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WO2018145458A1 - Équipement destiné à être utilisé pour extraire de l'acide humique du sol et procédé de fabrication de l'équipement - Google Patents

Équipement destiné à être utilisé pour extraire de l'acide humique du sol et procédé de fabrication de l'équipement Download PDF

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Publication number
WO2018145458A1
WO2018145458A1 PCT/CN2017/101707 CN2017101707W WO2018145458A1 WO 2018145458 A1 WO2018145458 A1 WO 2018145458A1 CN 2017101707 W CN2017101707 W CN 2017101707W WO 2018145458 A1 WO2018145458 A1 WO 2018145458A1
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Prior art keywords
acid
tank
acidification tank
liquid
outlet
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PCT/CN2017/101707
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English (en)
Chinese (zh)
Inventor
白英臣
吴丰昌
王彬
魏源
宋凡浩
赵天慧
朱焰
Original Assignee
中国环境科学研究院
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Priority claimed from CN201710069198.2A external-priority patent/CN106893114B/zh
Priority claimed from CN201710069441.0A external-priority patent/CN106905382B/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 WO2018145458A1 publication Critical patent/WO2018145458A1/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
    • G01N1/34—Purifying; Cleaning

Definitions

  • the invention relates to the field of humic acid extraction, in particular to an apparatus for extracting soil humic acid and a preparation method thereof.
  • Humic acid is a macromolecular organic mixture formed by complex physical, chemical and biological processes of animal and plant residues. It is widely found in environmental media such as soil, water and sediment. Humic acid can be dissolved in alkaline and neutral solutions. Insoluble in acid accounts for 60-80% of total soil organic matter, which is the most important component of soil organic matter.
  • Humic acid plays an important role in agriculture and the environment. At present, humic acid can stimulate the growth of wheat, tomato, cotton and other crops at seedling stage, improve soil pH environment through its own acidity, and reduce soil compaction. Humic acid also increases the amount of microorganisms and soil enzymes in the soil, providing a carbon source for crop growth. By combining with soil nutrients, humic acid can increase the nutrient storage and nutrient availability of the soil. In addition, humic acid can interact with toxic heavy metal ions and organic pollutants in the environment to change the migration, transformation and bioavailability of pollutants. Therefore, the study of soil humic acid is of great significance.
  • Chinese invention patent (201510586520.X: a method for extracting small molecule humic acid from soil by XAD resin) discloses a method for extracting small molecule humic acid from soil by XAD resin, and the extraction step is as follows:
  • Step b Extraction of soil humic acid by sodium pyrophosphate:
  • step a Add deionized water to the soil sample in step a to achieve a solid-liquid ratio of 1:5 to 1:15, adjust the pH of the solution to 1.0-3.0 with HCl and NaOH, and then add HCl solution to the ratio of solid to liquid 1:10 , stirring continuously for 4-8h, then standing for 20-40h, centrifugally separating to obtain solid soil sample 1;
  • Step c Extraction of soil humic acid by sodium hydroxide:
  • Step d remove fulvic acid impurities from humic acid:
  • the humic acid sample was repeatedly operated according to the method in the step d until the total organic carbon content in the supernatant after centrifugation was ⁇ 0.5 mg/L, and the obtained solid was collected and labeled as a purified humic acid sample;
  • Step e Separation of macromolecular humic acid from small molecule humic acid:
  • Step f Removal of silicon-containing minerals from small molecule humic acids:
  • Step g Enrichment and extraction of small molecule humic acid:
  • the method for extracting soil humic acid disclosed in the above invention mainly utilizes the adsorption characteristics of XAD-8 resin to adsorb small molecule humic acid to XAD-8 branches at a specific pH value, and then through analysis, ion exchange and freezing. Drying, finally obtaining small molecules of humic acid, this method relies on laboratory and a large number of manual operating conditions, the operation process is complicated, the degree of automation is low, the extraction amount of humic acid is small, and the method is not suitable for large-scale Sample collection;
  • the humic acid extraction method disclosed in this paper is greatly affected by the human influence operation, and the humic acid in the soil cannot be extracted in a large amount, and the implementation is not good.
  • the present invention provides a device for extracting soil humic acid, which can realize efficient extraction of soil humic acid, and is convenient to operate and high in automation.
  • the present invention provides an apparatus for extracting soil humic acid, comprising a reaction kettle, a pH adjusting unit, a filtration purification unit, a first acidification tank, a first pH adjustment unit, and a humic acid extraction unit. And total control unit;
  • 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 first acidification tank, An inlet of the first acidification tank is connected to an outlet of the first pH unit; an outlet of the first acidification tank is connected to an inlet of the humic acid extraction unit;
  • the humic acid extraction unit includes a hydrophobic humic acid extraction unit and a humic acid full component extraction unit;
  • the pH adjusting unit and the first pH adjusting unit are all connected to the overall control unit.
  • the hydrophobic humic acid extraction unit comprises an adsorption enrichment unit, a second acidification tank, a second pH adjustment unit, a leaching device, a second filter and a liquid reservoir; an inlet of the adsorption enrichment unit and An outlet of the first acidification tank is connected, an outlet of the adsorption enrichment unit is connected to an inlet of the second acidification tank; an inlet of the second acidification tank is further connected to an outlet of the second pH adjustment unit, a second pH adjustment unit is coupled to the overall control unit; an outlet of the second acidification tank is coupled to an inlet of the second filter, and an inlet of the second filter is further coupled to an outlet of the rinsing device An outlet of the second filter is connected to an inlet of the liquid reservoir, and a bottom of the liquid reservoir is provided with a waste liquid discharge valve.
  • the second filter comprises a sample chamber, a filter membrane and a sand core
  • the filter membrane is disposed in the sample chamber and supported by a sand core
  • the filter membrane has a pore diameter ranging from 0.1 to 0.7 ⁇ m. .
  • the adsorption and enrichment unit comprises a first rinsing device, a second medicating device and an adsorption and enrichment device, and the outlet of the first rinsing device and the outlet of the second medicating device are both rich in the adsorption Inlet connection of the collection device, the adsorption enrichment
  • the inlet of the apparatus is also connected to the outlet of the first acidification tank, the outlet of the adsorption enrichment unit is connected to the inlet of the second acidification tank, and the bottom of the adsorption enrichment apparatus is 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 second pH adjustment unit comprises a third acid solution tank, a fourth acid solution tank and a third metering dosing pump; the third metering dosing pump inlet and the third acid solution respectively
  • An outlet of the reagent tank, an outlet connection of the fourth acid solution tank, an outlet of the third metering dosing pump is connected to an inlet of the second acidification tank; the third acid liquid medicine tank and the fourth acid liquid
  • the kits are arranged side by side.
  • the humic acid component extraction unit comprises a rinsing device, a second filter and a liquid reservoir; an outlet of the rinsing device is connected to an inlet of the second filter, the second filtering The outlet of the device is connected to the inlet of the liquid reservoir; the second filter comprises a sample chamber, a filter membrane and a sand core, the filter membrane is disposed in the sample chamber and supported by a sand core, the filter membrane
  • the pore size ranges from 0.1 to 0.7 ⁇ m.
  • the pH adjusting unit comprises a first metering dosing pump and a first dosing device, and a first metering dosing pump is disposed between the first dosing device and the reaction kettle, the first metering An inlet of the dosing pump is coupled to an outlet of the first dosing device, and an outlet of the first metered dosing pump is coupled to an inlet of the reaction vessel.
  • the reaction vessel is provided with a soil storage chamber supported by the support and disposed in the reaction kettle; the outer wall of the soil storage chamber is provided with a plurality of holes having a pore diameter of less than 1 mm.
  • the filtration purification unit comprises a first filter and a vacuum pump, an inlet of the first filter is connected to an outlet of the reaction kettle through a pipe, an outlet of the first filter and the first acidification tank An inlet connection; the vacuum pump is coupled to the first acidification tank.
  • the pipeline between the reaction vessel and the first filter extends into the reaction vessel, and the height of the pipeline extending into the reactor is 1/20-1/10 of the height of the reactor, and A protective cover is provided, and the protective cover is provided with a plurality of holes having a hole diameter of 1 mm.
  • 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.
  • a pipe between the first filter and the first acidification tank extends into the first acidification tank, and the pipeline extending into the first acidification tank is located above the liquid level in the first acidification tank
  • the suction ports of the vacuum pump are respectively located above the liquid level in the first acidification tank and above the liquid level in the liquid reservoir.
  • the first pH adjustment unit comprises a pH sensor, a stirrer, a first acid solution tank, a second acid solution tank, and a second metering dosing pump; the pH sensor and the agitator are disposed in the first 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 second metering medicine pump is respectively connected with the outlet of the first acid liquid medicine tank and the second acid liquid medicine tank The outlet connection, the outlet of the second metering dosing pump is connected to the inlet of the first acidification tank.
  • the total control system comprises a control unit and a touch screen, and the control unit is respectively connected with a pH sensor, a stirrer, a liquid level sensor, a first metering dosing pump, and a second metering dosing in the reaction kettle.
  • a method for extracting soil humic acid by using a device for extracting soil humic acid comprising the following steps:
  • the first 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 lye into the reaction kettle through the first alkali-resistant alkali pipeline, and simultaneously starts The stirring motor in the reaction kettle uniformly disperses the alkali liquid until the preset pH value is reached, and the first metering dosing pump stops working;
  • the second metering dosing pump receives the pH sensor signal located in the acidification tank to initiate the acid addition procedure, and the second metering dosing pump passes the first channel from the first acid
  • the liquid medicine tank extracts the acid solution into the acidification tank through the first acid-proof pipeline, and simultaneously starts the non-oxidizing acid liquid in the acidification tank, and starts the stirring motor in the acidification tank to uniformly disperse the acid liquid until the preset pH value is reached, the second metering dosing pump
  • the first channel plus acid program stops working, and the sensor lifting platform raises the pH sensor probe;
  • the second 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 second metering dosing pump stops working;
  • the outlet valve of the first acidification tank is opened, and the communication valve between the first acidification tank and the adsorption enrichment device is opened, and the first acidification tank and the second filter are closed.
  • the valve is connected, the liquid in the first acidification tank flows into the adsorption enrichment device through the pipeline, and after the adsorption is completed, the switch between the first elution device and the adsorption enrichment device is opened, and the pure water in the first elution device is flushed and adsorbed through the pipeline.
  • Enriching the device, and opening the waste liquid discharge valve at the bottom of the adsorption and enrichment device flushing the waste liquid through the pipeline, completing the flushing of the adsorption and enrichment device, and closing the waste liquid discharge valve;
  • the outlet valve of the leaching device is closed, and the outlet valve of the second medicating device is opened, and the second medicinal device injects the alkali solution into the adsorption and enrichment device through the second alkali-resistant pipe, and is adsorbed by the resin.
  • the natural dissolved organic matter is desorbed by the action of the lye, and the desorbed liquid flows into the second acidification tank through the pipeline;
  • the third metering dosing pump receives the pH sensor signal located in the acidification tank to initiate the acid addition procedure, and the third metering dosing pump passes the third channel from the third acid
  • the liquid medicine tank extracts the acid solution into the acidification tank through the third acid-proof pipeline, and simultaneously starts the stirring motor in the acidification tank, so that the acid liquid is evenly dispersed until the preset pH value is reached, and the third metering dosing pump
  • the third channel plus acid program stops working, and the sensor lifting platform raises the pH sensor probe;
  • the third metering dosing pump draws hydrofluoric acid from the fourth acid solution tank through the fourth passage into the acidification tank through the fourth acid-proof pipeline until the preset hydrofluoric acid concentration is reached, and the third metering dosing pump stops working;
  • the outlet valve of the second acidification tank is closed, and the outlet valve of the eluent device is opened.
  • the pure water in the eluent device flows into the second filter through the pipeline, and the filter membrane is washed, and the rinse liquid directly flows into the liquid.
  • the liquid in the liquid reservoir is directly discharged through the discharge valve, and the organic matter remaining on the filter membrane is the soil humic acid to be extracted.
  • the lye in the first dosing device is a saturated or near-saturated strong alkali solution
  • the first alkali-resistant pipeline is required to withstand a saturated strong alkali
  • the alkali-resistant pipeline is required to withstand 0.001-0.5.
  • a strong base of mol/L
  • a pH of the liquid in the reaction vessel is preset to be 10-14
  • a lye in the second dosing device is a 0.1 mol/L strong alkali solution, and the second alkali resistance
  • the pipeline is required to withstand a strong base of 0.5 mol/L.
  • the first acid-resistant pipeline is required to withstand a non-oxidizing strong acid of 10 mol/L; the second acid-resistant pipeline is required to withstand 6 mol/L of hydrofluoric acid; and the hydrofluoric acid in the first acidification tank is pre-treated
  • concentration is set to 0.01-1 mol/L; the pH of the liquid in the first acidification tank is preset to be 0.5-1.5.
  • the third 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; and the hydrofluoric acid in the first acidification tank is pre-treated
  • the concentration is set to 0.01-1 mol/L; the pH of the liquid in the first acidification tank is preset to be 0.5-1.5.
  • a method for extracting whole components of soil humic acid by using a device for extracting soil humic acid comprising the following steps:
  • the first metering dosing pump receives the pH sensor signal in the reaction kettle to start the lye addition procedure, and the dosing device injects the alkali solution into the reaction kettle through the strong alkali resistant pipeline, and simultaneously starts the reaction kettle. Stir the motor to evenly disperse the lye until the preset pH value is reached, and the first metering dosing pump stops working;
  • the second metering dosing pump receives the pH sensor signal in the first acidification tank to initiate the acid addition procedure, and the second metering dosing pump draws the acid from the first acid solution tank through the first channel
  • the liquid is injected into the acidification tank through the first acid-proof pipeline, and the stirring motor is started in the first acidification tank, so that the acid liquid is evenly dispersed until the preset pH value is reached, and the second metering dosing pump first passage
  • the acid solution program stops working, and the sensor lifter raises the pH sensor probe;
  • the second metering dosing pump draws hydrofluoric acid from the second acid solution tank through the second passage into the first acidification tank through the second acid-resistant pipeline until the preset hydrofluoric acid concentration is reached, and the second metering dosing pump stops. jobs;
  • the outlet valve of the first acidification tank is opened, and the communication valve between the first acidification tank and the second filter is opened, and the communication valve between the first acidification tank and the adsorption enrichment device is closed.
  • the vacuum pump is started, and the pressure is applied by the vacuum pump, and the organic matter solution in the acidification tank is filtered through the filter membrane in the second filter, and the whole component of the humic acid is trapped on the filter membrane, and the impurities flow into the liquid reservoir;
  • the outlet valve of the first acidification tank is closed, and the outlet valve of the leaching device is opened, and the pure water in the leaching device flows into the second filter through the pipe, and the filter membrane is washed, and the rinsing liquid flows directly In the liquid reservoir, the liquid in the liquid reservoir is directly discharged through the discharge valve, and the organic matter remaining on the filter membrane is the entire component of the soil humic acid to be extracted.
  • the lye in the first dosing device is a saturated or near-saturated strong alkali solution
  • the first alkali-resistant alkali pipeline is required to withstand a saturated strong alkali
  • the first alkali-resistant alkali pipeline is required to withstand 0.001 - 0.5 mol / L of strong base
  • the pH of the liquid in the reactor is preset to 10-14
  • the first acid-resistant pipeline is required to withstand 10 mol / L of non-oxidizing strong acid
  • the second acid-resistant pipeline requirements It can withstand 6 mol/L of hydrofluoric acid
  • the preset concentration of hydrofluoric acid in the first acidification tank is 0.01-1 mol/L
  • the pH of the liquid in the first acidification tank is preset to 0.5-1.5.
  • the device for extracting soil humic acid has the advantages of simple structure, convenient operation and high degree of automation, and can conveniently and effectively separate the hydrophobic humic acid and other impurities, and can extract a large amount of soil drowning water. Soluble humic acid can also extract a large amount of soil humic acid components, which largely meets the customer's demand for different soil humic acid components;
  • the bottom of the reaction kettle, the first acidification tank and the second acidification tank are all funnel-shaped, and a filter cover is arranged outside the pipeline extending into the reaction kettle and the first acidification tank, and the height of the pipeline extending into the reaction kettle is taken as the reaction kettle.
  • the height of 1/20-1/10, the height of the pipe extending into the first acidification tank is 1/30-1/20 of the height of the first acidification tank, and a filter cover is arranged outside the pipeline extending into the first acidification tank. It can ensure the maximum collection of humic acid, improve the efficiency of the device, and effectively prevent the impurities particles from being mixed into the sample, thus ensuring the purity of the extract;
  • the pH adjustment, the first pH adjustment unit, and the second pH adjustment unit are all fully automatic, saving labor, and the pH of the adjusted pH is relatively high; the first acid solution tank and the second acid solution
  • the tank shares a metering dosing pump, and the third acid liquid medicine tank and the fourth acid liquid medicine tank share a metering dosing pump, and a further optimized pH adjusting unit, a first pH adjusting unit and a second pH adjusting unit can share one
  • the multi-channel metering dosing pump further reduces the production cost; the first acidizing tank, the second acidifying tank and the liquid storage share a vacuum pump, which reduces the production cost;
  • the inert gas inlet and outlet are reserved in the reactor, and the oxidation of the whole component of the humic acid in the soil under strong alkaline conditions can be effectively suppressed by introducing an inert gas such as nitrogen or helium in the production.
  • FIG. 1 is a process flow diagram of an apparatus for extracting soil humic acid provided by the present invention.
  • FIG. 1 is a process flow diagram of an apparatus for extracting soil humic acid provided by the present invention.
  • the apparatus for extracting whole components of soil humic acid provided by the invention comprises a reaction kettle 1, a pH adjusting unit, a filtering and purifying unit, a first acidizing tank 8, a first pH adjusting unit, a humic acid extracting unit and a total control unit 6
  • the humic acid extraction unit comprises a hydrophobic humic acid extraction unit and a humic acid full component extraction unit; wherein the reaction vessel 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, 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;
  • the pH adjusting unit comprises a first metering dosing pump 4 and a first dosing device 5;
  • the filter purification unit includes a first filter 7 and a vacuum pump 12, wherein the first filter 7 includes a sample chamber 71, a filter membrane 72 and a sand core 73, and the filter membrane 72 is disposed in the sample chamber 71 and supported by the sand core 73;
  • the first pH adjustment unit includes a metering dosing pump 9, a first acid solution tank 10 and a second acid tank 11;
  • the hydrophobic humic acid extraction unit comprises an adsorption enrichment unit, a second pH adjustment unit, a second acidification tank 22, and a rinse device 13.
  • the second filter 14 and the liquid reservoir 15, the adsorption enrichment unit comprises a first elution device 16, a second dosing device 17, and an adsorption enrichment device 18;
  • the second pH adjustment unit comprises a third acid solution reagent tank 20.
  • the humic acid component extracting unit comprises a rinsing device 13, a second filter 14, and a liquid reservoir 15; wherein the second filter 14
  • the sample chamber 141, the filter membrane 142 and the sand core 143 are disposed.
  • the filter membrane 142 is disposed in the sample chamber 141 and supported by the sand core 143.
  • the total control unit 6 is mainly controlled by an automatic control, wherein the centralized control operation is uniformly performed in the control cabinet. , the entire system can be automatically controlled and manually operated.
  • the first dosing device 5 is connected to the reaction kettle 1 by a first metering dosing pump 4, the inlet of the first metering dosing pump 4 is connected to the first dosing device 5, and the outlet thereof is connected to the reaction vessel 1;
  • the outlet of 1 is connected to the inlet of the first filter 7, and the connecting pipe between the reaction vessel 1 and the first filter 7 is inserted into the reaction vessel 1, and the height of the pipe extending into the reactor is taken as 1 of the height of the reactor 1.
  • the protective cover is disposed outside, and the protective cover is provided with a plurality of holes having a hole diameter of 1 mm;
  • the outlet of the first filter 7 is connected to the first acidification tank 8, and the outlet of the vacuum pump 12 is placed In the cavity of the first acidification tank 8;
  • the first acid liquid medicine tank 10 and the second acid liquid medicine tank 11 are arranged side by side, and the second metering dosing pump 9 is disposed in the first acid liquid medicine tank 10 and the second acid liquid medicine
  • the inlet of the second metering dosing pump 9 is connected to the outlet of the first acid solution tank 10, the outlet of the second acid solution tank 11, the outlet of the second metering dosing pump 9 and the first acidification tank.
  • the inlet of the first acidification tank 8 is connected to the inlet of the adsorption enrichment device 18 and the inlet of the second filter 14 respectively; adsorption and enrichment
  • the inlet of 18 is also connected to the outlet of the first rinse device 16, the outlet of the second dosing device 17, the outlet of the adsorption enrichment device 18 is connected to the inlet of the second acidification tank 22, and the bottom of the adsorption enrichment device is provided with waste.
  • the outlet of the third acid solution tank 20 and the outlet of the fourth acid tank 21 are both connected to the inlet of the third metering dosing pump 19, and the outlet of the third metering dosing pump 19 is connected to the inlet of the second acidification tank 22;
  • the outlet of the second acidification tank 22 is connected to the inlet of the second filter 14;
  • the inlet of the second filter 14 is also connected to the outlet of the rinsing device 13, and the outlet of the second filter 14 is connected to the inlet of the liquid reservoir 15;
  • the outlets of 12 are respectively placed in the chamber of the first acidification tank 8 and the chamber of the liquid reservoir 15; the bottom of the liquid reservoir 15 is provided with a waste liquid discharge valve.
  • the total control system 6 comprises 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 sensor, the pH sensor, the first metering dosing pump 4, the second metering dosing pump 9, the vacuum pump 12 connections.
  • 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 independently operated control cabinet, as well as electrical switches and electrical components. They are all concentrated in the control cabinet, and the power switch and the electric control cabinet door interlock protection can achieve the effects of dustproof, fast heat dissipation and easy installation.
  • the reaction vessel 1 An inert gas is introduced into the reaction vessel 1, and the pH adjusting unit is activated under the protection of an inert gas.
  • the first 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
  • the alkaline liquid is injected into the reaction vessel 1 through the alkali-resistant pipeline, and the stirring motor in the reaction vessel 1 is started to uniformly disperse the alkali liquid until the preset pH value is reached, and the first metering dosing pump 4 stops working.
  • 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 12 is started, and the pressure is applied by the vacuum pump 12.
  • the solution in the reaction vessel 1 flows into the first acidification tank 8 through the first filter 7, and the alkali-insoluble impurities are removed by the filter to remove impurities. After the liquid flows through the filter into the first acidification tank 8;
  • the first pH adjustment unit is activated to perform the initial adjustment of the pH
  • the second metering dosing pump 9 receives the pH sensor signal in the first acidification tank 8 to initiate the acid addition procedure
  • the second metering dosing pump 9 passes through the first channel.
  • the acid solution tank 10 takes the acid solution and injects the non-oxidizing acid solution into the first acidification tank 8 through the first acid-resistant pipeline, and simultaneously starts the stirring motor in the first acidification tank, so that the acid liquid is uniformly dispersed until the preset pH is reached. Value, the second metering dosing pump 9 first channel plus acid program stops working, the sensor lifting platform raises the pH sensor probe;
  • the second metering dosing pump 9 draws hydrofluoric acid from the second acid solution tank 11 through the second passage into the acidification tank through the second acid-proof pipeline until the preset hydrofluoric acid concentration is reached, and the second metering dosing pump 9 stop working;
  • the outlet valve of the first acidification tank 8 is opened, and the communication valve between the first acidification tank 8 and the adsorption enrichment device 18 is opened, and the first acidification tank 8 and the second filter 14 are closed.
  • the communication valve between the first acidification tank 8 flows into the adsorption enrichment device 18 through the pipeline.
  • the first rinse device 16 is opened and the adsorption is enriched.
  • the switch between the first rinsing device 16 and the concentrating and accumulating device 18 is turned off, and the switch between the second medicinal device 17 and the concentrating and accumulating device 18 is opened, and the second medicating device is opened. 17 through the second alkali-resistant pipeline into the adsorption and enrichment device 18 into the lye, the natural dissolved organic matter adsorbed by the resin is desorbed by the action of the lye, the desorbed liquid flows into the second acidification tank 22 through the pipeline;
  • the second pH adjustment unit is activated to perform the re-adjustment of the pH
  • the third metering dosing pump 19 receives the pH sensor signal located in the second acidification tank 22 to initiate the acid addition procedure
  • the third metering dosing pump 19 passes through the third channel from the third
  • the acid solution tank 20 takes the acid solution and injects the non-oxidizing acid liquid into the acidification tank through the third acid-proof pipeline, and simultaneously starts the stirring motor in the acidification tank, so that the acid liquid is evenly dispersed until the preset pH value is reached, and the third metering is added.
  • the third channel plus acid program of the medicine pump 19 stops working, and the sensor lifting platform raises the pH sensor probe;
  • the third metering dosing pump 19 draws hydrofluoric acid from the fourth acid solution tank 21 through the fourth passage into the acidification tank through the fourth acid-proof pipeline until the preset hydrofluoric acid concentration is reached, and the third metering dosing pump 19 stop working;
  • the outlet valve of the second acidification tank 22 is opened, and the vacuum pump 12 is started, and the pressure is applied by the vacuum pump 12, and the organic matter solution in the second acidification tank 22 is filtered through the membrane in the second filter, and the water is drained.
  • the humic acid is trapped on the filter membrane and the impurities flow into the liquid reservoir;
  • the outlet valve of the second acidification tank 22 is closed, the outlet valve of the second rinsing device 13 is opened, and the pure water in the second rinsing device 13 flows into the second filter 14 through the pipe to rinse the filter 142.
  • the rinsing liquid directly flows into the liquid reservoir 15, and the liquid in the liquid reservoir 15 is directly discharged through the discharge valve, and the organic matter remaining on the filter membrane 142 is the soil humic acid to be extracted, and the soil is drained. Extraction of humic acid.
  • the pH adjustment process in the pH adjustment unit, the first pH adjustment unit, and the second pH adjustment unit are all fully automated processes, saving labor, reducing production costs, and preparing the pH value with high precision.
  • the process of preparation is also more efficient.
  • the agitator motor is turned on to agitate the liquid in the reaction vessel 1, the first acidification tank 8, and the second acidification tank 22, so that the acid solution flowing therein is uniformly dissolved in the water, thereby avoiding the local pH value. High or low.
  • the outlet valve of the first acidification tank 8 is opened, and the communication valve between the first acidification tank 8 and the second filter 14 is opened, and the first acidification tank 8 and the adsorption enrichment device 18 are closed.
  • the communication valve is activated to start the vacuum pump 12, and the pressure is applied by the vacuum pump 12.
  • the solution in the first acidification tank 8 is filtered through the filter 142 in the second filter 8, and the entire component of the humic acid is trapped on the filter membrane. Flowing into the liquid reservoir 15;
  • the outlet valve of the first acidification tank 8 is closed, the outlet valve of the rinsing device 13 is opened, and the pure water in the rinsing device 13 is injected into the second filter 14 through the pipeline to the crude rot in the second filter 14.
  • the acid is washed, the rinsing liquid flows directly into the liquid reservoir 15, the liquid in the liquid reservoir is directly discharged through the discharge valve, and the whole component of the soil humic acid is left on the filter membrane to complete the whole component of the soil humic acid. extract.
  • the filter membrane used in the first filter is a disposable filter membrane, the filter membrane needs to be able to withstand 1 mol/L strong alkali, 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;
  • the filter used in the second filter is a disposable filter membrane, and the filter membrane needs to be able to withstand 0.5 mol/L of strong acid, 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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  • Engineering & Computer Science (AREA)
  • Biomedical Technology (AREA)
  • Molecular Biology (AREA)
  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
  • Processing Of Solid Wastes (AREA)
  • Water Treatment By Sorption (AREA)

Abstract

La présente invention concerne un équipement destiné à être utilisé pour extraire de l'acide humique du sol, comprenant une cuve de réaction (1), une unité de régulation de pH, une unité de filtration et de purification, un premier récipient d'acidification (8), une première unité de régulation d'acidité/alcalinité, une unité d'adsorption et d'enrichissement, un second récipient d'acidification (22), une seconde unité de régulation d'acidité/alcalinité, une unité d'extraction d'acide humique et une unité de commande générale (6). L'unité d'extraction d'acide humique comprend une unité d'extraction tout composant et une unité d'extraction d'acide humique hydrophile. L'équipement destiné à être utilisé pour extraire de l'acide humique du sol est structurellement simple et pratique à utiliser, a un degré élevé d'automatisation, permet une séparation pratique et efficace d'acide humique hydrophile à partir d'autres impuretés, non seulement est capable d'extraire une grande quantité de tous les composants d'acide humique, mais aussi peut extraire une grande quantité d'acide humique hydrophile dissous, et améliore l'utilisation de l'acide humique extrait.
PCT/CN2017/101707 2017-02-08 2017-09-14 Équipement destiné à être utilisé pour extraire de l'acide humique du sol et procédé de fabrication de l'équipement WO2018145458A1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
CN201710069198.2A CN106893114B (zh) 2017-02-08 2017-02-08 一种用于提取土壤腐殖酸全组分的设备
CN201710069198.2 2017-02-08
CN201710069441.0 2017-02-08
CN201710069441.0A CN106905382B (zh) 2017-02-08 2017-02-08 一种提取土壤憎水腐殖酸的装置

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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004325425A (ja) * 2003-04-28 2004-11-18 Silk Kogei:Kk 水中フルボ酸の粉末標準試料の製造方法
CN101033241A (zh) * 2007-04-29 2007-09-12 晋城市炬坤生物科技有限公司 一种高纯度腐植酸的制备方法
CN103131023A (zh) * 2013-02-06 2013-06-05 何林 一种腐植酸的提取新工艺
CN105043838A (zh) * 2015-09-16 2015-11-11 中国环境科学研究院 一种水体中富里酸亚组分的分级提取方法
CN105203374A (zh) * 2015-09-16 2015-12-30 中国环境科学研究院 一种xad树脂提取土壤中小分子腐殖酸的方法
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
CN106893114A (zh) * 2017-02-08 2017-06-27 中国环境科学研究院 一种用于提取土壤腐殖酸全组分的设备
CN106905382A (zh) * 2017-02-08 2017-06-30 中国环境科学研究院 一种提取土壤憎水腐殖酸的装置

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004325425A (ja) * 2003-04-28 2004-11-18 Silk Kogei:Kk 水中フルボ酸の粉末標準試料の製造方法
CN101033241A (zh) * 2007-04-29 2007-09-12 晋城市炬坤生物科技有限公司 一种高纯度腐植酸的制备方法
CN103131023A (zh) * 2013-02-06 2013-06-05 何林 一种腐植酸的提取新工艺
CN105043838A (zh) * 2015-09-16 2015-11-11 中国环境科学研究院 一种水体中富里酸亚组分的分级提取方法
CN105203374A (zh) * 2015-09-16 2015-12-30 中国环境科学研究院 一种xad树脂提取土壤中小分子腐殖酸的方法
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
CN106893114A (zh) * 2017-02-08 2017-06-27 中国环境科学研究院 一种用于提取土壤腐殖酸全组分的设备
CN106905382A (zh) * 2017-02-08 2017-06-30 中国环境科学研究院 一种提取土壤憎水腐殖酸的装置

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