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WO2018145457A1 - Appareil d'extraction et de purification de matières organiques dissoutes hydrophobes de sol - Google Patents

Appareil d'extraction et de purification de matières organiques dissoutes hydrophobes de sol Download PDF

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Publication number
WO2018145457A1
WO2018145457A1 PCT/CN2017/101705 CN2017101705W WO2018145457A1 WO 2018145457 A1 WO2018145457 A1 WO 2018145457A1 CN 2017101705 W CN2017101705 W CN 2017101705W WO 2018145457 A1 WO2018145457 A1 WO 2018145457A1
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Prior art keywords
adsorption
outlet
organic matter
tank
inlet
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PCT/CN2017/101705
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English (en)
Chinese (zh)
Inventor
白英臣
吴丰昌
冯承莲
吴代赦
谌书
林道辉
孙文春
Original Assignee
中国环境科学研究院
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Priority claimed from CN201710069420.9A external-priority patent/CN106932259B/zh
Priority claimed from CN201710069146.5A external-priority patent/CN106885721B/zh
Application filed by 中国环境科学研究院 filed Critical 中国环境科学研究院
Publication of WO2018145457A1 publication Critical patent/WO2018145457A1/fr

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q

Definitions

  • the invention relates to the field of organic matter extraction, in particular to an extraction and purification device for dissolving organic matter in soil water.
  • Soil water-soluble organic matter refers to natural organic matter in the soil that is soluble in water and can pass through a 0.45 ⁇ m filter. It is a kind of special polymer compound formed by the residues of animals and plants and formed by microorganisms. The main components are humic acid and fulvic acid. Studies have shown that soil water-soluble organic matter is both a source of plant nutrients and an energy source for heterotrophic microorganisms in the soil. It directly affects the soil's fertility, conservation, buffering capacity, ventilation, etc., which determines the soil nutrient storage and supply level, and is an important indicator of soil fertility.
  • the dissolved organic matter in the soil can interact with heavy metals, which in turn affects the migration, transformation and fate of toxic and harmful refractory substances such as heavy metals in the environment.
  • soil hydrophobic dissolved organic matter enters the aquatic ecosystem through material circulation and participates in various processes in the water environment. It can also enter the atmosphere through microbial action and have a great impact on the global climate.
  • Research on the dissolution of organic matter in soil water has become a hot topic in agronomy, environmental science and ecology research.
  • soil organic matter content is low and soil types are numerous. How to achieve efficient extraction of organic matter from soil is an urgent problem to be solved.
  • Chinese invention patent (201010289718.9: soil organic matter extraction device and method of use thereof) provides a soil organic matter extraction device, which comprises an extraction bottle, which is composed of a bottle body and a bottle cap, and is characterized in that it further comprises a turnover box , a rotating shaft, a fixing rod, a flat plate, a closing cover and a box body, the fixing rod is composed of two vertical rods and two horizontal rods connecting the vertical rods, and the upper part of the turning box is provided with at least one opening, the extracting The bottle is placed in the opening, and two opposite planes of the turning box are respectively welded with a flat plate.
  • the rotating shaft passes through the entire turning box from the flat plate on one side of the turning box and passes out from the other side of the turning box.
  • the rotor of the motor passes through the transmission device.
  • the other end of the rotating shaft is inserted between the two vertical rods of the fixed rod, the closing cover is placed on the upper part of the turning box, and is connected with the turning box, the turning box is placed in the box body, and the transmission device is placed in the box body.
  • the utility model patent (201420455113.6: a soil organic matter extraction purification and concentration device) provides a soil organic matter extraction purification and concentration device, which comprises an extraction tube, a communication tube and a concentrating tube, and a condensation tube is arranged at the top of the extraction tube.
  • the extraction pipe and the communication pipe are respectively connected through the air flow pipe and the return pipe, and the bottom of the communication pipe is connected with the sample bottle; the top of the communication pipe is connected with the inlet end of the concentrating pipe, the outlet end of the concentrating pipe is connected to the condensing pipe 2, and the bottom of the condensing pipe is connected
  • the bottle is recycled and has a vacuum pump port on the bottle.
  • the soil organic matter extracting device provided by the above invention patent firstly places a soil sample in an extraction bottle, dehydrates it by adding anhydrous sodium sulfate, and then extracts the soil by extracting the extraction reagent, and then passes the extracted extract through the loading.
  • Water The organic matter of the soil was extracted by a funnel filtration of sodium sulfate.
  • the device uses acetone, dichloromethane and n-hexane as organic solvents, and the extraction of soil organic matter is incomplete; the degree of automation of the device is low, and the amount of extracted organic matter is small; the extraction of soil organic matter is generally used for the determination of organic pollutants and is not suitable for a large number of solids. Preparation of soil hydrophobic organic matter.
  • the above utility model patent provides a soil organic matter extraction purification and concentration device, which mainly extracts soil organic matter by steam, and when the extraction time is sufficient, the extraction liquid is returned to the sample bottle, and then the extraction of the sample bottle is performed by using the condensed water. The liquid was concentrated.
  • the device is a small laboratory device suitable for experimental analysis of organic matter in soil. It is not suitable for large-scale soil water-soluble organic matter extraction and solid soil water-soluble organic matter preparation; low-melting organic solvent should be used as extractant, soil organic matter extraction Incomplete, the concentration of extracted organic matter is low.
  • the present invention provides an extraction and purification device for dissolving organic matter in soil water, which can realize efficient extraction of organic matter in soil water, convenient operation and high degree of automation.
  • the present invention provides a device for extracting and purifying soil-dissolved organic matter, including a reaction kettle, a pH adjusting unit, a filtering and purifying unit, an acidizing tank, a pH adjusting unit, and an organic substance. Extraction unit and overall control system;
  • An inlet of the reaction vessel is connected to an outlet of the pH adjustment unit; an outlet of the reaction vessel is connected to an inlet of the filtration purification unit, and an outlet of the filtration purification unit is connected to an inlet of the acidification tank;
  • An inlet of the acidification tank is further connected to an outlet of the pH adjustment unit, and an outlet of the acidification tank is connected to an inlet of the organic matter extraction unit;
  • the pH adjusting unit and the pH adjusting unit are connected to the total control system;
  • a soil storage chamber is arranged in the reaction kettle, and the soil storage chamber is supported by the support and located in the reaction kettle;
  • a plurality of holes having a pore diameter of less than 1 mm are disposed on the outer wall of the soil storage chamber to prevent impurities in the soil from entering the reaction vessel.
  • the organic matter extracting unit comprises a rinsing device, a second medicating device, an concentrating and accumulating device, and an ion exchange device; the outlet of the rinsing device and the outlet of the second medicating device are both concentrated and adsorbed An inlet connection of the device, an outlet of the adsorption-concentrating device being connected to an inlet of the ion exchange device; an inlet of the ion exchange device is also connected to an outlet of the elution device;
  • the bottom of the adsorption and enrichment device and the bottom of the ion exchange device are provided with a waste liquid discharge valve.
  • the adsorption and enrichment device comprises an adsorption column and a filler, wherein the filler is disposed in the adsorption column, and the filler is one or more of XAD-8 resin, DAX-8 resin and XAD-7 resin.
  • the ion exchange device includes an adsorption column and a filler, the filler is disposed in the adsorption column, and the filler is a hydrogen type cation exchange resin.
  • the organic matter extracting unit comprises a first-stage adsorption and enrichment device, a first ion exchange device, a second-stage adsorption and enrichment device, a second ion exchange device, a rinse device, and a third dosing device;
  • An inlet of the device is connected to an outlet of the acidification tank, and an outlet of the first-stage adsorption and enrichment device is respectively connected to an inlet of the first ion exchange device and an inlet of the second adsorption and concentration device;
  • An outlet of the collecting device is connected to an inlet of the second ion exchange device;
  • an outlet of the eluent device is respectively connected to an inlet of the first-stage adsorption enrichment device, an inlet of the first ion exchange device, and a secondary adsorption enrichment device
  • the inlet of the second ion exchange device; the outlet of the third dosing device is respectively connected to the inlet of the first-stage adsorption and enrichment device and
  • the bottom of the first-stage adsorption and concentration device, the bottom of the first ion exchange device, the bottom of the secondary adsorption and concentration device, and the bottom of the second ion exchange device are all provided with a waste liquid discharge valve.
  • the first-stage adsorption and enrichment device comprises an adsorption column and a filler, and the filler is disposed in the adsorption column, and the filler is one of XAD-8 resin, DAX-8 resin and XAD-7 resin.
  • the first ion exchange device comprises an adsorption column and a filler, the filler is disposed in the adsorption column, and the filler is a hydrogen type cation exchange resin.
  • the secondary adsorption-enrichment device comprises an adsorption column and a filler, the filler is disposed in the adsorption column, the filler is XAD-4 resin; and the second ion exchange device comprises an adsorption column and a filler, The filler is disposed in the adsorption column, and the filler is a hydrogen type cation exchange resin.
  • the organic matter extracting unit comprises a rinsing device, an organic solvent drug tank, a first-stage adsorption and enrichment device, and a second-stage adsorption and enrichment device; an inlet of the first-stage adsorption and enrichment device is connected to an outlet of the acidification tank The outlet of the first-stage adsorption and enrichment device is connected to the inlet of the second-stage adsorption and enrichment device; the outlet of the eluent device and the outlet of the organic solvent reagent tank are connected to the inlet of the first-stage adsorption and enrichment device; The bottom of the first-stage adsorption and enrichment device and the bottom of the second-stage adsorption and enrichment device are provided with a waste liquid discharge valve.
  • the first-stage adsorption and enrichment device comprises an adsorption column and a filler, and the filler is disposed in the adsorption column, and the filler is one of XAD-8 resin, DAX-8 resin and XAD-7 resin.
  • the secondary adsorption-enrichment device comprises an adsorption column and a filler, the filler is disposed in the adsorption column, and the filler is XAD-4 resin.
  • the organic matter extracting unit comprises a rinsing device, an organic solvent medicinal tank and an adsorption and enrichment device, an inlet of the sorption and enrichment device is connected to an outlet of the acidification tank; an outlet of the rinsing device, an organic solvent
  • the outlet of the chemical tank is connected to the inlet of the adsorption and enrichment device, and the bottom of the adsorption and concentration device is provided with a waste liquid discharge valve.
  • the adsorption and enrichment device comprises an adsorption column and a filler, and the filler is disposed in the adsorption column, and the filler is one or more of XAD-8 resin, DAX-8 resin and XAD-7 resin.
  • the filler is one or more of XAD-8 resin, DAX-8 resin and XAD-7 resin.
  • the filtration purification unit comprises a filter and an evacuation pump, an inlet of the filter is connected to an outlet of the reaction kettle, an outlet of the filter is connected to an inlet of the acidification tank, and an outlet of the acidification tank Connected to an inlet of the adsorptive enrichment device; the vacuum pump is coupled to the acidification tank.
  • the acidification tank adopts an acid-resistant and alkali-resistant material, and has a sealing cover on the upper side and a funnel shape on the lower end, and at least five through holes are provided on the end surface of the sealing cover.
  • the conduit between the filter and the acidification tank extends into the acidification tank, and the conduit extending into the acidification tank is located above the liquid level in the acidification tank.
  • the filter comprises an impurity storage chamber, a filter membrane and a sand core, the filter membrane is disposed in the impurity storage chamber and supported by the sand core; the filter membrane has a pore diameter ranging from 0.1 to - 0.7 ⁇ m.
  • the pH adjustment unit comprises a pH sensor, a stirrer, a first metering dosing pump, a first acid solution tank and a second acid solution tank; the pH sensor and the agitator are disposed in the acidification tank
  • the first acid liquid medicine tank and the second acid liquid medicine tank are arranged side by side; the inlet of the first metering dosing pump is respectively connected with the outlet of the first acid liquid medicine tank and the outlet of the second acid liquid medicine tank Connected, the outlet of the first metering dosing pump is connected to the acidification tank.
  • the reaction kettle is made of an alkali-resistant material, and has a sealing cover on the upper side and a funnel shape on the lower end, and a stirrer, a liquid level sensor and a pH sensor are further disposed in the reaction kettle; the end surface of the sealing cover is provided with at least 5 Through holes.
  • the pipeline between the reaction vessel and the filter extends into the reaction vessel, and the height of the pipeline extending into the water tank is 1/20-1/10 of the height of the water tank, and the protection is externally provided.
  • the protective cover is provided with a plurality of holes having a hole diameter of 1 mm.
  • the pH adjusting unit comprises a second metering dosing pump and a first dosing device, and a second metering dosing pump is disposed between the first dosing device and the reaction kettle, the second metering An inlet of the dosing pump is coupled to an outlet of the first dosing device, and an outlet of the second dosing pump is coupled to an inlet of the reaction vessel.
  • the total control system comprises a control unit and a touch screen, the control unit and a pH sensor, a stirrer, a liquid level sensor, a second metering dosing pump, and a first metering dosing pump in the reaction kettle.
  • the method for extracting soil water-dissolved organic matter by using the two-stage alkali-washing method for extracting soil hydrophobic organic matter comprises the following steps:
  • the second metering dosing pump receives the pH sensor signal in the reaction kettle to start the lye addition procedure, and the first dosing device injects the alkali solution into the reaction vessel through the alkali resistant pipeline, and starts the reaction kettle.
  • the stirring motor in the mixer makes the alkali liquid evenly distributed until the preset pH value is reached, and the second metering dosing pump stops working;
  • the first metering dosing pump receives the pH sensor signal located in the acidification tank to initiate the acid addition procedure, and the first metering dosing pump draws the acid solution from the first acid solution tank through the first passage
  • the first acid-resistant pipeline injects a non-oxidizing acid into the acidizing tank, and starts the stirring motor in the acidizing tank, so that the acid liquid is evenly dispersed until the preset pH value is reached, and the first metering dosing pump first channel plus acid program stop working;
  • the first metering dosing pump draws hydrofluoric acid from the second acid solution tank through the second passage into the acidification tank through the second acid-proof pipeline until the preset hydrofluoric acid concentration is reached, and the first metering dosing pump and the agitating motor stop. Work, the sensor lifts raise the pH sensor probe;
  • the liquid flows into the adsorption enrichment device through the pipeline.
  • the communication valve between the elution device and the adsorption enrichment device is opened, and the waste liquid discharge valve at the bottom of the adsorption enrichment device is opened.
  • the pure water in the washing device is injected into the adsorption enrichment device through the pipeline for flushing, and the flushed waste liquid is discharged through the waste liquid discharge valve to complete the flushing of the adsorption and enrichment device;
  • the liquid discharge valve, the pure water in the ejecting device is injected into the ion exchange device through the pipeline for flushing, and the flushed waste liquid is discharged through the waste liquid discharge valve to complete the flushing of the ion exchange device;
  • the communication valve between the eluent device and the ion exchange device is closed, and the waste liquid discharge valve at the bottom of the ion exchange device is closed, and the communication valve between the second dosing device and the adsorption enrichment device is opened, and the second valve is opened.
  • the dosing device injects the alkali solution into the adsorption and enrichment device through the alkali-resistant pipeline, and the organic matter adsorbed by the resin is desorbed by the action of the alkali liquid, and the desorbed liquid flows into the ion exchange device, and the hydrogen-type cation exchange resin in the ion exchange device is Discharge, the discharged liquid is the concentrated soil of the desired extracted soil, dissolved in organic matter, and freeze-dried to obtain solid soil water-soluble organic matter.
  • the lye in the first dosing device is a high concentration saturated or nearly saturated strong alkali solution, and the alkali resistant pipeline is required to withstand a saturated strong base.
  • the alkali solution in the second dosing device and the third dosing device is a strong base of 0.01-0.5 mol/L; the alkali-resistant pipe is required to withstand a strong base of 0.5 mol/L.
  • the pH of the liquid in the reactor is preset to a value of 10-14.
  • the organic solvent tank and the non-polar volatile organic solvent in the organic-resistant pipeline are methanol, ethanol or a mixture thereof.
  • the first acid-resistant pipeline is required to withstand 10 mol/L of non-oxidizing strong acid; the second acid-resistant pipeline is required to withstand 6 mol/L of hydrofluoric acid; the preset concentration of hydrofluoric acid in the acidizing tank It is 0.01-1 mol/L; the pH of the liquid in the acidification tank is preset to be 1.5-3.5.
  • the total control system adopts low-voltage power distribution
  • the voltage level of the power supply and distribution equipment is 220VAC
  • the low-voltage power distribution cabinet is provided to supply power to the process system power equipment; the power switch and the electric control cabinet door interlock protection in the control system, It can achieve dustproof, fast heat dissipation and easy installation.
  • the reaction vessel is provided with an inert gas inlet and an outlet.
  • an inert gas such as nitrogen or helium gas can be introduced to effectively inhibit the oxidation of the dissolved organic matter in the soil under strong alkaline conditions;
  • the bottom of the reaction kettle and the acidification tank are all funnel-shaped, and a filter cover is arranged outside the pipeline extending into the water tank, and the height of the pipeline extending into the water tank is 1/20-1/10 of the height of the water tank. It ensures the maximum collection of organic matter, improves the efficiency of the device, and can effectively prevent the soil particles in the reactor and the acid insoluble matter in the acidification tank from being mixed into the sample, thus ensuring the purity of the extract;
  • the filler in the adsorption and concentration device in the organic matter extracting unit adopts one or more kinds of XAD-8 resin, DAX-8 resin and XAD-7 resin or a hydrophobic adsorbent material, and the filler in the ion exchange device adopts a hydrogen type
  • the cation exchange resin can more effectively adsorb and purify impurities in the concentrated water, and obtain a high concentration of hydrophobic water to dissolve the organic liquid;
  • the first acid solution tank and the second acid tank share a first metering dosing pump, which reduces the production cost; after further optimizing the pH adjusting unit and the pH adjusting unit, a multi-channel metering dosing pump can be shared, further reduce manufacturing cost;
  • the device for extracting soil hydrophobic organic matter by using two-stage alkali-washing extraction provided by the invention has the advantages of simple structure, convenient operation, high degree of automation, and can effectively extract the liquid of the desired concentration, and better utilize the extract liquid. Hydrophobic water dissolves organic matter.
  • Figure 1 is a schematic view showing the structure of a first embodiment of the present invention
  • Figure 2 is a schematic view showing the structure of a second embodiment of the present invention.
  • Figure 3 is a schematic structural view of a third embodiment of the present invention.
  • Figure 4 is a schematic view showing the structure of a fourth embodiment of the present invention.
  • FIG. 1 is a process flow diagram of an apparatus for extracting soil hydrophobic organic matter by using two-stage alkaline washing type extraction provided by the present invention.
  • the invention provides a device for extracting soil hydrophobic organic matter by two-stage alkaline washing, comprising a reaction kettle 1, a pH adjusting unit, a filtering and purifying unit, an acidizing tank 10, a pH adjusting unit, an organic matter extracting unit and a total control system 6;
  • the reactor 1 is provided with a soil storage chamber 2, a support 3, a stirrer, a liquid level sensor and a pH sensor.
  • the soil storage chamber 2 is supported by the support 3 and located in the reaction vessel 1, and the outer wall of the soil storage chamber 2 is provided.
  • the pH adjusting unit comprises a second metering dosing pump 4 and a first dosing device 5;
  • the filter purifying unit comprises a filter and a vacuum pump 14, wherein the filter comprises an impurity storage chamber 7, a membrane 8 and sand The core 9, the filter 8 is disposed in the impurity storage chamber 7 and supported by the sand core 9;
  • the pH adjustment unit includes a first metering dosing pump 11, a first acid solution tank 12 and a second acid solution tank 13;
  • the control system 6 mainly adopts automatic control, wherein the centralized control operation is uniformly performed in the control cabinet, so that the entire system can realize automatic control operation and manual operation.
  • the first dosing device 5 is connected to the reaction kettle 1 by a second metering dosing pump 4, the inlet of the second metering dosing pump 4 is connected to the outlet of the first dosing device 5, and the second dosing pump 4 is The outlet is connected to the reaction vessel 1; the outlet of the reaction vessel 1 is connected to the inlet of the filter, and the connection pipe between the reaction vessel 1 and the filter is inserted into the reaction vessel 1, and the height of the pipe extending into the reactor is taken as the height of the reactor.
  • the protective cover is provided with a plurality of holes having a hole diameter of 1 mm;
  • the outlet of the filter is connected with the acidification tank 10, and the outlet of the vacuum pump 14 is placed in the acidification tank
  • the first acid liquid medicine tank 12 and the second acid liquid medicine tank 13 are arranged side by side, and the first metering dosing pump 11 is disposed in the acidizing tank and the first acid liquid medicine tank 12 and the second acid liquid medicine tank 13 Between the inlet of the first metering dosing pump 11 and the outlet of the first acid solution tank 12 and the outlet of the second acid solution tank 13, the outlet of the first metering dosing pump 11 is connected to the acidification tank 10, acidifying Box
  • the outlet of 10 is connected to the inlet of the organic matter extraction unit, and the acidification tank is provided with a stirrer and a pH sensor;
  • the total control system 6 includes a control unit and a touch screen, the control unit is connected with the touch screen, the control unit and the agitator, the liquid level
  • the total control system uses low-voltage power distribution, the voltage level of the power supply and distribution equipment is 220VAC, and the low-voltage power distribution cabinet is provided to supply power to the process system power equipment.
  • the control system is equipped with an independent operation of the control cabinet, as well as electrical switches and electrical components are concentrated in the control cabinet, the power switch and the electronic control cabinet door interlock protection, can achieve dust, heat dissipation and easy to install.
  • the organic matter extracting unit comprises a rinsing device 15a, a second dosing device 16a, an adsorption enrichment device 17a, an ion exchange device 18a; an inlet of the adsorption enrichment device 17a is connected to an outlet of the acidification tank 10, an outlet thereof is connected to an inlet of the ion exchange device 18a; and an outlet of the eluent device 15a
  • the outlet of the second dosing device 16a is connected to the inlet of the adsorption enrichment device 17a, and the outlet of the eluent device 15a is also connected to the inlet of the ion exchange device 18a; the bottom of the adsorption enrichment device 17a, the bottom of the ion exchange device 18a
  • An inert gas is introduced into the reaction kettle to start the pH adjusting unit, and the second metering dosing pump 4 receives the pH sensor signal in the reaction vessel 1 to start the lye addition procedure, and the first dosing device 5 reacts to the reaction through the alkali resistant pipeline.
  • the lye is injected into the kettle 1 while the agitation motor in the reaction vessel 1 is started, so that the lye is uniformly dispersed until the preset pH value is reached, and the second metering dosing pump 4 and the agitation motor are stopped.
  • the soil sample leachate in the soil storage chamber 2 flows into the reaction vessel 1 through a hole in the outer wall of the soil storage chamber.
  • the outer wall of the soil storage chamber 2 is provided with a plurality of holes having a pore diameter of less than 1 mm, which can effectively prevent impurities in the soil from entering the liquid of the reaction vessel 1.
  • the reaction kettle 1 is made of an alkali-resistant material, and a sealing cover is arranged on the lower end.
  • the shape of the funnel is provided with an agitator, a liquid level sensor and a pH sensor, and the end surface of the sealing cover is provided with at least 5 through holes.
  • the outlet valve of the reaction vessel 1 is opened, and the vacuum pump 14 is started, and the pressure is applied by the vacuum pump 14.
  • the liquid in the reaction vessel 1 flows into the acidification tank 10 through the filter, and the alkali-insoluble impurities are removed by the filtration membrane 8 to remove the impurities. It flows into the acidification tank 10 through the filter membrane 8.
  • the acidification tank 10 is made of an acid-resistant and alkali-resistant material, and has a sealing cover on the upper side and a funnel shape on the lower end, and at least five through holes are provided on the end surface of the sealing cover.
  • the pH adjustment unit is activated, the desired pH is set in the overall control system 6, the pH is set to 1.5-3.5, and the pH sensor signal is transmitted to the pH sensor located in the acidification tank 10, the pH sensor will pH
  • the value signal is transmitted to the first metering dosing pump 11, the first metering dosing pump 11 receives the pH sensor signal located in the acidification tank 10 to initiate the acid addition procedure, and the first metering dosing pump 11 passes the first pass from the first acid
  • the liquid medicine tank 12 takes the acid solution and injects the non-oxidizing acid liquid into the acidification tank 10 through the first acid-proof pipeline, and simultaneously starts the stirring motor in the acidification tank 10, so that the acid liquid is evenly dispersed until the preset pH value is reached, the first metering
  • the first channel of the dosing pump 11 is stopped by the acid solution program, and the sensor lifting platform raises the pH sensor probe;
  • the first metering dosing pump 11 extracts hydrofluoric acid from the second acid solution tank 13 through the second passage, and injects hydrofluoric acid into the acidification tank 10 through the second acid-resistant pipe until the preset hydrofluoric acid concentration is reached.
  • the pH adjusting unit and the pH adjusting unit can share a multi-channel metering dosing pump, that is, the first metering dosing pump 11 and the second metering dosing pump 4 are combined into one metering dosing pump of at least 3 channels.
  • the liquid flows into the adsorption enrichment device 17a through the pipeline.
  • the communication valve between the eluent device 15a and the adsorption enrichment device 17a is opened, and the waste liquid discharge valve at the bottom of the adsorption enrichment device 17a is opened.
  • the pure water in the rinsing device 15a is injected into the adsorption and enrichment device 17a through the pipeline for rinsing, and the sterilized waste liquid is discharged through the waste liquid discharge valve to complete the rinsing of the adsorption and enrichment device 17a;
  • the communication valve between the ejecting device 15a and the adsorption enrichment device 17a is closed, and the waste liquid discharge valve at the bottom of the adsorption enrichment device 17a is closed; the communication valve between the eluent device 15a and the ion exchange device 18a is opened, and the ions are simultaneously opened.
  • the waste liquid discharge valve at the bottom of the exchange device 18a, the pure water in the rinse device 15a is injected into the ion exchange device 18a through the pipe for flushing, and the flushed waste liquid is discharged through the waste liquid discharge valve to complete the flushing of the ion exchange device 18a;
  • the communication valve between the eluent device 15a and the ion exchange device 18a is closed, and the waste liquid discharge valve at the bottom of the ion exchange device 18a is closed, and the communication between the second dosing device 16a and the adsorption enrichment device 17a is opened.
  • the second dosing device 16a injects the alkali solution into the adsorption and enrichment device 17a through the alkali-resistant pipe, and the organic matter adsorbed by the resin is in the alkali solution Desorption occurs under the action, and the desorbed liquid flows into the ion exchange device 18a, and the hydrogen-type cation exchange resin in the ion exchange device 18a is discharged, and the discharged liquid is the desired extracted soil water-soluble organic concentrated solution, which is obtained after freeze-drying. Solid soil water dissolves organic matter.
  • FIG. 2 is a schematic structural view of a second embodiment of the apparatus for extracting soil water-dissolving organic matter provided by the present invention.
  • the organic matter extracting unit includes a rinsing device 15b and a third medicating device 16b.
  • a first-stage adsorption and enrichment device 17b a first-stage adsorption and enrichment device 17b, a first ion exchange device 18b, a second-stage adsorption and enrichment device 19b, and a second ion exchange device 20b;
  • the inlet of the first-stage adsorption and enrichment device 17b is connected to the outlet of the acidification tank 10, and the outlet thereof Connected to the inlet of the first ion exchange unit 18b and the inlet of the second adsorption unit 19b;
  • the outlet of the second adsorption unit 19b is connected to the inlet of the second ion exchange unit 20b;
  • the outlet of the dosing device 16b is connected to the inlet of the primary adsorption enrichment device 17b; the bottom of the primary adsorption enrichment device 17b, the first ion exchange device 18b, the secondary adsorption enrichment device 19b, and the second ion
  • the filtration process and the pH adjustment process of the soil organic matter are the same as those in the first embodiment, except that the organic matter extraction unit is different.
  • the organic matter extraction process is as follows: the organic acid liquid after the acidity and alkalinity adjustment is completed in the acidification tank 10.
  • the pipeline is sequentially flowed into the first-stage adsorption and enrichment device 17b and the second-stage adsorption and enrichment device 19b, and the organic matter is adsorbed on the resin;
  • the communication valve between the primary adsorption enrichment device 17b and the first ion exchange device 18b is closed, and the communication valve between the primary adsorption enrichment device 17b and the secondary adsorption enrichment device 19b is closed, and the shower is opened.
  • the communication valve between the washing device 15b and the first-stage adsorption and enrichment device 17b simultaneously opens the waste liquid discharge valve at the bottom of the first-stage adsorption and enrichment device 17b, and the pure water in the rinse device 15b is flushed through the pipeline to the first-stage adsorption and enrichment device.
  • the flushing waste liquid is discharged through the waste liquid discharge switch, completes the flushing of the first-stage adsorption and enrichment device 17b, and closes the waste liquid discharge switch at the bottom of the first-stage adsorption and enrichment device 17b, and simultaneously closes the elution device 15b and the first-stage adsorption and enrichment.
  • the flushed waste liquid is discharged through the waste liquid discharge valve, completes the flushing of the first ion exchange device 18b, closes the waste liquid discharge valve at the bottom of the first ion exchange device 18b, and simultaneously closes the rinse device 15b and the first ion exchange device 18b.
  • the first-stage adsorption and concentration device 17b and the second-stage adsorption and concentration device 19b are closed.
  • the communication valve between the first opening and the first ion exchange device 18b opens a communication valve between the first-stage adsorption and enrichment device 17b and the first ion exchange device 18b, and the third
  • the dosing device 16b injects the alkali solution into the first-stage adsorption and enrichment device 17b through the alkali-resistant pipe, and the dissolved organic matter adsorbed by the resin is desorbed by the action of the alkali solution, and the desorbed effluent is passed through the first ion exchange device 18b.
  • the hydrogen-type cation exchange resin in the first ion exchange device 18b should be ensured to be activated in a sufficient amount or in time, and the discharged liquid is marked as a first-stage adsorption-concentrating liquid;
  • the third dosing device 16b injects the alkali solution into the secondary adsorption and enrichment device 19b through the alkali-resistant pipe, and the dissolved organic matter adsorbed by the resin is under the action of the alkali solution Desorption occurs, and the desorbed effluent is discharged through the hydrogen-type cation exchange resin in the second ion exchange device 20b, and the hydrogen-type cation exchange resin in the second ion exchange device 20b is ensured to be activated in a sufficient amount or in time to be discharged.
  • the liquid is labeled as a secondary adsorption enrichment liquid;
  • the first-stage adsorption enrichment liquid and the second-stage adsorption enrichment liquid are combined, and after lyophilization, the high-purity soil is dissolved in the organic matter powder solid.
  • the first-stage adsorption and enrichment device 17b includes an adsorption column and a filler, and the filler is disposed in the adsorption column, and the filler is one or more of XAD-8 resin, DAX-8 resin and XAD-7 resin.
  • the first ion exchange device 18b includes an adsorption column and a filler, the filler is disposed in the adsorption column, and the filler is a hydrogen-type cation exchange resin;
  • the second adsorption-concentration device 19b includes an adsorption column and a filler, the filler is disposed in the adsorption column, the filler is XAD-4 resin, and the second ion exchange device 20b includes an adsorption column and a filler.
  • the filler is disposed in the adsorption column, and the filler is a hydrogen type cation exchange resin.
  • FIG. 3 is a schematic structural view of a third embodiment of an apparatus for extracting and purifying soil-dissolved organic matter provided by the present invention.
  • the organic matter extracting unit includes a rinsing device 15c and an organic solvent reagent box 16c.
  • a first-stage adsorption and enrichment device 17c a second-stage adsorption and enrichment device 18c; an inlet of the first-stage adsorption and enrichment device 17c is connected to an outlet of the acidification tank 10, and an outlet thereof is connected to an inlet of the second-stage adsorption and enrichment device 18c;
  • the outlet of the device 15c and the outlet of the organic solvent reagent tank 16c are all connected to the inlet of the first-stage adsorption and enrichment device 17c; the bottom of the first-stage adsorption and enrichment device 17c and the bottom of the second-stage adsorption and enrichment device 18c are provided with waste liquid discharge. valve.
  • the filtration process and the pH adjustment process of the soil organic matter are the same as those in the first embodiment, except that the soil hydrophobic organic matter extraction unit is different.
  • the extraction process of the dissolved organic matter in the hydrophobic water is as follows: the acidification tank 10 is completed.
  • the pH-adjusted organic matter liquid flows into the first-stage adsorption and enrichment device 17c and the second-stage adsorption and enrichment device 18c through the pipeline.
  • the outlet valve of the eluent device 15c is opened, and the pure water in the eluent device 15c is
  • the adsorption and enrichment device 17c performs flushing, and simultaneously opens the waste liquid discharge valve at the bottom of the first-stage adsorption and enrichment device 17c, and the flushed waste liquid is discharged through the waste liquid discharge valve;
  • the outlet valve of the elution device is closed, and the communication valve between the organic solvent reagent tank 16c and the first-stage adsorption and enrichment device 17c is opened, and the organic solvent reagent tank 16c passes through the organic-resistant pipeline to the first-stage adsorption and concentration device 17c.
  • injecting a non-polar volatile organic solvent the organic matter solution adsorbed by the resin is desorbed by a non-polar volatile organic solvent, and the collected effluent is marked as a first-stage adsorption and enrichment device eluent;
  • the communication valve between the organic solvent reagent tank 16c and the first-stage adsorption and enrichment device 17c is closed, and the communication valve between the elution device 15c and the second-stage adsorption and enrichment device 18c is opened.
  • the waste liquid discharge valve at the bottom of the second-stage adsorption and enrichment device 18c is opened; the pure water in the rinse device 15c is flushed through the pipeline to the second-stage adsorption and enrichment device 18c, and the rinsed waste liquid is discharged through the waste liquid discharge valve;
  • the communication valve between the elution device 15c and the secondary adsorption enrichment device 18c is closed, and the communication valve between the organic solvent solution tank 16c and the secondary adsorption enrichment device 18c is opened, and the organic solvent reagent tank 16c is resistant.
  • the organic pipeline injects a non-polar volatile organic solvent into the secondary adsorption and enrichment device 18c, and the organic matter solution adsorbed by the resin is desorbed by the non-polar volatile organic solvent, and the collected effluent is marked as secondary adsorption and enrichment.
  • the eluent of the first-stage adsorption enrichment device and the eluent of the second-stage adsorption enrichment device are combined, and after rotary evaporation, the soil organic solid powder is obtained by nitrogen blowing or natural evaporation.
  • FIG. 4 is a schematic structural view of a fourth embodiment of the apparatus for extracting and purifying soil-dissolved organic matter provided by the present invention
  • the organic matter extracting unit includes a rinsing device 15d and an organic solvent reagent box. 16d, the adsorption and enrichment device 17d; the inlet of the adsorption and enrichment device 17d is connected to the outlet of the acidification tank 10; the outlet of the eluent device 15d and the outlet of the organic solvent reagent tank 16d are all connected to the inlet of the adsorption and enrichment device 17d; A waste liquid discharge valve is provided at the bottom of the collecting device 17d.
  • the filtration process and the pH adjustment process of the soil organic matter are the same as those in the first embodiment, except that the organic matter extraction unit is different.
  • the organic matter extraction process is as follows: the organic acid liquid after the acidity and alkalinity adjustment is completed in the acidification tank 10. Flowing into the adsorption enrichment device 17d through the pipeline, the organic matter is adsorbed on the resin;
  • the outlet valve of the rinsing device 15d is opened, the pure water in the rinsing device 15d is flushed to the adsorption and enrichment device 17d, and the waste liquid discharge valve at the bottom of the adsorption and enrichment device 17d is opened, and the sterilized waste liquid is passed through.
  • the waste liquid discharge valve is discharged;
  • the outlet valve of the rinsing device 15d is closed, the communication valve between the organic solvent solution tank 16d and the adsorption and enrichment device 17d is opened, and the organic solvent reagent tank 16d is injected into the adsorption and enrichment device 17d through the organic-resistant pipeline.
  • a volatile organic solvent the organic matter solution adsorbed by the resin is desorbed by the action of a non-polar volatile organic solvent, and the collected effluent is marked as an eluent of the adsorption enrichment device;
  • the adsorption-enrichment device 17d includes an adsorption column and a filler, and the filler is disposed in the adsorption column, and the filler is one or more of XAD-8 resin, DAX-8 resin, and XAD-7 resin.
  • the pH adjustment process in the pH adjustment unit and the pH adjustment unit is a fully automated process, which saves labor, reduces production costs, and has a high precision of the pH value to be prepared, and the process efficiency of the preparation process is also high.
  • the agitator motor is turned on to agitate the liquid in the reaction vessel 1 and the acidification tank 10, so that the agent flowing therein is uniformly dispersed, and the local pH value is prevented from being high or low.
  • the filter purification unit uses a filter membrane as a disposable filter membrane, and the filter membrane is stored and used as required, but a silicon-containing filter membrane such as a glass fiber filter membrane cannot be used.

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Abstract

L'invention concerne un appareil d'extraction et de purification de matières organiques dissoutes hydrophobes de sol, comprenant une cuve de réaction (1), une unité de réglage de pH, une unité de filtration et de purification, une cuve d'acidification (10), une unité de réglage d'acidité et d'alcalinité, une unité d'extraction de matière organique et un système de commande maître (6) ; les procédés de réglage de pH réalisés par l'unité de réglage de pH et l'unité de réglage d'acidité et d'alcalinité sont entièrement automatiques ; l'appareil d'extraction et de purification de matière organique dissoute hydrophobe de sol possède une structure simple, un fonctionnement pratique, un degré élevé d'automatisation et permet efficacement d'obtenir une solution de matière organique dissoute hydrophobe de sol à haute concentration à grande échelle afin de préparer une matière organique dissoute hydrophobe de sol solide.
PCT/CN2017/101705 2017-02-08 2017-09-14 Appareil d'extraction et de purification de matières organiques dissoutes hydrophobes de sol WO2018145457A1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
CN201710069420.9A CN106932259B (zh) 2017-02-08 2017-02-08 一种用于提取土壤憎水溶解有机质的装置
CN201710069420.9 2017-02-08
CN201710069146.5A CN106885721B (zh) 2017-02-08 2017-02-08 一种采用两级碱洗式提取土壤憎水有机质的设备
CN201710069146.5 2017-02-08

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JP2015226866A (ja) * 2014-05-30 2015-12-17 栗田工業株式会社 イオン交換装置供給水の評価方法及び運転管理方法
CN106315956A (zh) * 2016-10-21 2017-01-11 中国环境科学研究院 两级碱洗式水体溶解有机质的提取设备
CN106336041A (zh) * 2016-10-21 2017-01-18 中国环境科学研究院 反渗透与一级树脂联用提取淡水富里酸的装置
CN106336515A (zh) * 2016-10-21 2017-01-18 中国环境科学研究院 一种采用两级树脂联用提取水体富里酸的设备
CN106365354A (zh) * 2016-10-21 2017-02-01 中国环境科学研究院 一种淡水水体中憎水性溶解腐殖酸提取装置
CN106885721A (zh) * 2017-02-08 2017-06-23 中国环境科学研究院 一种采用两级碱洗式提取土壤憎水有机质的设备
CN106932259A (zh) * 2017-02-08 2017-07-07 中国环境科学研究院 一种用于提取土壤憎水溶解有机质的装置

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2003082748A1 (fr) * 2002-04-03 2003-10-09 Orica Australia Pty Ltd Procede de regeneration de resines echangeuses d'ions
JP2015226866A (ja) * 2014-05-30 2015-12-17 栗田工業株式会社 イオン交換装置供給水の評価方法及び運転管理方法
CN106315956A (zh) * 2016-10-21 2017-01-11 中国环境科学研究院 两级碱洗式水体溶解有机质的提取设备
CN106336041A (zh) * 2016-10-21 2017-01-18 中国环境科学研究院 反渗透与一级树脂联用提取淡水富里酸的装置
CN106336515A (zh) * 2016-10-21 2017-01-18 中国环境科学研究院 一种采用两级树脂联用提取水体富里酸的设备
CN106365354A (zh) * 2016-10-21 2017-02-01 中国环境科学研究院 一种淡水水体中憎水性溶解腐殖酸提取装置
CN106885721A (zh) * 2017-02-08 2017-06-23 中国环境科学研究院 一种采用两级碱洗式提取土壤憎水有机质的设备
CN106932259A (zh) * 2017-02-08 2017-07-07 中国环境科学研究院 一种用于提取土壤憎水溶解有机质的装置

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