using the extraction device is as follows
(1) Pretreatment of biomass pyrolysis liquid: the method comprises the following steps that after fly ash is removed by filtering biomass pyrolysis liquid through a basket filter 2, the biomass pyrolysis liquid is conveyed into a heating furnace 4 through a biomass pyrolysis liquid conveying pump 3, the heated temperature is 450-500 ℃, the biomass pyrolysis liquid is changed into steam to enter a fractionating tower 5, fractions with different temperatures are cut in the fractionating tower 5, crude fulvic acid liquid collected from a side line enters a crude fulvic acid storage tank, namely, a gas phase enters the fractionating tower 5, the gas enters the fractionating tower and flows upwards to exchange heat with descending liquid, non-condensable gas is led out from the top of the tower, and condensate is led out from the side line according to different boiling points of the fractions to obtain the crude fulvic acid;
(2) preparing pure water: raw water sequentially enters a quartz sand filter 10, an activated carbon filter 11, a softener 12 and a reverse osmosis device 13 from a raw water storage tank through pipelines by a pressure pump to prepare required pure water, and the pure water is stored in a pure water storage tank 14 for later use; wherein the filtering precision of the quartz sand filter 10 is 6 mm-12 mm, the inner part is filled with quartz sand with the height of 0.5 m-1.2 m and the grain diameter of 1 mm-3 mm; the filtering precision of the activated carbon filter 11 is 0.1 mm-5 mm, the inside is filled with activated carbon particles with the height of 0.5-1.2 m and the diameter of 0.5-1.5 mm.
(3) And (3) extraction: adding 10-40 parts by volume of crude yellow humic acid liquid, 10-40 parts by volume of extractant pure water and 20-80 parts by volume of ion exchange resin into an extraction tower 17; wherein, the crude fulvic acid is fed into the extraction tower 17 through a feed inlet I171 at the upper part of the extraction tower by a crude fulvic acid delivery pump 3, the pure water is fed into the lower part of the extraction tower 17 through a feed inlet II172 by a pure water delivery pump 15, the ion exchange resin is fed into the extraction tower from a feed inlet IV at the top of the extraction tower 17, and the crude fulvic acid liquid is in countercurrent contact with the pure water; and starting the fan 16 to blow air into the extraction tower through the feed port III173 and the air distribution cap, so that the crude fulvic acid, the pure water and the ion exchange resin are in a boiling state for 3-6 hours, and the mass transfer and ion exchange efficiency of the crude fulvic acid, the pure water and the ion exchange resin are enhanced. Exchanging hydrogen ions contained in the ion exchange resin in the extraction tower with metal ions of the crude fulvic acid solution to convert fulvic acid salt into fulvic acid, and extracting fulvic acid solution by using pure water as an extracting agent; after extraction is completed, the gas is stopped, and the liquid and the ion exchange resin are treated separately.
(4) Concentrating: the extracted fulvic acid solution is discharged to a three-effect evaporator for concentration through a discharge hole II176 at the bottom of the extraction tower 17, and the concentrated fulvic acid solution enters a fulvic acid storage tank.
(5) Regeneration: the amphoteric ion exchange resin after adsorption flows to a first-stage ion exchange resin washing tower 23 under the action of gravity from the extraction tower, and flows to a second-stage ion exchange resin washing tower 24 after being washed by pure water, so that the amphoteric ion exchange resin is regenerated. The regenerated amphoteric ion exchange resin is added into the extraction tower for recycling through a feed inlet IV at the top of the extraction tower 17.
The concentration of the yellow humic acid solution extracted by the method can reach 10%, the purity is more than 98.6%, and the extraction rate is as high as 82%.
The foregoing is only a preferred embodiment of the present invention; the scope of the invention is not limited thereto. Any person skilled in the art should be able to cover the technical scope of the present invention by equivalent or modified solutions and modifications within the technical scope of the present invention.
Claims (10)
1. A method for extracting medical fulvic acid from biomass pyrolysis liquid is characterized by comprising the following steps:
(1) pretreatment of biomass pyrolysis liquid: the biomass pyrolysis liquid is filtered in a biomass pyrolysis liquid pretreatment unit and then subjected to fraction splitting, and crude yellow humic acid liquid collected from the side line of a fractionating tower is stored for later use;
(2) preparing pure water: preparing pure water from raw water through a pure water preparation unit, and storing the pure water in a pure water storage tank;
(3) and (3) extraction: adding the crude fulvic acid liquid, pure water and ion exchange resin into an extraction tower of an extraction unit, and blowing air into the extraction tower to enable the crude fulvic acid liquid, the pure water and the ion exchange resin to be in a boiling state for 3-6 hours;
(4) concentrating: discharging the extracted fulvic acid solution from the bottom of the extraction tower to a fulvic acid concentration unit for concentration by evaporation, and obtaining fulvic acid solution after concentration, and feeding the fulvic acid solution into a fulvic acid storage tank;
(5) regeneration: the amphoteric ion exchange resin after adsorption flows to a regeneration unit from the extraction tower under the action of gravity to complete regeneration.
2. The method for extracting medical fulvic acid from biomass pyrolysis liquid as claimed in claim 1, is characterized in that: in the step (1), the biomass pyrolysis liquid is filtered, thermally vaporized and then enters a fractionating tower for splitting fraction.
3. The method for extracting medical fulvic acid from biomass pyrolysis liquid as claimed in claim 1, is characterized in that: the proportion of the crude fulvic acid liquid, the pure water and the ion exchange resin added in the step (3) is that, by volume, 10-40 parts of the crude fulvic acid liquid, 10-40 parts of the extractant pure water and 20-80 parts of the ion exchange resin are added.
4. The method for extracting medical fulvic acid from biomass pyrolysis liquid as claimed in claim 2, is characterized in that: the temperature during heating and vaporization is 450-500 ℃.
5. The utility model provides an extraction element of medical fulvic acid is drawed to living beings pyrolysis liquid, includes pure water preparation unit, its characterized in that: the device is characterized by further comprising a biomass thermal decomposition liquid pretreatment unit, an extraction unit, a fulvic acid concentration unit and a regeneration unit, wherein the extraction unit is respectively connected with the biomass thermal decomposition liquid pretreatment unit, the pure water preparation unit, the fulvic acid concentration unit and the regeneration unit through pipelines.
6. The device for extracting medical fulvic acid from biomass pyrolysis liquid as claimed in claim 5, is characterized in that: the extraction unit comprises a crude fulvic acid delivery pump (7), a pure water delivery pump (15), a fan (16) and an extraction tower (17); the feeding end of the crude fulvic acid delivery pump (7) is connected with the biomass pyrolysis liquid pretreatment unit through a pipeline, and the discharging end of the crude fulvic acid delivery pump is connected with a feeding hole I (171) of the extraction tower (17) through a pipeline; the feed end of the pure water delivery pump (15) is connected with the pure water preparation unit through a pipeline, the discharge end of the pure water delivery pump is connected with the feed inlet II (172) of the extraction tower (17) through a pipeline, and the discharge outlet I (175) of the extraction tower (17) is connected with the feed inlet of the regeneration unit through a pipeline; the discharge hole of the regeneration unit is connected with the feed inlet IV (174) of the extraction tower (17) through a pipeline.
7. The device for extracting medical fulvic acid from biomass pyrolysis liquid according to claim 5 or 6, is characterized in that: the biomass thermal decomposition liquid pretreatment unit comprises a biomass thermal decomposition liquid storage tank (1), a basket type filter (2), a biomass thermal decomposition liquid delivery pump (3), a heating furnace (4), a fractionating tower (5) and a crude fulvic acid storage tank (6) which are sequentially connected through a pipeline, wherein the crude fulvic acid storage tank (6) is connected with the feed end of the crude fulvic acid delivery pump (7) through a pipeline.
8. The device for extracting medical fulvic acid from biomass pyrolysis liquid as claimed in claim 7, wherein: the regeneration unit comprises a primary ion exchange resin washing tower (23) and a secondary ion exchange resin washing tower (24) which are connected in series through a pipeline with a flow valve, wherein a feed inlet of the primary ion exchange resin washing tower (23) is connected with a discharge outlet I (175) through a pipeline; the discharge hole of the secondary ion exchange resin water washing tower (24) is connected with the feed hole IV (174) through a pipeline; and pure water inlets of the primary ion exchange resin water washing tower (23) and the secondary ion exchange resin water washing tower (24) are connected with the pure water delivery pump (15) through pipelines.
9. The device for extracting medical fulvic acid from biomass pyrolysis liquid as recited in claim 8, wherein: the fulvic acid concentration unit comprises a three-effect evaporator and a steam condenser (21) which are sequentially connected through a pipeline; the feed inlet of the triple-effect evaporator is connected with the discharge outlet II (176) through a pipeline; the feed inlet of the triple-effect evaporator is connected with a medical fulvic acid storage tank (22) through a pipeline.
10. The device for extracting medical fulvic acid from biomass pyrolysis liquid as recited in claim 8, wherein: an air distribution cap cover (177) is installed in the extraction tower (17), and the air distribution cap cover (177) is conical and is fully distributed with small holes.
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Cited By (1)
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| CN112957770A (en) * | 2021-03-11 | 2021-06-15 | 江苏扬农化工集团有限公司 | Continuous extraction device and continuous extraction method for epichlorohydrin |
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