CN106519259B - A kind of equipment for extracting water body fulvic acid - Google Patents
A kind of equipment for extracting water body fulvic acid Download PDFInfo
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- CN106519259B CN106519259B CN201610922048.7A CN201610922048A CN106519259B CN 106519259 B CN106519259 B CN 106519259B CN 201610922048 A CN201610922048 A CN 201610922048A CN 106519259 B CN106519259 B CN 106519259B
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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 a kind of equipment and preparation method for being used to extract water body fulvic acid, wherein, equipment for extracting water body fulvic acid includes 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, and the fulvic acid extraction unit includes elution device, alkali lye chemical tank, adsorption and enrichment device and ion interchange unit;Filtration, purification unit can separate fulvic acid with insoluble impurity, and fulvic acid can be adsorbed, purified by fulvic acid extraction unit, obtain high concentration fulvic acid extract solution.A kind of device structure for extracting water body fulvic acid of present invention offer is simple, automaticity is high, easy to operate.
Description
Technical field
The present invention relates to concentration technique field, more particularly to a kind of equipment for extracting water body fulvic acid.
Background technology
DOM is to be mixed by aperture span for a kind of natural macromolecular organic matter of 0.1-0.7 μm of filter membrane
Compound, it changes from animals and plants secretion and its Residue decay product, the Nomenclature Composition and Structure of Complexes with space-time and source.In fresh water
In Marine water, DOM has important ecology 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 degrades, is main in DOM
Composition, by extensive concern.Solvable under any pH value condition, migration is strong, fulvic acid and the heavy metal in water and poisonous and harmful
Material interacts, 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 concentration is generally 1-5mg/L in fresh water, and 0.1- is generally in seawater
1mg/L.But the problem of humic acid that high concentration is efficiently extracted from water body is urgent need to resolve how is realized at present.
Nanofiltration process is a kind of low-pressure driving membrane separating process of similar mechanical screening.Apparatus of the present invention utilize nanofiltration
Journey, realize and DOM in water body is dammed, monovalention is removed while nanofiltration concentrates (such as:Sodium ion and chlorine
Ion) and molecular weight be less than 200 dalton organic matter.Apparatus of the present invention are for fresh water or Marine water DOM
Nanofiltration concentration, purification.
Li Huijie has delivered a 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
Purify and depend primarily on what laboratory condition was completed with some simple equipment, this method is included in the extraction and richness of fulvic acid
Two steps of purifying of acid.
Detailed extraction purification flow 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, and one can not be formed during whole extraction completely and is operated
Convenient system;In addition, fulvic acid extracting method disclosed in this paper is influenceed greatly by manual operation, it is impossible to is widely used in fresh water
It is bad with the extraction and contrast of DOM fulvic acid in Marine water, exploitativeness.
The content of the invention
It is separated from the water fulvic acid in order to realize and it is extracted and purified, is used to extract the invention provides one kind
The equipment of water body fulvic acid, it effectively can easily extract required fulvic acid.
In order to solve the above-mentioned technical problem, a kind of equipment for extracting water body fulvic acid of the invention, including raw water supply
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 vavuum pump, the entrance of the filter with it is described
The outlet connection of water tank, the outlet of the filter is connected with the entrance of the liquid memory;The vavuum pump and the liquid
Body holder 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 lye 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 lye chemical tank
Connection, the outlet of adsorption and enrichment device is connected with the entrance of the ion interchange unit;
The outlet of the entrance and elution device of the ion interchange unit connects, 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, the filler is the filler
The 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, the filler is the filler
Hydrogen type cation exchange resin.
Preferably, it is preferable that the raw water feed unit uses self-priming water supplying pump, and raw water is seawater or fresh water, raw water water
The turbidity of matter is within 1000NTU, and TOC value is within 1000mg/l, and electrical conductivity value is within 40000 μ S/cm;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 uses acid resisting material, and it is provided with closure above;Agitator, level sensing are provided with it
Device and pH sensors;The end face of the closure is provided with least five through hole;Pipeline between the water tank and the filter is deep
Enter in water tank, it is sealing structure to stretch at the top of the pipeline of water tank, and 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 micro-filtration filter, two level precision micro-filtration filter, three-level essence
Close micro-filtration filter, the aperture of precision Filter element is 1 μm in one-level precision micro-filtration filter, accurate in two level precision micro-filtration filter
The aperture of filter core is 0.45 μm, and the aperture of precision Filter element is 0.22 μm in three-level precision micro-filtration filter;The one-level precision is micro-
The outlet for filtering the entrance and self priming pump of filter connects, outlet and the two level precision micro-filtration filter of one-level precision micro-filtration filter
Entrance connection, the outlet of two level precision micro-filtration filter is connected with the entrance of three-level precision micro-filtration filter, and three-level precision is micro-
The outlet of filtration filter is connected with water tank.
Preferably, one-level, two level, three-level precision Filter element use polypropylene filter core, and precision Filter element needs 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, the first TOC on-line monitorings probe and second
TOC on-line monitoring probes;Wherein nano-filtration unit includes NF membrane and stainless 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 passes through 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, 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;
The pH sensors are located in water tank, and the entrance for measuring dosing pump is connected 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
Control unit is stated 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, if necessary can rise to pH sensors outside water tank.
Using the method for dissolve fulvic acid extraction for extracting the equipment of water body fulvic acid, comprise the following steps:
(1) total control switch is opened:Start the general supply 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 filtering is pressurized enter in pretreatment unit one by self priming pump
The accurate micro-filtration filter of level is once filtered to raw water, and the raw water after once filtering is entered into two level precision micro-filtration filter
Row secondary filter;Raw water after secondary filter is filtered three times into three-level precision micro-filtration filter, the original after filtering three times
Water enters water tank by pipeline;When the water level in water tank reaches 4/5 tank height, self priming pump is stopped;
(3) nanofiltration concentrates:Raw water in water tank is pressurized through high-pressure pump enters nanofiltration upgrading unit, NF membrane by pipeline
Natural Dissolved Organic Matter in raw water can be concentrated, obtain waste water and concentrated water;By the direct discharging of waste water of NF membrane, concentrated water
Water tank is recycled into, when the content of the organic carbon of the dissolved organic carbon on-line determination device measure in water tank 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 added
Enter program, acid solution is extracted from acid solution chemical tank by pipeline and injects non-oxidizable acid solution into water tank by acid-resistant pipeline, simultaneously
Stirring motor starts in water tank so that acid solution and concentrated water uniformly mix, and until reaching default pH value, measure dosing pump acid liquid
Program stopped works;
(5) filtering purification:The outlet valve of water tank is opened, while starts vavuum pump, is pressed by vavuum pump, in water tank
Concentrated water is by the way that in filter influent holder, the insoluble impurity of acid is removed by membrane retention, slightly carries fulvic acid solution and passes through
In filter membrane influent holder;
(6) adsorption and enrichment:After the completion of filtering, the outlet valve of water tank is closed, opens the outlet valve of liquid memory, liquid
Liquid in body holder flows into adsorption and enrichment device, and fulvic acid is attracted on resin, and waste liquid is discharged from tapping valve;
(7) alkali lye elutes:After the completion of absorption, the valve between elution device and adsorption and enrichment device is opened, is opened simultaneously
The tapping valve of adsorption and enrichment bottom of device, the pure water in elution device injects 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 between closing elution device and ion interchange unit, alkali lye chemical tank is opened with inhaling
Communicating valve between attached enriching apparatus, the alkali lye in alkali lye chemical tank inject alkali by alkaline-resisting pipeline into adsorption and enrichment device
Liquid, desorbed by the fulvic acid after resin adsorption in the presence of alkali lye, after the solution after desorption flows through ion interchange unit
Outflow, 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
Provided with flow speed control valve, the wastewater flow rate of NF membrane discharge is 1 with the ratio of the concentrated water amount of discharge:9-9:1, preferably 2:1-1:2.
Preferably, the degree of the acid-resistant pipeline can bear 10mol/L non-oxidizing acid;The preset value of the pH is 0.5-
3;The alkali lye chemical tank and alkaline-resisting requirements for pipes can bear 0.5mol/L highly basic.
Preferably, the front end of the high-pressure pump is provided with pressure gauge and safety valve, in raw water concentration process, before the high-pressure pump
When pressure is more than preset value, the safety valve is opened, and avoids high-pressure pump damage and pipeline burst phenomenon.
Preferably, NF membrane can not dry-storage, it is necessary to assure has water in putamina, if equipment is left unused for some reason exceedes 70h, answers
NF membrane is soaked in clean water, if long-term leave unused must be sealed up for safekeeping by NF membrane requirement storage mode.
Preferably, general control system uses low-voltage distribution, and the voltage class of power supplying and distributing equipment is 220VAC, and sets low pressure and match somebody with somebody
Electric cabinet, powered to process system power-equipment;Power switch in control system is protected with electrical control cubicles gate interlock, can be reached anti-
Dirt, rapid heat dissipation and the effect being easily installed.
Preferably, the front end of the self priming pump is provided with safety valve, is provided with liquid level sensor in the water tank, its water level is in water
During 4/5 water tank volume of case, the safety valve is opened, and self priming pump shuts down, and avoids cistern water level too high.
Compared with prior art the beneficial effect comprise that:
(1) a kind of device structure for extracting water body fulvic acid of present invention offer is simple, automaticity is high, operation side
Just, easily and effectively the other impurity of fulvic acid can be separated, extracts 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 level precision Filter element aperture is 0.45 μm, and three-level is accurate
Filter core aperture is 0.22 μm, has more effectively filtered out the impurity such as suspension of larger particles in water, it is miscellaneous preferably to avoid particle
Thing scratches to caused by film, blocks and impacting with high pressure, reduces the replacement frequency of precision Filter element;
(3) whole process of acid-base value adjustment unit regulation pH value is full automatic, saves labour, reduces production
Cost, the accuracy rate of the pH value of modulation are higher;
(4) ratio of the pure water amount discharged in nanofiltration upgrading unit in nano-filtration unit and the concentrated water amount of discharge is 2:1-1:2,
And then pure water discharge can be avoided excessive or it is too small to caused by film injury or device efficiency reduce.
Brief description of the drawings
Fig. 1 is a kind of apparatus and process flow chart for being used to extract water body fulvic acid of the present invention;
Fig. 2 is fulvic acid extraction purification flow chart in background technology.
Embodiment
Below in conjunction with the accompanying drawings, the embodiment of the present invention is described in detail.
Join shown in Fig. 1, Fig. 1 is the process chart that the present invention is used to extract the equipment of water body fulvic acid.The present invention provides
The equipment for extracting water body fulvic acid, including raw water feed unit, pretreatment unit, nanofiltration upgrading unit, acid-base value adjust
Save unit, water tank 7, general control system 4, filtration, purification unit and fulvic acid extraction unit;Wherein raw water feed unit mainly wraps
Include self priming pump 1;Pretreatment unit includes one-level precision micro-filtration filter 2, two level precision micro-filtration filter 3 and three-level precision micro-filtration
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
Member 9 includes NF membrane and stainless steel putamina;Acid-base value adjustment unit includes PH sensor, metering dosing pump 5, acid solution chemical tank 6;
Filtration, purification unit includes liquid memory 16, filter, vavuum pump 15, and wherein filter includes impurity room 12, the and of filter membrane 13
Core 14, filter membrane 13 are located in impurity room 12, and supported by core 14;Fulvic acid extraction unit includes elution device 17, alkali lye
Chemical tank 19, adsorption and enrichment device 20, ion interchange unit 21;General control system 4 is mainly controlled using electrical equipment, therein
Collection control operation is unified in switch board to be carried out, and can realize whole system and automatically control operation and manually operated.
Wherein, the entrance of one-level precision micro-filtration filter 2 is connected with the outlet of self priming pump 1, one-level precision micro-filtration filter 2
Outlet be connected with the entrance of two level precision micro-filtration filter 3, the outlet of two level precision micro-filtration filter 3 and three-level precision are micro-
The entrance connection of filter 18 is filtered, the outlet of three-level precision micro-filtration filter 18 is connected with water tank 7;PH sensors are located at water tank 7
In, the entrance of metering dosing pump 5 is connected with the outlet of acid solution chemical tank 6, and the outlet of metering 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 by high-pressure pump 8 with water tank 7, 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 vavuum 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, the outlet of alkali lye chemical tank 19 of the entrance of adsorption and enrichment device 20 also with elution device 17 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;Bottom, the bottom of ion interchange unit 21 of adsorption and enrichment device 20 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 vavuum pump 15 connect.
Equipment provided by the present invention for extracting water body fulvic acid, its water body water source is seawater or fresh water, the water of raw water
Matter requires turbidity within 1000NTU, and TOC value is within 1000mg/L, and electrical conductivity value is within 40000 μ S/cm;From
The front end of sucking pump is provided with filter bag, and the aperture of filter bag is 10 μm.
General control system uses low-voltage distribution, and the voltage class of power supplying and distributing equipment is 220VAC, and sets low-voltage distribution cabinet, to
Process system power-equipment is powered.In addition, the switch board of independent operation is equipped with control system, and electric switch and electric member
Part is all concentrated in switch board, and power switch is protected with electrical control cubicles gate interlock, can be reached dust-proof, rapid heat dissipation and is easily installed
Effect.
General supply and start button are first turned on, makes whole system in running order, self priming pump 1 is drawn former by pipeline
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, by preliminary filtering
The one-level precision micro-filtration filter 2 that is entered by the supercharging of self priming pump in pretreatment unit of raw water once mistake is carried out to raw water
Filter, the raw water after once filtering carry out secondary filtering into two level precision micro-filtration filter 3, the raw water after secondary filter
Into three-level precision micro-filtration filter 18, wherein, the filter core aperture in one-level precision micro-filtration filter 2 is 1 μm, and two level precision is micro-
It is 0.45 μm to filter the filter core aperture in filter 3, and the filter core aperture in three-level precision micro-filtration filter 18 is 0.22 μm, such a filter
Core diameter, which is set, can preferably filter out the impurity such as suspension of larger particles in water, increase water quality, more effectively avoid particle
Thing impurity scratches to caused by film, blocks and impacting with high pressure.In addition, precision Filter element needs to change in time, avoid blocking and excessive
Pollutant gathers cooperating microorganisms.
Raw water after the filtering of three-level precise filtering device enters water tank 7 by connecting pipe, the liquid level biography in water tank 7
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, it is stopped, that is, stops
The water filling into water tank.
The water tank uses acid resisting material, and it is provided with closure above, is provided with agitator and pH sensors in it;It is described close
The end face of capping is provided with least five through hole.
The NF membrane that raw water in water tank 7 enters in nano-filtration unit 9 by the pressurization of high-pressure pump 8, NF membrane can by fresh water or
Marine water is separated into concentrated water and waste water, and the waste water of the saliferous and small molecule organic matter that can pass through NF membrane is expelled directly out, and is being received
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, its speed adjustable range is
0-200L/h;Concentrated water through nanofiltration UF membrane is back in water tank 7 by pipeline, in nano-filtration unit 9 and the connecting pipe of water tank 7
Provided with flow speed control valve, the speed that concentrated stream goes out NF membrane can be adjusted, its speed adjustable range is 0-200L/h;Waste water stream goes out nanofiltration
The speed value that the speed and concentrated stream of film go out NF membrane is arranged in appropriate scope, makes wastewater flow rate and row that NF membrane is discharged
The ratio of the concentrated water amount gone out is 1:9-9:1, so can avoid because waste water outflow excessive velocities or excessively slowly to NF membrane caused by
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 fewer,
The concentration more and more higher of the content of organic matter, when the organic carbon content of the dissolved organic carbon on-line determination device measure in water tank reaches
During preset value, stop concentration, close concentration systems.
During raw water concentrates, avoid that cocnentration factor is too high, and cocnentration factor is higher as far as possible, concentration containing organic matter is higher, mistake
High concentration can damage to NF membrane, therefore, by content of organic matter control in concentrated water in below 10000mg/L.
The waste outflow pipe of nano-filtration unit 9 is provided with the 2nd TOC on-line monitorings probe 11, nano-filtration unit concentrated water discharge line
Place is provided with the first TOC on-line monitorings probe 10, is visited by contrasting the first TOC on-line monitorings probe 10 and the 2nd TOC on-line monitorings
It is first 11 detection numerical value, it is possible to determine that NF membrane whether seepage;I.e. if the first TOC on-line monitorings probe 10 and the 2nd TOC exist
The numerical difference of the detection of line monitoring probe 10 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 is less than the 1/5 of water tank, security valve is opened
Open, high-pressure pump 8 shuts down, it is possible thereby to avoid high-pressure pump causes high-pressure pump to burn phenomenon 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, and can avoid high-pressure pump damage and pipeline
Decrepitation Phenomena.
After raw water concentration terminates, start acid-base value adjustment unit.Required pH value is set in general control system 4, and it sets
Fixed pH value is 0.5-3, and pH value signal is passed to metering dosing pump 5 by pH sensors, and metering dosing pump startup acid solution adds journey
Sequence, extract acid solution from acid solution chemical tank 6 and inject non-oxidizable acid solution, while stirring in water tank 7 into water tank by acid-resistant pipeline
Mix motor starting so that acid solution and concentrated water uniformly mix, and carry out pH value regulation, until pH value reaches the value pre-set, metering
Dosing pump acid liquid program stopped works, and measures dosing pump and water tank stirring motor is stopped, solution left standstill 4-24h.
If containing excessive ash content in extracted fulvic acid, non-oxidizable acid solution regulation is being added to the pH pre-set
After value, dense hydrofluoric acid is added, making hydrofluoric acid concentration, then solution left standstill 4-24h, solid so as to reduce between 0.1-0.5mol/L
State fulvic acid ash content.
The process of whole pH value regulation is full automatic, saves labour, reduces production cost, and the pH modulated
The accuracy of value is higher, and the efficiency of process for preparation is also higher.During pH regulations, 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, local pH value can be avoided higher or relatively low.
Water tank 7 uses acid resisting material, and it is provided with closure above, and the end face of closure is provided with least five through hole;Lower end
Preferably funnel shaped, be advantageous to the output of concentrated water;Agitator and pH sensors are provided with it;PH sensors are provided with lifting platform,
After the completion of pH value regulation, lifting platform can rise to pH sensors on the water surface.
Pipeline between water tank and filter gos deep into water tank, is sealing structure at the top of pipeline, duct wall is provided with multiple holes
Footpath is 50 μm of hole, and the minimum altitude in hole is controlled at the 1/100-1/10 of tank height, and the tank pipe that stretches into is externally provided with
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 starts vavuum pump 15, is pressed by vavuum pump 15, the concentrated water in water tank 7 is led to
Cross in solution strainer influent holder 16, the insoluble impurity of acid is retained and removed by filter membrane 13, slightly carries fulvic acid solution and leads to
In filter membrane influent holder 16.
After the completion of filtering, the outlet valve of water tank is closed, opens the outlet valve of liquid memory, 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 open adsorption and enrichment
The tapping valve of the bottom of device 20, the pure water in elution device 17 inject adsorption and enrichment device 20 by pipeline, adsorption and enrichment are 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 injects ion interchange unit 21 by pipeline, ion interchange unit 21 rushed
Wash, the waste liquid after flushing is directly discharged from tapping valve;
After the completion of flushing, the communicating valve between closing elution device 17 and ion interchange unit 21, alkali lye chemical tank is opened
Communicating valve between 19 and adsorption and enrichment device 20, alkali lye in alkali lye chemical tank 19 is by alkaline-resisting pipeline to adsorption and enrichment device
Alkali lye is injected in 20, is desorbed by the fulvic acid after resin adsorption in the presence of alkali lye, the solution after desorption flows through ion
Flowed out after switch 21, 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 the filler is in the adsorption column, the filler
For the one or more in XAD-8 resins, DAX-8 resins and XAD-7 resins;Ion interchange unit 21 includes adsorption column and filled out
Material, for the filler in adsorption column, the filler is hydrogen type cation exchange resin.
After fulvic acid extraction terminates, the valve between closing water tank 7 and filter, the pure water in elution device 18 is poured into
Water tank, start concentration, concentrated water valve is reached into maximum, the cleaning of NF membrane is realized to washing away for film using pure water.NF membrane is forbidden
Stored dry, it is necessary to assure have water in putamina, if for some reason more than 70h without using, NF membrane should be soaked in clean water, if
Long-term leave unused must be sealed up for safekeeping by NF membrane requirement storage mode.
It is disposable filter membrane that the double property of the hydrophilic-hydrophobic, which dissolve humic acid extraction unit using filter membrane, and filter membrane needs to be resistant to
By 0.4mol/L strong acid, filter membrane is stored and used on request, but the siliceous filter membrane such as unusable glass fiber filter.
The equipment that the equipment of present invention extraction fulvic acid can extract fulvic acid with restoration and reuse in organic solvent, major alterations
Including transforming alkali lye chemical tank as resistance to organic dosing tank, it 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
Extraction and purifying.
A series of detailed description described above illustrates only for the feasibility embodiment of the present invention,
They are not to limit the scope of the invention, in the technical field those of ordinary skill possessed knowledge
Interior, the various change made on the premise of present inventive concept is not departed from 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 entrance of the pretreatment unit is connected with the raw water feed unit, the outlet of pretreatment unit and entering for the water tank
Mouth connection;The entrance of the filtration, purification unit is connected with the outlet of the water tank, the outlet of filtration, purification unit and the richness
In the connection of sour extraction unit;The water tank is also connected with the acid-base value adjustment unit and nanofiltration upgrading unit;The master control
System is connected with the raw water feed unit, acid-base value adjustment unit, nanofiltration upgrading unit.
The filtration, purification unit includes filter, liquid memory and vavuum 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 vavuum pump stores 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 lye chemical tank, adsorption and enrichment device and ion interchange unit, described
The entrance of adsorption and enrichment device is connected with the outlet of the liquid memory, the outlet of elution device, the outlet of alkali lye chemical tank,
The outlet of adsorption and enrichment device is connected with the entrance of the ion interchange unit;
The outlet of the entrance and elution device of the ion interchange unit connects, 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 for the filler in the adsorption column, the filler is XAD-8
The one or more of resin, DAX-8 resins and XAD-7 resins;
The ion interchange unit includes adsorption column and filler, and for the filler in the adsorption column, the filler is Hydrogen
Cationic ion-exchange resin.
2. the equipment as claimed in claim 1 for being used to extract water body fulvic acid, it is characterised in that the water tank uses acidproof material
Material, it is provided with closure above, is provided with agitator, liquid level sensor and pH sensors in it;The end face of the closure is provided with
At least five through hole;Pipeline between the water tank and the filter gos deep into 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. the equipment as claimed in claim 2 for being used to extract water body fulvic acid, it is characterised in that the raw water feed unit bag
Self priming pump is included, for extracting raw water;The pretreatment unit includes one-level precision micro-filtration filter, two level precision micro-filtration filter
With three-level precision micro-filtration filter, the aperture of precision Filter element is 1 μm in one-level precision micro-filtration filter, the filtering of two level precision micro-filtration
The aperture of precision Filter element is 0.45 μm in device, and the aperture of precision Filter element is 0.22 μm in three-level precision micro-filtration filter;Described one
The entrance of the accurate micro-filtration filter of level is connected with the outlet of the self priming pump, outlet and the two level essence of one-level precision micro-filtration filter
The entrance connection of close micro-filtration filter, the outlet of two level precision micro-filtration filter connects with the entrance of three-level precision micro-filtration filter
Connect, the outlet of three-level precision micro-filtration filter is connected with water tank.
4. the equipment as claimed in claim 3 for being used to extract water body fulvic acid, it is characterised in that the nanofiltration concentration
Unit includes nano-filtration unit, high-pressure pump, the first TOC on-line monitorings probe and the 2nd TOC on-line monitoring probes;Wherein nano-filtration unit
Including NF membrane and stainless steel putamina, the aperture value of the NF membrane is 1-2 nm;
The first TOC on-line monitorings probe is located at the nano-filtration unit concentrated water exit, and the 2nd TOC on-line monitoring probes are located at
At the wastewater outlet of nano-filtration unit.
5. it is used for the equipment for extracting water body fulvic acid as claimed in claim 4, 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 by high-pressure pump with water tank, and the concentrated water outlet connects with water tank
Connect, the waste water is discharged by pipeline;Security valve is provided between the nano-filtration unit and high-pressure pump, concentrated water outlet is provided with security
Valve.
6. it is used for the equipment for extracting water body fulvic acid as claimed in claim 5, 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 are located in water tank, measure dosing pump
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 the equipment for extracting water body fulvic acid as claimed in claim 1, it is characterised in that the filter includes impurity
Room, filter membrane and core, the filter membrane are supported in impurity room by core;The aperture span of the filter membrane is
0.1-0.7 μm。
8. it is used for the equipment for extracting water body fulvic acid as claimed in claim 6, it is characterised in that the general control system includes control
Unit and touch screen device processed, described control unit are connected with touch screen device, and described control unit passes with self priming pump, liquid level sensor, pH
Sensor, metering dosing pump, high-pressure pump connect with acid-base value adjustment unit;The pH sensors are provided with lifting platform.
9. the method for carrying out fulvic acid extraction using any equipment for extracting water body fulvic acid of claim 1-8, its
It is characterised by, it comprises the following steps:
(1) total control switch is opened:Start the general supply start button of general control system;
(2) treating nature water:Start self priming pump start button, self priming pump draws raw water, the filtering of self priming pump front end by pipeline
Bag is tentatively filtered to raw water, the one-level essence that the raw water after preliminary filtering is entered in pretreatment unit by the supercharging of self priming pump
Close micro-filtration filter is once filtered to raw water, and the raw water after once filtering enters two level precision micro-filtration filter and carries out two
Secondary filtering;Raw water after secondary filter is filtered three times into three-level precision micro-filtration filter, and the raw water after filtering three times is led to
Piping enters water tank;When the water level in water tank reaches 4/5 tank height, self priming pump is stopped;
(3) nanofiltration concentrates:Raw water in water tank is pressurized through high-pressure pump enters nanofiltration upgrading unit by pipeline, and NF membrane can be right
Natural Dissolved Organic Matter is concentrated in raw water, obtains waste water and concentrated water;By the direct discharging of waste water of NF membrane, concentrated water circulation
Into water tank, when the content of the organic carbon of the dissolved organic carbon on-line determination device measure in 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, acid solution is extracted from acid solution chemical tank by pipeline and injects non-oxidizable acid solution, while water tank into water tank by acid-resistant pipeline
Middle stirring motor starts so that acid solution and concentrated water uniformly mix, and until reaching default pH value, measure dosing pump acid liquid program
It is stopped;
(5) filtering purification:The outlet valve of water tank is opened, while starts vavuum pump, is pressed by vavuum pump, the concentrated water in water tank
By the way that in filter influent holder, the insoluble impurity of acid is removed by membrane retention, slightly carries fulvic acid solution and passes through filter membrane
In influent holder;
(6) adsorption and enrichment:After the completion of filtering, the outlet valve of water tank is closed, opens the outlet valve of liquid memory, liquid storage
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 lye elutes:After the completion of absorption, the valve between elution device and adsorption and enrichment device is opened, while open absorption
The tapping valve of enriching apparatus bottom, the pure water in elution device injects 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 discharged from tapping valve;
After the completion of flushing, the communicating valve between closing elution device and ion interchange unit, it is rich with absorption to open alkali lye chemical tank
Communicating valve between acquisition means, the alkali lye in alkali lye chemical tank inject alkali lye, quilt into adsorption and enrichment device by alkaline-resisting pipeline
Fulvic acid after resin adsorption desorbs in the presence of alkali lye, and the solution after desorption flows out after flowing through ion interchange unit,
Labeled as fulvic acid solution;
After fulvic acid solution is freeze-dried, gained solid is solid-state fulvic acid powder.
10. fulvic acid extracting method is dissolved in water body as claimed in claim 9, it is characterised in that the acid-resistant pipeline is wanted
10mol/L non-oxidizing acid can be born by asking;The preset value of the pH is 0.5-3;The alkali lye chemical tank requirement can be born
0.5mol/L highly basic.
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PCT/CN2016/109465 WO2018072282A1 (en) | 2016-10-21 | 2016-12-12 | Apparatus for extracting fulvic acid in water body |
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