CN106519259A - Equipment for extracting fulvic acid from water body - Google Patents
Equipment for extracting fulvic acid from water body Download PDFInfo
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- CN106519259A CN106519259A CN201610922048.7A CN201610922048A CN106519259A CN 106519259 A CN106519259 A CN 106519259A CN 201610922048 A CN201610922048 A CN 201610922048A CN 106519259 A CN106519259 A CN 106519259A
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- 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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Abstract
The invention provides equipment for extracting fulvic acid from a water body and a preparation method thereof. The equipment for extracting fulvic acid from a water body comprises a raw water supply unit, a pretreatment unit, a nanofiltration concentration unit, an acid-base value regulating unit, a water tank, a master control system, a filtration purification unit and a fulvic acid extraction unit. The fulvic acid extraction unit comprises a leaching apparatus, an alkali lye chemical tank, an adsorption enrichment apparatus and an ion exchange unit. The filtration purification unit can separate fulvic acid from insoluble impurities. The fulvic acid extraction unit can be used for adsorbing and purifying fulvic acid so as to obtain high-concentration fulvic acid extracting solution. The equipment for extracting fulvic acid from the water body has a simple structure, has high degree of automation and is convenient to operate.
Description
Technical field
A kind of the present invention relates to concentration technique field, more particularly to equipment for extracting water body fulvic acid.
Background technology
DOM is that a class natural macromolecular Organic substance that can be by aperture span for 0.1-0.7 μm of filter membrane is mixed
Compound, it derives from animals and plants secretions and its Residue decay product, and the Nomenclature Composition and Structure of Complexes changes with space-time and source.In fresh water
In Marine water, DOM has important ecological and environmental activity.DOM mainly includes humic acid, fulvic acid
Deng acidic materials, and the acidic materials molecular weight such as humic acid, fulvic acid is big, it is difficult to degrade, and is main in DOM
Composition, by extensive concern.Solvable under any pH value condition, animal migration is strong, the heavy metal and poisonous and harmful in fulvic acid and water
Material occurs to interact, and then realizes the conversion in the environment of heavy metal and poisonous and harmful hard-degraded substance, migrates and return
Place.In natural water body, fulvic acid absolute content is very low, and in fresh water, concentration is generally 1-5mg/L, is generally 0.1- in sea water
1mg/L.But, how to realize that the humic acid for efficiently extracting high concentration from water body is the problem of urgent need to resolve at present.
Nanofiltration process is that a kind of low-pressure of similar mechanical screening drives membrane separating process.Apparatus of the present invention utilize nanofiltration
Journey, realization are dammed to DOM in water body, remove monovalention (such as while nanofiltration is concentrated：Sodium ion and chlorine
Ion) and molecular weight less than 200 dalton Organic substance.Apparatus of the present invention are used for fresh water or Marine water DOM
Nanofiltration concentration, purification.
Li Huijie has delivered master thesis, and thesis topic is that " extraction of humic acid and fulvic acid is ground with sign
Study carefully (Central China University of Science and Technology, architectural and civil engineering specialty) ", disclose a kind of extraction of fulvic acid, purification process, its extract and
Purification depends primarily on what laboratory condition and some simple equipment were completed, and the method is included in the extraction of fulvic acid and richness
Two steps of purification of acid.
Detailed extraction purification flow process is as shown in Figure 2.
Fulvic acid method for extraction and purification disclosed in this Master's thesis depends primarily on laboratory condition and some are simple
What equipment was completed, operating process is complicated, and automaticity is low, can not form a complete and operation during whole extraction
Convenient system；In addition, fulvic acid extracting method disclosed in this paper is affected greatly by manual operation, it is impossible to be widely used in fresh water
With the extraction and contrast of DOM fulvic acid in Marine water, exploitativeness is good.
The content of the invention
In order to realize being separated from the water fulvic acid and which be extracted and purification, the invention provides a kind of be used for extracting
The equipment of water body fulvic acid, the fulvic acid needed for effectively easily can extracting.
In order to solve above-mentioned technical problem, a kind of equipment for extracting water body fulvic acid of the present invention is supplied including raw water
To unit, pretreatment unit, nanofiltration upgrading unit, acid-base value adjustment unit, water tank, general control system, filtration, purification unit and
Fulvic acid extraction unit；
The filtration, purification unit includes filter, liquid memory and vacuum pump, the entrance of the filter with it is described
The outlet connection of water tank, the outlet of the filter are connected with the entrance of the liquid memory；The vacuum pump and the liquid
Body bin connects；The outlet of the liquid memory is connected with the entrance of the adsorption and enrichment device；
The fulvic acid extraction unit includes elution device, alkali liquor chemical tank, adsorption and enrichment device and ion interchange unit,
The entrance of the adsorption and enrichment device and the outlet of the liquid memory, the outlet of elution device, the outlet of alkali liquor chemical tank
Connection, the outlet of adsorption and enrichment device are connected with the entrance of the ion interchange unit；
The entrance of the ion interchange unit is connected with the outlet of elution device, the adsorption and enrichment device, ion exchange
The bottom of device is equipped with tapping valve；
The adsorption and enrichment device includes adsorption column and filler, and in the adsorption column, described filler is described filler
One or more of XAD-8 resins, DAX-8 resins and XAD-7 resins；
The ion interchange unit includes adsorption column and filler, and in the adsorption column, described filler is described filler
Hydrogen type cation exchange resin.
Preferably, it is preferable that the raw water feed unit adopts self-priming water supplying pump, raw water to be sea water or fresh water, raw water water
, within 1000NTU, within 1000mg/l, electrical conductivity value is within 40000 μ S/cm for the value of TOC for the turbidity of matter；Self-priming
The front end of pump is provided with filter bag, and the aperture of the filter bag is 10 μm.
Preferably, the water tank adopts acid resisting material, and which is provided with closure above；Agitator, level sensing is provided with which
Device and pH sensors；The end face of the closure is provided with least 5 through holes；Pipeline depth between the water tank and the filter
Enter in water tank, it is sealing structure to stretch at the top of the pipeline of water tank, duct wall is provided with the hole that multiple apertures are 50 μm, the minimum height in hole
At the 1/100-1/10 of tank height, the tank pipe that stretches into is externally provided with filter mantle, the aperture of the filter mantle for degree control
For 100 μm.
Preferably, the pretreatment unit includes one-level precision microfiltration filter, two grades of accurate microfiltration filters, three-level essences
Close microfiltration filter, in one-level precision microfiltration filter, the aperture of precision Filter element is 1 μm, accurate in two grades of accurate microfiltration filters
The aperture of filter element is 0.45 μm, and in three-level precision microfiltration filter, the aperture of precision Filter element is 0.22 μm；The one-level precision is micro-
The entrance of filtration filter be connected with the outlet of self priming pump, the outlet of one-level precision microfiltration filter and two grades of precision microfiltration filters
Entrance connection, the outlet of two grades of accurate microfiltration filters is connected with the entrance of the accurate microfiltration filter of three-level, and three-level precision is micro-
The outlet of filtration filter is connected with water tank.
Preferably, one-level, two grades, three-level precision Filter element adopt polypropylene filter element, precision Filter element to need to change in time, can
To avoid blocking and excessive contaminants cooperating microorganisms.
Preferably, the nanofiltration upgrading unit includes nano-filtration unit, high-pressure pump, TOC on-line monitorings probe and second
TOC on-line monitoring probes；Wherein nano-filtration unit includes NF membrane and rustless steel putamina, and the aperture value of the NF membrane is 1-
2nm；
The first TOC on-line monitorings probe is located at the nano-filtration unit concentrated water exit, the 2nd TOC on-line monitoring probes
At the wastewater outlet of nano-filtration unit, by contrasting two TOC on-line monitoring probe detection numerical value, it can be determined that NF membrane work
Whether good make state.
Preferably, the nano-filtration unit is provided with liquid-inlet, concentrated water outlet and wastewater outlet；The liquid-inlet is by height
Press pump is connected with water tank, and the concentrated water outlet is connected with water tank, and the waste water is discharged by pipeline；The nano-filtration unit and high pressure
Security valve is provided between pump, and concentrated water outlet is provided with security valve.
Preferably, the acid-base value adjustment unit includes pH sensors, agitator, metering dosing pump, acid solution chemical tank；
In water tank, the entrance for measuring dosing pump is connected the pH sensors with the outlet of acid solution chemical tank, measures going out for dosing pump
Mouth is connected with water tank.
Preferably, the filter includes impurity room, filter membrane and core, and the filter membrane is located in impurity room, and by core
Support；The aperture span of the filter membrane is 0.1-0.7 μm.
Preferably, the general control system includes control unit and touch screen device, and described control unit is connected with touch screen device, institute
State control unit to be connected with self priming pump, liquid level sensor, pH sensors, metering dosing pump, high-pressure pump and acid-base value adjustment unit；
The pH sensors are provided with lifting platform, can rise to pH sensors outside water tank if necessary.
Utilizing carries out dissolving the method that fulvic acid is extracted for the equipment for extracting water body fulvic acid, comprises the steps：
(1) open total control switch：Start the main power start button of general control system；
(2) treating nature water：Start self priming pump start button, self priming pump draws raw water by pipeline, self priming pump front end
Filter bag is tentatively filtered to raw water, and the raw water after preliminary filtration is by the supercharging of self priming pump in pretreatment unit
The accurate microfiltration filter of level is once filtered to raw water, and the raw water Jing after once filtering is entered into two grades of accurate microfiltration filters
Row secondary filter；Raw water after secondary filter carries out three filtrations, the original after three filtrations into three-level precision microfiltration filter
Water enters water tank by pipeline；When the water level in water tank reaches 4/5 tank height, self priming pump quits work；
(3) nanofiltration concentration：Raw water Jing high-pressure pump supercharging in water tank enters into nanofiltration upgrading unit, NF membrane by pipeline
Natural Dissolved Organic Matter in raw water can be concentrated, obtain waste water and concentrated water；Through the direct discharging of waste water of NF membrane, concentrated water
Water tank is recycled into, the content of the organic carbon that the dissolved organic carbon on-line determination device in positioned at water tank is determined reaches preset value
When, stop concentration；
(4) acid-base value is adjusted：Start acid-base value adjustment unit, metering dosing pump receives pH sensor signals startup acid solution and adds
Enter program, acid solution is extracted from acid solution chemical tank by pipeline non-oxidizable acid solution is injected in water tank by acid-resistant pipeline, while
In water tank, stirring motor starts so that acid solution and concentrated water uniformly mix, and until reaching default pH value, measures dosing pump acid liquid
Program stopped works；
(5) filter purification：The outlet valve of water tank is opened, while starting vacuum pump, is pressed by vacuum pump, in water tank
Concentrated water is by, in filter influent bin, sour insoluble impurity is removed by membrane retention, is slightly carried fulvic acid solution and is passed through
In filter membrane influent bin；
(6) adsorption and enrichment：The outlet valve of water tank after the completion of filtration, is closed, the outlet valve of liquid memory, liquid is opened
Liquid in body bin flows into adsorption and enrichment device, and fulvic acid is attracted on resin, and waste liquid is discharged from tapping valve；
(7) alkali liquor eluting：After the completion of absorption, the valve between elution device and adsorption and enrichment device is opened, while opening
The tapping valve of adsorption and enrichment bottom of device, the pure water in elution device inject adsorption and enrichment device by pipeline, to adsorption and enrichment
Device is rinsed, and the waste liquid after flushing is directly discharged from tapping valve；Open the company between elution device and ion interchange unit
Port valve, the pure water in elution device inject ion interchange unit by pipeline, ion interchange unit are rinsed, after flushing
Waste liquid is directly discharged from tapping valve；
After the completion of flushing, the communicating valve closed between elution device and ion interchange unit opens alkali liquor chemical tank and suction
Communicating valve between attached enriching apparatus, the alkali liquor in alkali liquor chemical tank inject alkali by alkaline-resisting pipeline in adsorption and enrichment device
, there is desorbing by the fulvic acid after resin absorption in liquid in the presence of alkali liquor, after the solution after desorbing flows through ion interchange unit
Flow out, be labeled as fulvic acid solution；
After fulvic acid solution is freeze-dried, gained solid is solid-state fulvic acid powder.
Preferably, nano-filtration unit waste liquid discharge line is provided with flow speed control valve, on the discharge line of the nano-filtration unit concentrated water
Flow speed control valve is provided with, the wastewater flow rate that NF membrane is discharged is 1 with the ratio of the concentrated water amount discharged:9-9:1, preferably 2:1-1:2.
Preferably, the degree of the acid-resistant pipeline can bear the non-oxidizing acid of 10mol/L；The preset value of the pH is 0.5-
3；The alkali liquor chemical tank and alkaline-resisting requirements for pipes can bear the highly basic of 0.5mol/L.
Preferably, the front end of the high-pressure pump is provided with pressure gauge and relief valve, in raw water concentration process, before the high-pressure pump
When pressure is more than preset value, the relief valve is opened, it is to avoid high-pressure pump is damaged and pipeline burst phenomenon.
Preferably, NF membrane can not dry-storage, it is necessary to assure have water in putamina, if equipment is left unused for some reason more than 70h, answers
NF membrane is soaked in clean water, if long-term leaving unused must be sealed up for safekeeping by NF membrane requirement storage mode.
Preferably, general control system adopts low-voltage distribution, and the electric pressure of power supplying and distributing equipment is 220VAC, and sets low pressure and match somebody with somebody
Electric cabinet, powers to process system power-equipment；On and off switch in control system is protected with electrical control cubicles gate interlock, can be reached anti-
Dirt, rapid heat dissipation and easy-to-install effect.
Preferably, the front end of the self priming pump is provided with relief valve, is provided with liquid level sensor in the water tank, and its water level is in water
During 4/5 water tank volume of case, the relief valve is opened, and self priming pump shuts down, it is to avoid cistern water level is too high.
The beneficial effect comprise that compared with prior art：
(1) present invention provides a kind of simple device structure for extracting water body fulvic acid, high degree of automation, operation side
Just, easily and effectively by other impurity separation of fulvic acid can extract substantial amounts of fulvic acid, preferably utilize in extracted richness
Acid；
(2) the one-level precision Filter element aperture in the present invention is 1 μm, and two grades of precision Filter element apertures are 0.45 μm, and three-level is accurate
Filter element aperture is 0.22 μm, has more effectively filtered the impurity such as the float of larger particles in water, has preferably avoided granule miscellaneous
Scuffing, blocking and impacting with high pressure that thing is caused to film, reduce the replacement frequency of precision Filter element；
(3) whole process that acid-base value adjustment unit adjusts pH value is full automatic, saves labour force, reduces production
Cost, the accuracy rate of the pH value of modulation are higher；
(4) the pure water amount discharged in nano-filtration unit in nanofiltration upgrading unit is 2 with the ratio of the concentrated water amount discharged:1-1:2,
And then pure water discharge can be avoided excessive or the too small injury caused to film or device efficiency reduction.
Description of the drawings
Fig. 1 is a kind of apparatus and process flow chart for extracting water body fulvic acid of the present invention；
Fig. 2 is fulvic acid extraction purification flow chart in background technology.
Specific embodiment
Below in conjunction with the accompanying drawings, the specific embodiment of the present invention is described in detail.
Shown in ginseng Fig. 1, Fig. 1 is the present invention for extracting the process chart of the equipment of water body fulvic acid.The present invention is provided
The equipment for extracting water body fulvic acid, including raw water feed unit, pretreatment unit, nanofiltration upgrading unit, acid-base value adjust
Section unit, water tank 7, general control system 4, filtration, purification unit and fulvic acid extraction unit；Wherein raw water feed unit is mainly wrapped
Include self priming pump 1；Pretreatment unit includes the accurate microfiltration filter 3 of 2, two grades of one-level precision microfiltration filter and three-level precision microfiltration
Filter 18；Nanofiltration upgrading unit includes nano-filtration unit 9, high-pressure pump 8 and dissolved organic carbon on-line monitoring equipment, wherein nanofiltration list
Unit 9 includes NF membrane and rustless steel putamina；Acid-base value adjustment unit includes PH sensors, metering dosing pump 5, acid solution chemical tank 6；
Filtration, purification unit includes liquid memory 16, filter, vacuum pump 15, and wherein filter includes impurity room 12,13 and of filter membrane
Core 14, filter membrane 13 are located in impurity room 12, and are supported by core 14；Fulvic acid extraction unit includes elution device 17, alkali liquor
Chemical tank 19, adsorption and enrichment device 20, ion interchange unit 21；General control system 4 is main to be controlled using electrical equipment, therein
Collection control operation unification in switch board is carried out, and whole system can be made to realize automatically controlling operation and manual operation.
Wherein, the entrance of one-level precision microfiltration filter 2 is connected with the outlet of self priming pump 1, one-level precision microfiltration filter 2
Outlet be connected with the entrance of two grades of accurate microfiltration filters 3, the outlet of two grades of precision microfiltration filters 3 is micro- with three-level precision
The entrance connection of filtration filter 18, the outlet of three-level precision microfiltration filter 18 are connected with water tank 7；PH sensors are located at water tank 7
In, the entrance for measuring dosing pump 5 is connected with the outlet of acid solution chemical tank 6, and the outlet for measuring dosing pump 5 is connected with water tank 7；Nanofiltration
Unit 9 is provided with liquid-inlet, concentrated water outlet and wastewater outlet；Liquid-inlet is connected with water tank 7 by high-pressure pump 8, concentrated water outlet
It is connected with water tank 7, direct discharging of waste water；The entrance of liquid memory 16 is connected with filter outlet, the entrance and water of filter
The outlet connection of case 7；The air entry of vacuum pump 15 is placed in the cavity of liquid memory 16；The outlet and suction of liquid memory 16
The entrance connection of attached enriching apparatus 20；
Outlet of the entrance of adsorption and enrichment device 20 also with elution device 17, the outlet of alkali liquor chemical tank 19 are connected, absorption
The outlet of enriching apparatus 20 is connected with the entrance of ion interchange unit 21；The entrance of ion interchange unit 21 also with elution device 17
Outlet, organic liquor chemical tank 19 outlet connection；The bottom of adsorption and enrichment device 20, the bottom of ion interchange unit 21 are all provided with
There is waste liquid waste cock；
General control system 4 includes control unit and touch screen device, and control unit is connected with touch screen device, control unit and self priming pump
1st, liquid level sensor, pH sensors, metering dosing pump 5, high-pressure pump 8 and vacuum pump 15 connect.
Provided by the present invention for extracting the equipment of water body fulvic acid, its water body water source is sea water or fresh water, the water of raw water
Matter requires turbidity within 1000NTU, and, within 1000mg/L, electrical conductivity value is within 40000 μ S/cm for the value of TOC；From
The front end of sucking pump is provided with filter bag, and the aperture of filter bag is 10 μm.
General control system adopts low-voltage distribution, and the electric pressure of power supplying and distributing equipment is 220VAC, and sets low-voltage distribution cabinet, to
Process system power-equipment is powered.In addition, in control system, be equipped with the switch board of independent operation, and electric switch and electric unit
Part is all concentrated in switch board, and on and off switch and electrical control cubicles gate interlock are protected, and can reach dust-proof, rapid heat dissipation and easy-to-install
Effect.
Main power and start button is first turned on, makes whole system in running order, self priming pump 1 is drawn by pipeline former
Water, raw water are tentatively filtered by the filter bag positioned at self priming pump front end, and the aperture of filter bag is 10 μm, through preliminary filtration
Raw water once mistake is carried out into the one-level precision microfiltration filter 2 in pretreatment unit to raw water by the supercharging of self priming pump
Filter, the raw water Jing after once filtering carry out secondary filtration into two grades of accurate microfiltration filters 3, the raw water Jing after secondary filter
Into three-level precision microfiltration filter 18, wherein, the filter element aperture in one-level precision microfiltration filter 2 is 1 μm, and two grades of precisions are micro-
Filter element aperture in filtration filter 3 is 0.45 μm, and the filter element aperture in three-level precision microfiltration filter 18 is 0.22 μm, this kind of filter
Core diameter is arranged and can preferably filter the impurity such as the float of larger particles in water, is increased water quality, is more effectively avoided granule
Scuffing, blocking and impacting with high pressure that thing impurity is caused to film.In addition, precision Filter element needs to change in time, it is to avoid block and excessive
Pollutant gather cooperating microorganisms.
Raw water after three-level precise filtering device is filtered enters water tank 7 by connecting pipe, and the liquid level in water tank 7 is passed
Sensor is detected to the water level in water tank, and when water level reaches the 4/5 of water tank volume, liquid level sensor is sent out to general control system
After sending liquid level signal, general control system to receive liquid level signal, control signal is sent to self priming pump so as to quit work, that is, stop
The water filling in water tank.
The water tank adopts acid resisting material, and which is provided with closure above, is provided with agitator and pH sensors in which；It is described close
The end face of capping is provided with least 5 through holes.
Raw water in water tank 7 through the pressurization of high-pressure pump 8 into the NF membrane in nano-filtration unit 9, NF membrane can by fresh water or
Marine water is separated into concentrated water and waste water, can be expelled directly out through the waste water of the saliferous of NF membrane and small molecule organic matter, receive
The waste water discharge opening of filter unit 9 is provided with flow speed control valve, can adjust the speed that waste water stream goes out NF membrane, and its speed range of accommodation is
0-200L/h；The concentrated water of Jing nanofiltration membrane separation is back in water tank 7 through pipeline, in nano-filtration unit 9 with 7 connecting pipe of water tank
Flow speed control valve is provided with, the speed that concentrated stream goes out NF membrane can be adjusted, its speed range of accommodation is 0-200L/h；Waste water stream goes out nanofiltration
The speed of film and concentrated stream go out the speed value of NF membrane and are arranged in appropriate scope, make wastewater flow rate and the row of NF membrane discharge
The ratio of the concentrated water amount for going out is 1:9-9:1, so can avoid because waste water flow out excessive velocities or slowly NF membrane is caused excessively
Injury or device efficiency reduce.Concentrated water water tank inlet can circulate concentration, and so repeatedly, the water in raw water box is fewer and feweri,
The concentration more and more higher of the content of organic matter, when the organic carbon content that the dissolved organic carbon on-line determination device in water tank is determined reaches
During preset value, stop concentration, close concentration systems.
During raw water is concentrated, avoid that cocnentration factor is too high as far as possible, cocnentration factor is higher, and concentration containing organic matter is higher, mistake
High concentration can be damaged to NF membrane, therefore, the content of organic matter in concentrated water is controlled in below 10000mg/L.
9 waste outflow pipe of nano-filtration unit is provided with the 2nd TOC on-line monitorings probe 11, nano-filtration unit concentrated water discharge line
Place is provided with TOC on-line monitorings probe 10, is visited by contrasting TOC on-line monitorings probe 10 and the 2nd TOC on-line monitorings
The numerical value of 11 detections, it is possible to determine that NF membrane whether seepage；If i.e. TOC on-line monitorings probe 10 and the 2nd TOC exist
The numerical difference of 10 detection of line monitoring probe is less than preset value, it is possible to determine that Seepage occurs in NF membrane.Nano-filtration unit concentrated water and
The exit of waste water is additionally provided with security valve, in raw water concentration process, the dissolved organic carbon difference of nano-filtration unit concentrated water and waste water
During less than preset value, security valve is opened, and now system is out of service.
The front end of high-pressure pump 8 is provided with security valve, and during concentration, when water level less than water tank 1/5, security valve is opened
Open, high-pressure pump 8 shuts down, it is possible thereby to avoid high-pressure pump from causing the phenomenon that high-pressure pump burns when dallying；The front end of high-pressure pump
Pressure gauge is additionally provided with, when the pressure before high-pressure pump is more than preset value, security valve is opened, high-pressure pump can be avoided to damage and pipeline
Decrepitation Phenomena.
After raw water concentration terminates, start acid-base value adjustment unit.PH value needed for arranging in general control system 4, which sets
Fixed pH value is 0.5-3, and pH value signal transmission adds journey to metering dosing pump 5, metering dosing pump startup acid solution by pH sensors
Sequence, extracts acid solution from acid solution chemical tank 6 and injects non-oxidizable acid solution in water tank by acid-resistant pipeline, while stirring in water tank 7
Mix motor starting so that acid solution and concentrated water uniformly mix, carry out pH value regulation, until pH value reaches the value for pre-setting, metering
Dosing pump acid liquid program stopped works, and metering dosing pump and water tank stirring motor quit work, solution left standstill 4-24h.
If containing excessive ash in extracted fulvic acid, the pH for pre-setting is adjusted to non-oxidizable acid solution is added
After value, dense Fluohydric acid. is added, make hydrofluoric acid concentration between 0.1-0.5mol/L, then solution left standstill 4-24h, solid so as to reduce
State fulvic acid ash.
The process that whole pH value is adjusted is full automatic, saves labour force, reduces production cost, and the pH for modulating
The degree of accuracy of value is higher, and the efficiency of process for preparation is also higher.During pH regulator, turn on agitator motor stirs agitator
Mix the water in water tank 7 so that flow into acid solution medicament therein and uniformly dissolve in water, the pH value of local can be avoided higher or low.
Water tank 7 adopts acid resisting material, and which is provided with closure above, and the end face of closure is provided with least 5 through holes；Lower end
Preferably funnel shaped, is conducive to the output of concentrated water；Agitator and pH sensors is provided with which；PH sensors are provided with lifting platform,
After the completion of pH value is adjusted, lifting platform can rise to pH sensors on the water surface.
Pipeline between water tank and filter gos deep in water tank, is sealing structure at the top of pipeline, and duct wall is provided with multiple holes
Footpath is 50 μm of hole, and at the 1/100-1/10 of tank height, the tank pipe that stretches into is externally provided with for the minimum altitude control in hole
Filter mantle, the aperture of the filter mantle is 100 μm, is more beneficial for precipitating the impurity in concentrated water.
The outlet valve of water tank 7 is opened, while starting vacuum pump 15, is pressed by vacuum pump 15, the concentrated water in water tank 7 is led to
Cross in solution strainer influent bin 16, sour insoluble impurity is retained and removed by filter membrane 13, slightly carry fulvic acid solution and lead to
In filter membrane influent bin 16.
The outlet valve of water tank after the completion of filtration, is closed, the outlet valve of liquid memory is opened, in liquid memory 16
Liquid flow into adsorption and enrichment device 20, fulvic acid is attracted on resin, and waste liquid is discharged from tapping valve；
After the completion of absorption, the valve between elution device 17 and adsorption and enrichment device 20 is opened, while opening adsorption and enrichment
The tapping valve of 20 bottom of device, the pure water in elution device 17 inject adsorption and enrichment device 20 by pipeline, and adsorption and enrichment is filled
Put 20 to be rinsed, the waste liquid after flushing is directly discharged from tapping valve；Open between elution device 17 and ion interchange unit 21
Communicating valve, the pure water in elution device 17 by pipeline inject ion interchange unit 21, ion interchange unit 21 is rushed
Wash, the waste liquid after flushing is directly discharged from tapping valve；
After the completion of flushing, the communicating valve closed between elution device 17 and ion interchange unit 21 opens alkali liquor chemical tank
Communicating valve between 19 and adsorption and enrichment device 20, the alkali liquor in alkali liquor chemical tank 19 is by alkaline-resisting pipeline to adsorption and enrichment device
Alkali liquor being injected in 20, desorbing being occurred in the presence of alkali liquor by the fulvic acid after resin absorption, the solution after desorbing flows through ion
Flow out after switch 21, be labeled as fulvic acid solution；
After fulvic acid solution is freeze-dried, gained solid is solid-state fulvic acid powder.
Wherein, adsorption and enrichment device 20 includes adsorption column and filler, and described filler is located in the adsorption column, described filler
For one or more in XAD-8 resins, DAX-8 resins and XAD-7 resins；Ion interchange unit 21 includes adsorption column and fills out
Material, in adsorption column, described filler is hydrogen type cation exchange resin to described filler.
Fulvic acid is extracted after terminating, and the pure water in elution device 18 is poured into by the valve closed between water tank 7 and filter
Water tank, starts concentration, concentrated water valve is reached maximum, washes away the cleaning for realizing NF membrane using pure water to film.NF membrane is forbidden
Stored dry, it is necessary to assure have water in putamina, if not using more than 70h for some reason, should be soaked in NF membrane in clean water, if
Long-term leaving unused must be sealed up for safekeeping by NF membrane requirement storage mode.
The double property dissolving humic acid extraction units of the hydrophilic-hydrophobic use filter membrane for disposable filter membrane, and filter membrane needs to be resistant to
By 0.4mol/L strong acid, filter membrane is stored on request and is used, but the siliceous filter membrane such as unusable glass fiber filter.
The present invention extracts the equipment of fulvic acid can be with restoration and reuse in the equipment of organic solvent extraction fulvic acid, major alterations
Resistance to organic dosing tank is transform as including by alkali liquor chemical tank, is resistance to organic pipeline by alkaline-resisting pipeline modification, filter membrane is transform as resistance to
Organic filter membrane, the device can carry out fulvic acid using methanol, ethanol, the volatile low pole of hexamethylene or non-polar organic solvent
Extract and purification.
A series of detailed description mentioned above is only for illustrating for the feasibility embodiment of the present invention,
They are not to limit the scope of the invention, in the ken that the technical field those of ordinary skill possesses
Interior, the various change made on the premise of without departing from present inventive concept belongs to protection scope of the present invention.
Claims (10)
1. a kind of equipment for extracting water body fulvic acid, including raw water feed unit, pretreatment unit, nanofiltration upgrading unit,
Acid-base value adjustment unit, water tank, general control system, filtration, purification unit and fulvic acid extraction unit；
The filtration, purification unit includes filter, liquid memory and vacuum pump, the entrance of the filter and the water tank
Outlet connection, the outlet of the filter is connected with the entrance of the liquid memory；The vacuum pump is stored up with the liquid
Storage connects；The outlet of the liquid memory is connected with the entrance of the adsorption and enrichment device；
The fulvic acid extraction unit includes elution device, alkali liquor chemical tank, adsorption and enrichment device and ion interchange unit, described
The outlet of the entrance of adsorption and enrichment device and the liquid memory, the outlet of elution device, the outlet of alkali liquor chemical tank are connected,
The outlet of adsorption and enrichment device is connected with the entrance of the ion interchange unit；
The entrance of the ion interchange unit is connected with the outlet of elution device, the adsorption and enrichment device, ion interchange unit
Bottom be equipped with tapping valve；
The adsorption and enrichment device includes adsorption column and filler, and in the adsorption column, described filler is XAD-8 to described filler
One or more of resin, DAX-8 resins and XAD-7 resins；
The ion interchange unit includes adsorption column and filler, and in the adsorption column, described filler is Hydrogen to described filler
Cation exchange resin.
2. it is used for as claimed in claim 1 extracting the equipment of water body fulvic acid, it is characterised in that the water tank adopts acidproof material
Material, which is provided with closure above, is provided with agitator, liquid level sensor and pH sensors in which；The end face of the closure is provided with
At least 5 through holes；Pipeline between the water tank and the filter gos deep in water tank, stretches at the top of the pipeline of water tank as sealing
Structure, duct wall are provided with the hole that multiple apertures are 50 μm, and the minimum altitude in hole is controlled at the 1/100-1/10 of tank height, institute
State and stretch into tank pipe and be externally provided with filter mantle, the aperture of the filter mantle is 100 μm.
3. it is used for as claimed in claim 1 extracting the equipment of water body fulvic acid, it is characterised in that the pretreatment unit includes
One-level precision microfiltration filter, two grades of accurate microfiltration filters and three-level precision microfiltration filter, one-level precision microfiltration filter
The aperture of middle precision Filter element is 1 μm, and in two grades of accurate microfiltration filters, the aperture of precision Filter element is 0.45 μm, three-level precision microfiltration
In filter, the aperture of precision Filter element is 0.22 μm；The entrance of one-level precision microfiltration filter is connected with the outlet of self priming pump
Connect, the outlet of one-level precision microfiltration filter is connected with the entrance of two grades of accurate microfiltration filters, two grades of accurate microfiltration filters
The entrance of outlet and three-level precision microfiltration filter be connected, the outlet of the accurate microfiltration filter of three-level is connected with water tank.
4. it is used for as claimed in claim 1 extracting the equipment of water body fulvic acid, it is characterised in that the nanofiltration concentration is single
Unit includes nano-filtration unit, high-pressure pump, TOC on-line monitorings probe and the 2nd TOC on-line monitoring probes；Wherein nano-filtration unit bag
NF membrane and rustless steel putamina is included, the aperture value of the NF membrane is 1-2nm；
The first TOC on-line monitorings probe is located at located at the nano-filtration unit concentrated water exit, the 2nd TOC on-line monitoring probes
At the wastewater outlet of nano-filtration unit.
5. it is used for as claimed in claim 4 extracting the equipment of water body fulvic acid, it is characterised in that the nano-filtration unit is provided with liquid
Import, concentrated water outlet and wastewater outlet；The liquid-inlet is connected with water tank by high-pressure pump, and the concentrated water outlet is connected with water tank
Connect, the waste water is discharged by pipeline；Security valve is provided between the nano-filtration unit and high-pressure pump, and concentrated water outlet is provided with security
Valve.
6. it is used for as claimed in claim 1 extracting the equipment of water body fulvic acid, it is characterised in that in the acid-base value adjustment unit
Including pH sensors, agitator, metering dosing pump, acid solution chemical tank；The pH sensors measure dosing pump in water tank
Entrance is connected with the outlet of acid solution chemical tank, and the outlet for measuring dosing pump is connected with water tank.
7. it is used for as claimed in claim 1 extracting the equipment of water body fulvic acid, it is characterised in that the filter includes impurity
Room, filter membrane and core, the filter membrane is in impurity room, and is supported by core；The aperture span of the filter membrane is
0.1-0.7μm。
8. it is used for as claimed in claim 1 extracting the equipment of water body fulvic acid, it is characterised in that the general control system includes control
Unit processed and touch screen device, described control unit are connected with touch screen device, and described control unit is passed with self priming pump, liquid level sensor, pH
Sensor, metering dosing pump, high-pressure pump and the connection of acid-base value adjustment unit；The pH sensors are provided with lifting platform.
9. utilize claim 1-8 arbitrary described for extracting the method that the equipment of water body fulvic acid carries out fulvic acid extraction, its
It is characterised by, which comprises the steps：
(1) open total control switch：Start the main power start button of general control system；
(2) treating nature water：Start self priming pump start button, self priming pump draws raw water, the filtration of self priming pump front end by pipeline
Bag is tentatively filtered to raw water, and the raw water after preliminary filtration is by the supercharging of self priming pump into the one-level essence in pretreatment unit
Close microfiltration filter is once filtered to raw water, and the raw water Jing after once filtering carries out two into two grades of accurate microfiltration filters
Secondary filtration；Raw water after secondary filter carries out three filtrations into three-level precision microfiltration filter, and the raw water after three filtrations is led to
Piping enters water tank；When the water level in water tank reaches 4/5 tank height, self priming pump quits work；
(3) nanofiltration concentration：Raw water Jing high-pressure pump supercharging in water tank enters into nanofiltration upgrading unit by pipeline, and NF membrane can be right
In raw water, Natural Dissolved Organic Matter is concentrated, and obtains waste water and concentrated water；Through the direct discharging of waste water of NF membrane, concentrated water circulation
When the content of the organic carbon determined into water tank, the dissolved organic carbon on-line determination device in positioned at water tank reaches preset value,
Stop concentration；
(4) acid-base value is adjusted：Start acid-base value adjustment unit, metering dosing pump receives pH sensor signals and starts acid solution addition journey
Sequence, extracts acid solution by pipeline from acid solution chemical tank and injects non-oxidizable acid solution in water tank by acid-resistant pipeline, while water tank
Middle stirring motor starts so that acid solution and concentrated water uniformly mix, and until reaching default pH value, measures dosing pump acid liquid program
Quit work；
(5) filter purification：The outlet valve of water tank is opened, while starting vacuum pump, is pressed by vacuum pump, the concentrated water in water tank
In by filter influent bin, sour insoluble impurity is removed by membrane retention, slightly carries fulvic acid solution by filter membrane
In influent bin；
(6) adsorption and enrichment：The outlet valve of water tank after the completion of filtration, is closed, the outlet valve of liquid memory, liquid storage is opened
Liquid in storage flows into adsorption and enrichment device, and fulvic acid is attracted on resin, and waste liquid is discharged from tapping valve；
(7) alkali liquor eluting：After the completion of absorption, the valve between elution device and adsorption and enrichment device is opened, while opening absorption
The tapping valve of enriching apparatus bottom, the pure water in elution device inject adsorption and enrichment device by pipeline, to adsorption and enrichment device
It is rinsed, the waste liquid after flushing is directly discharged from tapping valve；The communicating valve between elution device and ion interchange unit is opened,
Pure water in elution device injects ion interchange unit by pipeline, ion interchange unit is rinsed, the waste liquid after flushing
Directly discharge from tapping valve；
After the completion of flushing, the communicating valve closed between elution device and ion interchange unit opens alkali liquor chemical tank rich with absorption
Communicating valve between acquisition means, the alkali liquor in alkali liquor chemical tank inject alkali liquor, quilt by alkaline-resisting pipeline in adsorption and enrichment device
There is desorbing in the fulvic acid after resin absorption in the presence of alkali liquor, the solution after desorbing is flowed out after flowing through ion interchange unit,
It is labeled as fulvic acid solution；
After fulvic acid solution is freeze-dried, gained solid is solid-state fulvic acid powder.
10. in water body as claimed in claim 9 dissolve fulvic acid extracting method, it is characterised in that the acid-resistant pipeline will
Seek the non-oxidizing acid that can bear 10mol/L；The preset value of the pH is 0.5-3；The alkali liquor chemical tank requires to bear
The highly basic of 0.5mol/L.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610922048.7A CN106519259B (en) | 2016-10-21 | 2016-10-21 | A kind of equipment for extracting water body fulvic acid |
| PCT/CN2016/109465 WO2018072282A1 (en) | 2016-10-21 | 2016-12-12 | Apparatus for extracting fulvic acid in water body |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610922048.7A CN106519259B (en) | 2016-10-21 | 2016-10-21 | A kind of equipment for extracting water body fulvic acid |
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| CN106519259A true CN106519259A (en) | 2017-03-22 |
| CN106519259B CN106519259B (en) | 2018-03-09 |
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| CN201610922048.7A Expired - Fee Related CN106519259B (en) | 2016-10-21 | 2016-10-21 | A kind of equipment for extracting water body fulvic acid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113109126A (en) * | 2021-03-09 | 2021-07-13 | 中国环境科学研究院 | Phosphate oxygen isotope enrichment equipment, method and device |
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