Soil hydrophobic fulvic acid component extraction purification device
Technical field
Field, more particularly to soil hydrophobic fulvic acid component extraction purification device are extracted the present invention relates to fulvic acid.
Background technology
Fulvic acid is the acid natural organic substance of a class polydispersion, and typically in brown or brown color, it is distributed widely in
The surrounding mediums such as soil, water body and bed mud, are one of main components of humus.Fulvic acid contains a large amount of phenolic hydroxyl groups, carbonyl etc.,
Not only it had been dissolved in acid but also had been dissolved in alkali, can have been interacted with metal ion and organic pollution, so that influence pollutant chemistry to degrade,
Photocatalytic degradation, bio-absorbable, migration and vaporization behaviors.Fulvic acid can also improve soil hardening, influence soil fertility.Hydrophobic is rich
In acid be easier to be interacted with organic agricultural chemicals and persistent pollutant, be currently agronomy, learn and environmental science is common
The emphasis and focus of concern.Because hydrophobic fulvic acid content is low, difficulty is extracted greatly, the enrichment and separation of hydrophobic fulvic acid in soil
It is the bottleneck of fulvic acid research.
Chinese invention patent (201510586221.6:A kind of Soil fulvic acid subfraction fractional extraction method) disclose one
Soil fulvic acid subfraction fractional extraction method is planted, it comprises the following steps:
1. a kind of Soil fulvic acid subfraction fractional extraction method, it is characterised in that the extracting method includes following step
Suddenly:
Step a:Pedotheque is pre-processed:Natural soil is weighed, tree root and stone is rejected, air-dried, sieving of milling obtains pre-
Treatment pedotheque;
Step b:The fractional extraction of the soil organism:
To deionized water is added in the pretreatment pedotheque in step a, make its solid-to-liquid ratio between 1:10~3:Between 10,
2~5h is continuously stirred, after standing 20~28h, centrifugation obtains supernatant 1 and pedotheque 1;
To deionized water is added in pedotheque 1, make its solid-to-liquid ratio between 1:10~3:Between 10,2~5h is continuously stirred,
After standing 20~28h, centrifugation obtains supernatant 2 and pedotheque 2;
To deionized water is added in pedotheque 2, make its solid-to-liquid ratio between 1:5~3:Between 10, with hydrochloric acid and hydroxide
Sodium adjusts pH value of solution between 1.0~3.0, continuously adds the hydrochloric acid solution of 0.1~1.0mol/L, makes its solid-to-liquid ratio between 1:
10~3:Between 10, solution is then continuously stirred into 2~5h, after standing 20~28h, centrifugation obtains supernatant 3 and soil
Sample 3;
To the hydrochloric acid solution that 0.1~1.0mol/L is added in pedotheque 3, make its solid-to-liquid ratio between 1:10~3:10 it
Between, solution is then continuously stirred into 2~5h, after standing 20~28h, centrifugation obtains supernatant 4 and pedotheque 4;
To deionized water is added in pedotheque 4, make its solid-to-liquid ratio between 1:5~1:Between 3, with hydrochloric acid and NaOH
Its pH value is adjusted between 6.0~8.0, under nitrogen protection, to sodium pyrophosphate solution is added in solution, its solid-to-liquid ratio is situated between
In 1:10~3:Between 10 and sodium pyrophosphate concentration is between 0.1~0.2mol/L, solution is then continuously stirred into 2~5h,
After standing 20~28h, centrifugation obtains supernatant 5 and pedotheque 5;
Under nitrogen protection, to sodium pyrophosphate solution is added in pedotheque 5, its solid-to-liquid ratio is made between 1:10~3:10 it
Between and sodium pyrophosphate concentration between 0.1~0.2mol/L, solution is then continuously stirred into 2~5h, after standing 20~28h,
Centrifugation, obtains supernatant 6 and pedotheque 6;
Under nitrogen protection, to sodium pyrophosphate solution is added in pedotheque 6, its solid-to-liquid ratio is made between 1:10~3:10 it
Between and sodium pyrophosphate concentration between 0.1~0.2mol/L, solution is then continuously stirred into 2~5h, stand 20~28h
Afterwards, centrifugation, obtains supernatant 7 and pedotheque 7;
To deionized water is added in pedotheque 7, make its solid-to-liquid ratio between 1:5~3:Between 10, with hydrochloric acid and hydroxide
Sodium adjusts its pH between 6.0~8.0, under nitrogen protection, to sodium hydroxide solution is added in solution, its solid-to-liquid ratio is situated between
In 1:10~3:Between 10 and naoh concentration is between 0.1~0.3mol/L, solution is then continuously stirred into 2~5h,
After standing 20~28h, centrifugation obtains supernatant 8 and pedotheque 8;
Under nitrogen protection, to sodium hydroxide solution is added in pedotheque 8, its solid-to-liquid ratio is made between 1:10~3:10 it
Between and naoh concentration between 0.1~0.3mol/L, solution is then continuously stirred into 2~5h, after standing 20~28h,
Centrifugation, obtains supernatant 9 and pedotheque 9;
Under nitrogen protection, to sodium hydroxide solution is added in pedotheque 9, its solid-to-liquid ratio is made between 1:10~3:10 it
Between and naoh concentration between 0.1~0.3mol/L, solution is then continuously stirred into 2~5h, after standing 20~28h,
Centrifugation, obtains supernatant 10 and pedotheque 10;
Step c:It is prepared by classification fulvic acid subfraction crude product:By the 1~supernatant of supernatant 10 in step b, altogether 10 parts
Supernatant is adjusted to pH value between 1.0~2.0 respectively, then stirs 2~5h respectively, and 20~28h, centrifugation point are stood respectively
From being respectively labeled as slightly carrying fulvic acid subfraction solution 1~slightly carry fulvic acid subfraction solution 10 by 10 portions of supernatants;
Step d:The crude product concentration of classification fulvic acid subfraction:Thick in step c is carried into fulvic acid subfraction solution 1~slightly carry
Fulvic acid subfraction solution 10, altogether 10 parts thick to carry fulvic acid subfraction solution logical with 10~20 times of flow velocitys of column volume/h respectively
Cross XAD-8 resin columns;
After the completion of absorption, washed with 0.4~0.8 times of deionization of column volume with 10~20 times of flow velocitys of column volume/h respectively
XAD-8 resin columns are washed, then with 3~5 times of flow velocitys of column volume/h successively with 0.5~3 times of 0.1~1.0mol/L hydrogen of column volume
Sodium hydroxide solution and 1~3 times of column volume deionized water washing XAD-8 resin columns, efflux be acidified to immediately pH value between 1.0~
Between 3.0, finally give and slightly carry 10 parts of corresponding acidifying solutions of fulvic acid subfraction with 10 parts;
Step e:The purifying of fulvic acid subfraction sample:10 parts of acidifying solutions described above are separately added into hydrofluoric acid, are made every
Hydrofluoric acid concentration in part acidifying solution by 12~48h of solution left standstill, is then respectively labeled as molten without silicon when being 0.1~0.3mol/L
Liquid 1~without silicon solution 10,10 parts without silicon solution altogether;
XAD-8 resin columns are passed through with 3~5 times of column volumes/h flow velocitys respectively without silicon solution by above-mentioned 10 parts;
After the completion of absorption, washed with 0.4~0.8 times of column volume deionized water with 10~20 times of flow velocitys of column volume/h respectively
XAD-8 resin columns, discard efflux, then with 3~5 times of flow velocitys of column volume/h successively with 0.5~3 times of column volume 0.1~
0.3mol/L sodium hydroxide solutions and 1~3 times of column volume deionized water washing XAD-8 resin column, efflux are full by hydrogen ion
The hydrogen type cation exchange resin of sum, efflux is respectively labeled as fulvic acid 1~fulvic acid of subfraction subfraction 10;
Fulvic acid 1~fulvic acid of subfraction subfraction 10 is distinguished into freeze-drying, 10 parts of solid fulvic acid is finally given sub-
Component is classified sample.
Soil fulvic acid extracting method disclosed in foregoing invention, depends primarily on laboratory method by the richness in soil
Sour subfraction is progressively extracted, and prepares the fulvic acid subfraction classification sample of different stage;The method depends on laboratory and big
The artificial operation of amount, operating process is complicated, automaticity is low;In addition, fulvic acid extracting method is received disclosed in patent of the present invention
Manual operation influence is larger, it is impossible to realize the extraction and contrast of a large amount of fulvic acid, exploitativeness is not good.
The content of the invention
In order to effectively extract and the Soil fulvic acid full constituent of high concentration is obtained, the invention provides soil hydrophobic fulvic acid
Component extraction purification device, it is possible to achieve efficient to extract soil hydrophobic fulvic acid, easy to operate, high degree of automation.
In order to solve the above technical problems, the invention provides a kind of soil hydrophobic fulvic acid component extraction purification device, bag
Include reactor, pH adjustment units, the first filtration, purification unit, acidifying case, acid-base value adjustment unit, the second filtration, purification unit,
Liquid memory, fulvic acid extraction unit and general control system;
The entrance of the reactor is connected with the outlet of the pH adjustment units, and the outlet of reactor and described first is filtered
The entrance connection of clean unit;
The outlet of the first filtration, purification unit with it is described acidifying case entrance be connected, it is described be acidified case outlet and institute
State the entrance connection of the second filtration, purification unit, the outlet of the second filtration, purification unit and the entrance of the liquid memory
Connection;
The outlet of the liquid memory is connected with the entrance of the fulvic acid extraction unit;
The pH adjustment units, acid-base value adjustment unit are connected with general control system control.
Preferably, the fulvic acid extraction unit includes elution device, the second chemicals dosing plant, adsorption and enrichment device and ion
Switch;The outlet of the elution device, the outlet of the second chemicals dosing plant connect with the entrance of the adsorption and enrichment device respectively
Connect, the outlet of the adsorption and enrichment device is connected with the entrance of the ion interchange unit, the entrance of the ion interchange unit
Outlet also with the elution device is connected;
The bottom of the adsorption and enrichment device, the bottom of ion interchange unit are equipped with waste liquid dump valve.
Preferably, the adsorption and enrichment device includes adsorption column and filler, and described filler is described in the adsorption column
Filler is one or more of XAD-8 resins, DAX-8 resins and XAD-7 resins;The ion interchange unit include adsorption column and
Filler, in the adsorption column, described filler is hydrogen type cation exchange resin to described filler.
Preferably, the fulvic acid extraction unit include elution device, the second chemicals dosing plant, primary adsorption enriching apparatus,
First ion interchange unit, secondary absorption enriching apparatus, the second ion interchange unit;The entrance of the primary adsorption enriching apparatus
Outlet with the liquid memory is connected, primary adsorption enriching apparatus outlet respectively with first ion interchange unit
The entrance connection of entrance, secondary absorption enriching apparatus;The outlet of the secondary absorption enriching apparatus and second ion exchange
The entrance connection of device;The outlet of elution device entrance, the friendship of the first ion respectively with the primary adsorption enriching apparatus
The entrance of changing device, the entrance of secondary absorption enriching apparatus, the entrance connection of the second ion interchange unit;The second dosing dress
The outlet entrance respectively with the primary adsorption enriching apparatus put, the entrance of secondary absorption enriching apparatus are connected;
The bottom of the primary adsorption enriching apparatus, the bottom of the first ion interchange unit, secondary absorption enriching apparatus
Bottom, the bottom of the second ion interchange unit are equipped with waste liquid dump valve.
Preferably, the primary adsorption enriching apparatus include adsorption column and filler, and described filler is located in the adsorption column,
Described filler is one or more of XAD-8 resins, DAX-8 resins and XAD-7 resins;
The secondary absorption enriching apparatus include adsorption column and filler, and described filler is described to fill out in the adsorption column
Expect to be XAD-4 resins.
Preferably, first ion interchange unit and the second ion interchange unit include adsorption column and filler, described
In the adsorption column, described filler is hydrogen type cation exchange resin to filler.
Preferably, soil storage room is provided with the reactor, the soil storage room is supported and positioned at reaction by support
In kettle;The outer wall of the soil storage room is provided with hole of multiple apertures less than 1mm.
Preferably, the pH adjustment units include the first metering dosing pump and the first chemicals dosing plant, the first metering dosing pump
Between first chemicals dosing plant and the reactor, the entrance of the first metering dosing pump is filled with first dosing
The outlet connection put, the outlet of the first metering dosing pump is connected with the entrance of the reactor.
Preferably, the first filtration, purification unit includes the first filter and vavuum pump;First filter enters
Mouth is connected by pipeline with the outlet of the reactor, and the outlet of first filter is connected with the entrance of the acidifying case;
The vavuum pump is connected with the acidifying case;
Pipeline between the reactor and first filter stretches into reactor, and the pipeline for stretching into reactor is high
Degree value is the 1/20-1/10 of reactor height, and it is externally provided with protective cover, and the protective cover is provided with multiple apertures for 1mm
Hole, the impurity in soil can be avoided to be flowed into reactor;
Pipeline between first filter and the acidifying case is stretched into acidifying case, the pipeline for stretching into acidifying case
On liquid level in the acidifying case;The air entry of the vavuum pump is on liquid level in the acidifying case.
Preferably, the acidifying case uses acid-fast alkali-proof material, and it is provided with closure above, and lower end is funnel shaped, institute
The end face for stating closure is provided with least 5 through holes.
Preferably, the first filtration, purification unit includes the first filter and vavuum pump, and first filter includes
Sample room, filter membrane and core, the filter membrane are supported in the sample room by the core;The aperture of the filter membrane takes
Value scope is 0.1-0.7 μm.
Preferably, the acid-base value adjustment unit includes pH sensors, agitator, the first acid solution chemical tank, the second acid solution
Chemical tank and the second metering dosing pump;The pH sensors and agitator are in the acidifying case;The first acid solution medicament
Case and the second acid solution chemical tank are arranged in juxtaposition;The entrance of the second metering dosing pump goes out with the first acid solution chemical tank respectively
The outlet connection of mouth, the second acid solution chemical tank, the outlet of the second metering dosing pump is connected with the entrance of the acidifying case.
Preferably, the second filtration, purification unit includes the second filter and vavuum pump, and second filter enters
Mouth is connected with the outlet of the acidifying case, and the outlet of second filter is connected with the entrance of the liquid memory;It is described
The outlet of liquid memory is connected with the entrance of the adsorption and enrichment device;The air entry of the vavuum pump is stored up positioned at the liquid
In storage on liquid level.
Preferably, the pipeline between the acidifying case and second filter is stretched into and is acidified in case, described to stretch into acidifying
The height value of case pipeline is the 1/20-1/10 of the height for being acidified case, and it is externally provided with filter mantle, and the filter mantle is provided with many
Individual aperture is 100 μm of hole.
Preferably, second filter includes sample room, filter membrane and core, and the filter membrane is located in the sample room,
And supported by the core;The aperture span of the filter membrane is 0.1-0.7 μm.
Preferably, during the pipeline between the liquid memory and the adsorption and enrichment device stretches into liquid memory, institute
It is the 1/30-1/20 of the height of liquid memory to state and stretch into the height value of liquid memory pipeline, and it is externally provided with filter mantle,
The filter mantle is provided with the hole that multiple apertures are 100 μm.
Preferably, the reactor uses alkali resistant materials, and it is provided with closure above, and lower end is funnel shaped, reactor
Inside it is additionally provided with agitator, liquid level sensor and pH sensors;The end face of the closure is provided with least 5 through holes.
Preferably, the general control system include control unit and touch screen device, described control unit with the reactor
In interior pH sensors, agitator, liquid level sensor, the first metering dosing pump, the second metering dosing pump, vavuum pump, acidifying case
PH sensors, agitator control connection;The pH sensors are provided with lifting platform, can rise pH sensors if necessary.
The extraction of soil hydrophobic fulvic acid component is carried out using described soil hydrophobic fulvic acid component extraction purification device
Method, it comprises the following steps:
(1) soil is added in soil storage room, and to injecting pure water in reactor;
(2) pH adjustment units are started, the first metering dosing pump receives pH sensor signals in being located at reactor and starts alkali lye
Addition program, the first chemicals dosing plant passes through the pipeline of resistance to highly basic to alkali lye is injected in reactor, while starting the stirring in reactor
Motor, makes alkali lye dispersed, and until reaching default pH value, the first metering dosing pump is stopped;
(3) outlet valve of reactor is opened, while starting vavuum pump, the liquid in reactor is pressed through through vavuum pump
First filter is flowed into acidifying case, and the insoluble impurity of alkali is removed by membrane retention, and the liquid gone after the removal of impurity passes through filter membrane stream
Enter to be acidified in case;
(4) acid-base value adjustment unit is started, the second metering dosing pump receives the pH sensor signals being located in acidifying case and opens
Dynamic acid solution adds program, and it is acidproof by first that the second metering dosing pump extracts acid solution by first passage from the first acid solution chemical tank
Pipeline, while starting stirring motor in acidifying case, makes acid solution dispersed, until reaching to non-oxidizable acid solution is injected in acidifying case
To default pH value, the second metering dosing pump first passage acid liquid program stopped work, sensor lifting platform rise pH sensings
Device is popped one's head in;
Second metering dosing pump extracts hydrofluoric acid and passes through the second acid-resistant pipeline by second channel from the second acid solution chemical tank
In injection acidifying case, until reaching default hydrofluoric acid concentration, the second metering dosing pump is stopped;
(5) after completing pH value regulation, the outlet valve of acidifying case is opened, while starting vavuum pump, is pressed by vavuum pump,
Organic matter solution in acidifying case is by the way that in the second filter influent holder, sour insoluble impurity is by the second filter
Membrane retention and remove, the runic fulvic acid solution gone after the removal of impurity is by filter membrane influent holder;
(6) after completing filtering, the outlet valve of liquid memory is opened, the thick fulvic acid solution that carries in liquid memory leads to
Piping flows into adsorption and enrichment device, and fulvic acid is attracted on resin;
(7) after the completion of adsorbing, the communicating valve between elution device and adsorption and enrichment device is opened, while opening adsorption and enrichment
The waste liquid dump valve of bottom of device, the pure water in elution device injects adsorption and enrichment device by pipeline, to adsorption and enrichment device
It is rinsed, flushing liquor is directly discharged from waste liquid dump valve, completes the flushing to adsorption and enrichment device;
The communicating valve closed between elution device and adsorption and enrichment device, simultaneously closes off the waste liquid of adsorption and enrichment bottom of device
Dump valve;The communicating valve between elution device and ion interchange unit is opened, while opening the waste liquid of ion interchange unit bottom
Dump valve, the pure water in elution device injects ion interchange unit by pipeline, ion interchange unit is rinsed, flushing liquor
Directly from waste liquid dump valve discharge, the flushing to ion interchange unit is completed;
The communicating valve closed between elution device and ion interchange unit, simultaneously closes off the waste liquid of ion interchange unit bottom
Dump valve, opens the communicating valve between the second chemicals dosing plant and adsorption and enrichment device, the second chemicals dosing plant by alkaline-resisting pipeline to
Alkali lye is injected in adsorption and enrichment device, is desorbed in the presence of alkali lye by the hydrophobic fulvic acid after resin adsorption, after desorption
Liquid flow into ion interchange unit, through in ion interchange unit hydrogen type cation exchange resin adsorb after discharge, discharged
The soil hydrophobic fulvic acid solution that is extracted for needed for of liquid, solid-state soil hydrophobic fulvic acid is obtained after freeze-drying.
Preferably, the alkali lye in first chemicals dosing plant is saturation or nearly saturation strong base solution, in the second chemicals dosing plant
Alkali lye for 0.001-0.5mol/L highly basic;The resistance to highly basic requirements for pipes can bear saturation highly basic, and the alkaline-resisting pipeline will
Seek the highly basic that can bear 0.001-0.5mol/L;The pH preset values of liquid are 10-14 in the reactor.
Preferably, the first acid-resistant pipeline requirement can bear the non-oxidizable strong acid of 10mol/L;Second acid-proof pipe
Road requirement can bear the hydrofluoric acid of 6mol/L;The preset concentration of hydrofluoric acid is 0.01-1mol/L in the acidifying case;The acidifying
The pH preset values of liquid are 0.5-1.5 in case.
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, powers 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.
Compared with prior art, the beneficial effect comprise that:
(1) the soil hydrophobic fulvic acid component extraction purification device that the present invention is provided, simple structure is easy to operate, automatically
Change degree is high, can efficiently extract the liquid of required concentration, preferably using the hydrophobic fulvic acid in soil;
(2) reactor, acidifying case, the bottom of liquid memory are funnel shaped, stretch into reactor, the pipeline of acidifying case
Filter mantle is externally provided with, it is the 1/20-1/10 of the height of reactor to stretch into the height value of reactor pipeline, stretches into the pipe of acidifying case
Road is externally provided with filter mantle, and the height value for stretching into acidifying case pipeline is the 1/30-1/20 of tank height, can both ensure maximum limit
The collection fulvic acid of degree, improves unit efficiency, can effectively prevent impurity particle from being mixed into sample again, it is ensured that extract solution
Purity;
(3) pH value regulation and acid-base value adjustment unit are full automatic, save labour, the pH value of regulation it is accurate
Rate is higher;First acid solution chemical tank and the second acid solution chemical tank share a metering dosing pump, by further optimization pH value
Adjustment unit and acid-base value adjustment unit can share a metering dosing pump for multichannel, further reduce production cost;Acidifying
Case, liquid memory share a vavuum pump, reduce production cost;
(4) filler in fulvic acid extraction unit in adsorption and enrichment device uses XAD-8 resins, DAX-8 resins and XAD-7
One or more of resin, the filler in ion interchange unit uses hydrogen type cation exchange resin, can more effectively to dense
Impurity absorption and purification in water, obtain concentration DOM liquid higher;
(5) reactor has reserved inert gas entrance and outlet, aborning by being passed through the indifferent gas such as nitrogen, helium
Body, can effectively suppress the oxidation of soil hydrophobic fulvic acid under strong alkaline condition.
Brief description of the drawings
The structural representation of one embodiment that Fig. 1 is provided for the present invention;
Fig. 2 is second structural representation of embodiment that the present invention is provided.
Specific embodiment
Below in conjunction with the accompanying drawings, specific embodiment of the invention is described in detail.
Shown in ginseng Fig. 1, Fig. 1 is the technological process of the soil hydrophobic fulvic acid component extraction purification device that the present invention is provided
Figure.The soil hydrophobic fulvic acid component extraction purification device that the present invention is provided, including reactor 1, pH adjustment units, the first filtering
Clean unit, acidifying case 11, acid-base value adjustment unit, the second filtration, purification unit, liquid memory 14, fulvic acid extraction unit
With general control system 6;Soil storage room 2, support 3, agitator, liquid level sensor and pH sensors wherein are provided with reactor 1,
The soil storage room 2 is supported and in reactor 1 by support 3, and the outer wall of soil storage room 2 is provided with multiple apertures and is less than
The hole of 1mm;PH adjustment units include the first metering chemicals dosing plant 5 of dosing pump 4 and first;First filtration, purification unit includes filtering
Device 7 and vavuum pump 12, wherein the first filter 7 includes sample room 71, filter membrane 72 and core 73, filter membrane 72 is located at sample room 71
It is interior, and supported by core 73;Acid-base value adjustment unit includes the second metering dosing pump 8, the first acid solution chemical tank 9 and the second acid solution
Chemical tank 10;Second filtration, purification unit includes the second filter 13 and vavuum pump 12, and the second filter 13 includes sample room
131st, filter membrane 132 and core 133, filter membrane 132 are supported in sample room 131 by core 133;General control system 6 is mainly adopted
With automatically controlling, wherein collection control operation unification in switch board is carried out, whole system can be made to realize automatically controlling operation and manually
Operation.
Wherein, the first chemicals dosing plant 5 is connected by the first metering dosing pump 4 with reactor 1, the first metering dosing pump 4
Entrance is connected with the first chemicals dosing plant 5, and its outlet is connected with reactor 1;The outlet of reactor 1 and the entrance of the first filter 7
Connection, the connecting pipe between the filter 7 of reactor 1 and first is stretched into reactor 1, stretches into the height value of reactor pipeline
It is the 1/20-1/10 of the height of reactor 1, and it is externally provided with protective cover, the protective cover is provided with the hole that multiple apertures are 1mm;
The outlet of the first filter 7 is connected with the entrance of acidifying case 11, and the outlet of vavuum pump 12 is placed in the cavity of acidifying case 11;First
The acid solution chemical tank 10 of acid solution chemical tank 9 and second is arranged in juxtaposition, and the second metering dosing pump 8 is located at the first acid solution chemical tank 9 and the
Between two acid solution chemical tanks 10, outlet, the second acid solution medicament of the entrance and the first acid solution chemical tank 9 of the second metering dosing pump 8
The outlet connection of case 10, the outlet of the second metering dosing pump 8 is connected with acidifying case 11, is acidified outlet and second filter of case 11
13 entrance connection, agitator and pH sensors are provided with acidifying case 11;The outlet of the second filter 13 and liquid memory 14
Entrance connection, vavuum pump 12 is connected with liquid memory 14, and the outlet of liquid memory 14 is connected with fulvic acid extraction unit.
General control system 6 includes control unit and touch screen device, and control unit be connected with touch screen device, control unit and stirs
Device, liquid level sensor, pH sensors, the first metering dosing pump 4, the second measuring pump 8 and vavuum pump 12 are connected.
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, being equipped with the switch board of independent operation in control system, electric switch and electrical equipment are all
Concentrate in switch board, power switch is protected with electrical control cubicles gate interlock, can reach dust-proof, rapid heat dissipation and the effect being easily installed
Really.
Embodiment one
Shown in ginseng Fig. 1, Fig. 1 is first implementation of the soil hydrophobic fulvic acid component extraction purification device that the present invention is provided
The structural representation of example;In Fig. 1, fulvic acid extraction unit includes elution device 15a, the second chemicals dosing plant 16a, adsorption and enrichment
Device 17a and ion interchange unit 18a;Wherein, the entrance of adsorption and enrichment device 17a is connected with the outlet of liquid memory 14,
The outlet of adsorption and enrichment device 17a is connected with the entrance of ion interchange unit 18a, the outlet of elution device 15a respectively with absorption
The entrance connection of the entrance, ion interchange unit 18a of enriching apparatus 17a, outlet and the adsorption and enrichment of the second chemicals dosing plant 16a are filled
Put the entrance connection of 17a;The bottom of adsorption and enrichment device 17a, the bottom of ion interchange unit 18a are equipped with waste liquid dump valve.
The process that hydrophobic fulvic acid extraction is carried out using the soil hydrophobic fulvic acid component extraction purification device shown in Fig. 1 is such as
Under:
General supply and start button are first turned on, makes whole system in running order, to adding one in soil storage room
Pedotheque after quantitative grinding, and close soil storage room;Start water filling program, to adding pure water, reactor in reactor 1
Liquid level sensor in 1 is detected to the water level in reactor 1, and when water level reaches the 4/5 of reactor cumulative volume, liquid level is passed
Sensor sends liquid level signal to general control system, stops the injecting process.
To inert gas is passed through in reactor, under the protection of inert gas, start pH adjustment units, the first metering dosing
The pH sensor signals that pump 4 is received in reactor 1 start alkali lye and add program, and the first chemicals dosing plant 5 passes through the pipe of resistance to highly basic
Road in reactor 1 to injecting alkali lye, while starting the stirring motor in reactor 1 so that alkali lye is dispersed, pre- until reaching
If pH value, first metering dosing pump 4 is stopped.
Lasting stirring, the hole that the pedotheque leaching liquid in soil storage room 2 is stored on chamber outer wall by soil flows into anti-
In answering kettle 1.The outer wall of soil storage room 2 is provided with hole of multiple apertures less than 1mm, can effectively prevent the impurity in soil from entering
Enter in the liquid of reactor 1;Wherein reactor 1 uses alkali resistant materials, and it is provided with closure above, and lower end is funnel shaped,
Agitator, liquid level sensor and pH sensors are provided with it, the end face of the closure is provided with least 5 through holes.
The outlet valve of reactor 1 is opened, while starting vavuum pump 12, is pressed by vavuum pump 12, the liquid in reactor 1
Body is flowed into acidifying case 11 by the first filter 7, and the insoluble impurity of alkali is retained and removed, the liquid gone after the removal of impurity by filter membrane 72
Flowed into by filter membrane 72 and be acidified in case 11.
Acidifying case 11 uses acid-fast alkali-proof material, and it is provided with closure above, and lower end is funnel shaped, the closure
End face is provided with least 5 through holes.
Start acid-base value adjustment unit, required pH value is set in general control system 6, its pH value for setting is 0.5-
1.5, and this pH sensor signal is delivered to the pH sensors in acidifying case 11, pH sensors give pH value signal transmission
Second metering dosing pump 8, the pH sensor signals that the second metering dosing pump 8 is received in acidifying case 11 start acid solution and add journey
Sequence, second metering dosing pump 8 from the first acid solution chemical tank 9 extract acid solution by the first acid-resistant pipeline to acidifying case 11 in inject non-
Oxidisability acid solution, while starting stirring motor in acidifying case 11 so that acid solution is dispersed, until reaching default pH value, the
Two metering dosing pump 8 first passage acid liquid program stopped work, sensor lifting platform rises pH sensor probes;
Second metering dosing pump 8 extracts hydrofluoric acid by second channel from the second acid solution chemical tank 10, resistance to by second
To hydrofluoric acid is injected in acidifying case 11, until reaching default hydrofluoric acid concentration, the second metering dosing pump 8 stops work in acid tube road
Make.
PH value adjustment unit and acid-base value adjustment unit can share a multi-channel metering dosing pump.
After completing acid-base value regulation, the outlet valve of acidifying case 11 is opened, while start vavuum pump 12, by vavuum pump 12
Pressure, the organic matter solution in acidifying case 11 is by the way that in the influent holder 14 of the second filter 13, organic matter is through the second mistake
Sour insoluble impurity is trapped within filter membrane 132 after filter 13, in runic fulvic acid solution influent holder 14.
After completing filtering, the outlet valve of liquid memory 14 is opened, slightly fulvic acid solution is carried in liquid memory 14
Adsorption and enrichment device 17a is flowed into by pipeline, fulvic acid is attracted on resin;
After the completion of absorption, the communicating valve between elution device 15a and adsorption and enrichment device 17a is opened, while opening absorption
The waste liquid dump valve of enriching apparatus 17a bottoms, the pure water in elution device 15a is right by pipeline injection adsorption and enrichment device 17a
Adsorption and enrichment device 17a is rinsed, and flushing liquor is directly discharged from waste liquid dump valve, and completion is rushed to adsorption and enrichment device 17a
Wash;
The communicating valve closed between elution device 15a and adsorption and enrichment device 17a, simultaneously closes off adsorption and enrichment device 17a
The waste liquid dump valve of bottom;The communicating valve between elution device 15a and ion interchange unit 18a is opened, while open ion handing over
The waste liquid dump valve of changing device 18a bottoms, pure water in elution device 15a injects ion interchange unit 18a by pipeline, to from
Sub- switch 18a is rinsed, and flushing liquor is directly discharged from waste liquid dump valve, completes the flushing to ion interchange unit 18a;
The communicating valve closed between elution device 15a and ion interchange unit 18a, simultaneously closes off ion interchange unit 18a
The waste liquid dump valve of bottom, opens the communicating valve between the second chemicals dosing plant 16a and adsorption and enrichment device 17a, the second dosing dress
16a is put by alkaline-resisting pipeline to alkali lye is injected in adsorption and enrichment device 17a, by the hydrophobic fulvic acid after resin adsorption in alkali lye
Effect is lower to be desorbed, and the liquid after desorption flows into ion interchange unit 18a, through the Hydrogen sun in ion interchange unit 18a from
Sub-exchange resin is discharged after exchanging, the soil hydrophobic fulvic acid solution that the liquid discharged is extracted for needed for, after freeze-drying
To solid-state soil hydrophobic fulvic acid.
Embodiment two
Shown in ginseng Fig. 2, Fig. 2 is second implementation of the soil hydrophobic fulvic acid component extraction purification device that the present invention is provided
The structural representation of example;In fig. 2, fulvic acid extraction unit includes elution device 15b, the second chemicals dosing plant 16b, primary adsorption
Enriching apparatus 17b, the first ion interchange unit 18b, secondary absorption enriching apparatus 19b, the second ion interchange unit 20b;Wherein,
The entrance of primary adsorption enriching apparatus 17b is connected with the outlet of liquid memory 14, the outlet of adsorption and enrichment device 17b respectively with
The entrance connection of the entrance, secondary absorption enriching apparatus 19b of the first ion interchange unit 18b;The secondary absorption enrichment
The outlet of device 19b is connected with the entrance of the second ion interchange unit 20b;The outlet of the elution device 15b respectively with
The entrance of the primary adsorption enriching apparatus 17b, the entrance of the first ion interchange unit 18b, secondary absorption enriching apparatus 19b
The entrance connection of entrance, the second ion interchange unit 20b;The outlet of the second chemicals dosing plant 16b is inhaled with the one-level respectively
The entrance connection of the entrance, secondary absorption enriching apparatus 19b of attached enriching apparatus 17b;
The bottom of primary adsorption enriching apparatus 17b, the bottom of the first ion interchange unit 18b, secondary absorption enriching apparatus
The bottom of 19b, the bottom of the second ion interchange unit 20b are equipped with waste liquid dump valve.
The runic process and embodiment one of the filtering of the soil organism, the regulation of acid-base value and fulvic acid in the present embodiment be
Identical, difference is the difference of fulvic acid extraction unit, and in the present embodiment, the extraction process of fulvic acid is as follows:Completed
After filter, the outlet valve of liquid memory 14 is opened, thick in liquid memory 14 is carried fulvic acid solution and flowed successively by pipeline
Enter primary adsorption enriching apparatus 17b and secondary absorption enriching apparatus 19b, fulvic acid is attracted on resin;
Primary adsorption enriching apparatus alkali lye is eluted:Close primary adsorption enriching apparatus 17b and secondary absorption enriching apparatus 19b
Between communicating valve, close primary adsorption enriching apparatus 17b and the first ion interchange unit 18b between connection valve, open
Communicating valve between elution device 15b and primary adsorption enriching apparatus 17b, opens the useless of primary adsorption enriching apparatus 17b bottoms
Liquid waste cock, by pipe flushing primary adsorption enriching apparatus 17b, flushing waste is by useless for the pure water in elution device 15b
Liquid waste cock is discharged, and completes the flushing of primary adsorption enriching apparatus 17b, closes the useless of primary adsorption enriching apparatus 17b bottoms
Liquid waste cock, the communicating valve closed between elution device 15b and primary adsorption enriching apparatus 17b;
The communicating valve between elution device 15b and the first ion interchange unit 18b is opened, the first ion interchange unit is opened
The waste liquid waste cock of 18b bottoms, the pure water in elution device 15b is rinsed by pipe flushing the first ion interchange unit 18b
Waste liquid is discharged by waste liquid waste cock, completes the flushing of the first ion interchange unit 18b, closes the first ion interchange unit
The waste liquid waste cock of 18b bottoms, the communicating valve closed between elution device 15b and the first ion interchange unit 18b;
The communicating valve between the second chemicals dosing plant 16b and the first adsorption and enrichment device 17b is opened, primary adsorption enrichment is opened
Communicating valve between device 17b and the first ion interchange unit 18b, the alkali lye in the second chemicals dosing plant 16b passes through alkaline-resisting pipeline
To alkali lye is injected in primary adsorption enriching apparatus 17b, desorbed in the presence of alkali lye by the fulvic acid of resin adsorption, desorbed
Efflux afterwards is discharged after the hydrogen type cation exchange resin in the first ion interchange unit 18b, extracts discharged liquid,
It is subfraction 1 that directly freezed dries mark;
Secondary absorption enriching apparatus alkali lye is eluted:Close secondary absorption enriching apparatus 19b and the second ion interchange unit 20b
Between connection valve, open elution device 15b and secondary absorption enriching apparatus 19b between communicating valve, open secondary absorption
The waste liquid waste cock of enriching apparatus 19b bottoms, the pure water in elution device 15b passes through pipe flushing secondary absorption enriching apparatus
19b, flushing waste is discharged by waste liquid waste cock, completes the flushing of secondary absorption enriching apparatus 19b, closes secondary absorption rich
The waste liquid waste cock of acquisition means 19b bottoms, the communicating valve closed between elution device 15b and secondary absorption enriching apparatus 19b;
The communicating valve between elution device 15b and the second ion interchange unit 20b is opened, the second ion interchange unit is opened
The waste liquid waste cock of 20b bottoms, the pure water in elution device 15b is rinsed by pipe flushing the second ion interchange unit 20b
Waste liquid is discharged by waste liquid waste cock, completes the flushing of the second ion interchange unit 20b, closes the second ion interchange unit
The waste liquid waste cock of 20b bottoms, the communicating valve closed between elution device 15b and the second ion interchange unit 20b;
The communicating valve between the second chemicals dosing plant 16b and secondary absorption enriching apparatus 19b is opened, secondary absorption enrichment is opened
Communicating valve between device 19b and the second ion interchange unit 20b, the second chemicals dosing plant 16b is inhaled by alkaline-resisting pipeline to two grades
Alkali lye is injected in attached enriching apparatus 19b, is desorbed in the presence of alkali lye by the fulvic acid solution after resin adsorption, after desorption
Efflux exchanged through the hydrogen type cation exchange resin in the second ion interchange unit 20b after discharge, extract discharged liquid
Body, it is subfraction 2 that directly freezed dries mark;
It is fulvic acid solid sample to merge fulvic acid subfraction 1,2.
The process of the pH value regulation in pH value adjustment unit and acid-base value adjustment unit is full automatic process, saves
Labour, reduces production cost, and the accuracy of the pH value modulated is higher, and the process efficiency of preparation is also higher.In pH
During regulation, turn on agitator motor makes the liquid in agitator stirred autoclave 1, acidifying case 11 so that flow into therein
Acid solution medicament is uniformly dissolved in water, and local pH value can be avoided higher or relatively low.
The filter membrane used in first filter is disposable filter membrane, and filter membrane needs to be resistant to 1mol/L highly basic, filter membrane
Store on request and use, but the siliceous filter membrane such as unusable glass fiber filter;The filter membrane used in second filter
It is disposable filter membrane, filter membrane is needed to be resistant to 0.5mol/L strong acid, and filter membrane is stored and used on request, but unusable glass fibers
The siliceous filter membranes such as dimension filter membrane.
A series of detailed description illustrating only for feasibility implementation method of the invention mentioned above,
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 present inventive concept is not departed from belongs to protection scope of the present invention.