WO2018145458A1 - Equipment for use in extracting humic acid from soil and manufacturing method for equipment - Google Patents

Equipment for use in extracting humic acid from soil and manufacturing method for equipment 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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acid
tank
acidification tank
liquid
outlet
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PCT/CN2017/101707
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French (fr)
Chinese (zh)
Inventor
白英臣
吴丰昌
王彬
魏源
宋凡浩
赵天慧
朱焰
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中国环境科学研究院
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Priority claimed from CN201710069198.2A external-priority patent/CN106893114B/en
Priority claimed from CN201710069441.0A external-priority patent/CN106905382B/en
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/en

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/34Purifying; 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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Abstract

Equipment for use in extracting humic acid from soil, comprising a reaction vessel (1), a pH regulating unit, a filtering and purifying unit, a first acidifying container (8), a first acidity/alkalinity regulating unit, an adsorbing and enriching unit, a second acidifying container (22), a second acidity/alkalinity regulating unit, a humic acid extracting unit, and a general control unit (6). The humic acid extracting unit comprises an all-component extracting unit and a hydrophilic humic acid extracting unit. The equipment for use in extracting humic acid from soil is structurally simple and convenient to operate, has a high degree of automation, allows convenient and effective separation of hydrophilic humic acid from other impurities, not only is capable of extracting a large amount of all components of humic acid, but also is capable of extracting a large amount of dissolved hydrophilic humic acid, and improves the utilization of the humic acid extracted.

Description

一种用于提取土壤腐殖酸的装置及其制备方法Device for extracting soil humic acid and preparation method thereof 技术领域Technical field
本发明涉及腐殖酸提取领域,尤其涉及一种用于提取土壤腐殖酸的装置及其制备方法。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.
背景技术Background technique
腐殖酸是由动植物残体经过复杂的物理、化学、生物过程形成的大分子有机混合物,它广泛存在于土壤、水体、沉积物等环境介质中。腐殖酸能溶于碱性和中性溶液,不溶于酸约占土壤有机质总量的60-80%,是土壤有机质最重要的组成部分。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.
腐殖酸在农业和环境中具有重要作用。目前研究来看,腐殖酸能刺激小麦、番茄、棉花等作物的苗期生长,通过自身的酸性改善土壤pH环境,减轻土壤板结。腐殖酸还能增加土壤中的微生物数量和土壤酶活性,为作物生长提供碳源。通过与土壤营养元素结合,腐殖酸能够增加土壤的养分保蓄和营养盐的可利用性。此外,腐殖酸能与环境中的有毒重金属离子和有机质污染物等发生相互作用,改变污染物迁移、转化规律和生物有效性。因此,进行土壤腐殖酸的研究具有重要的意义。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.
中国发明专利(201510586520.X:一种XAD树脂提取土壤中小分子腐殖酸的方法)公开了一种XAD树脂提取土壤中小分子腐殖酸的方法,其提取步骤为: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:
(a):土壤处理:(a): Soil treatment:
剔除天然土壤中树根和石子等杂物,风干后,碾磨过筛,得到土壤样品备用;Remove the roots and stones from the natural soil, dry them, and then grind them through the sieve to obtain the soil samples for use;
步骤b:焦磷酸钠提取土壤腐殖酸:Step b: Extraction of soil humic acid by sodium pyrophosphate:
向步骤a中的土壤样品加入去离子水,使固液比达到1:5~1:15,用HCl和NaOH调节溶液pH=1.0—3.0,然后向其中加入HCl溶液至固液比1:10,连续搅拌4-8h后静置20-40h,离心分离得到固体土壤样品1;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;
向固体土壤样品1中加入去离子水,使固液比达到1:3~1:5,用HCl和NaOH调节溶液pH=6—8,得固液混合溶液;在氮气保护条件下,向固液混合溶液中加入焦磷酸钠溶液溶液,并用去离子水稀释,使焦磷酸钠浓度为0.1—0.2mol/L,持续搅拌溶液4—8h后再静置20—40h,离心分离得到上清液和固体土壤样品2;Add deionized water to solid soil sample 1 to achieve a solid-liquid ratio of 1:3 to 1:5, adjust the pH of the solution with HCl and NaOH=6-8 to obtain a solid-liquid mixed solution; under nitrogen protection, solidify The sodium pyrophosphate solution is added to the liquid mixed solution, and diluted with deionized water to make the concentration of sodium pyrophosphate 0.1-0.2 mol/L. The solution is continuously stirred for 4-8 hours, then allowed to stand for 20-40 hours, and the supernatant is obtained by centrifugation. And solid soil sample 2;
氮气保护条件下,向该上清液中加入HCl,使溶液pH=1.0—3.0,搅拌15—30min后,静置20—40h,离心分离得到腐殖酸样品1;Under nitrogen protection conditions, add HCl to the supernatant to make the solution pH = 1.0-3.0, stir for 15-30 minutes, then let stand for 20-40 h, centrifuge to obtain humic acid sample 1;
步骤c:氢氧化钠提取土壤腐殖酸: Step c: Extraction of soil humic acid by sodium hydroxide:
向步骤b的固体土壤样品2中加入去离子水,使固液比达到1:3~1:5,用HCl和NaOH调节其pH=6—8,得到固液混合物;在氮气保护条件下,向固液混合物中加入NaOH溶液,并用去离子水稀释,使溶液中NaOH浓度为0.1—0.2mol/L,持续搅拌溶液1—4h后再静置20—40h,离心分离得到上清液及土壤残渣;Add deionized water to the solid soil sample 2 of step b to achieve a solid-liquid ratio of 1:3 to 1:5, and adjust the pH to 6-8 with HCl and NaOH to obtain a solid-liquid mixture; under nitrogen protection conditions, Add NaOH solution to the solid-liquid mixture, and dilute with deionized water to make the NaOH concentration in the solution 0.1-0.2mol/L. Stir the solution for 1-4h, then let stand for 20-40h, and centrifuge to separate the supernatant and soil. Residue
在氮气保护条件下,向该上清液中加入浓HCl,使溶液pH=1.0—3.0,搅拌15—30min,后静置20-40h,离心分离得到腐殖酸样品2;Under nitrogen protection conditions, the concentrated supernatant was added to the supernatant, the solution pH = 1.0-3.0, stirred for 15-30 minutes, then allowed to stand for 20-40h, centrifuged to obtain humic acid sample 2;
合并腐殖酸样品1和腐殖酸样品2,标记为粗提腐殖酸样品;Combining humic acid sample 1 and humic acid sample 2, labeled as crude humic acid sample;
步骤d:去除腐殖酸中富里酸杂质:Step d: remove fulvic acid impurities from humic acid:
向步骤c所得的粗提腐殖酸样品中加入HCl溶液,使其pH=1.0—3.0且固液比1:5—1:10,持续搅拌4—8h,并静置20—40h,离心得到腐殖酸样品和上清液;Adding HCl solution to the crude humic acid sample obtained in step c, making pH=1.0-3.0 and solid-liquid ratio 1:5-1:10, stirring for 4-8 hours, standing for 20-40 h, and centrifuging Humic acid sample and supernatant;
将腐殖酸样品按照步骤d中的方法重复操作,直到离心分离后的上清液中溶解总有机碳含量<0.5mg/L后,收集离心所得固体,并标记为纯化后腐殖酸样品;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;
步骤e:大分子腐殖酸与小分子腐殖酸的分离:Step e: Separation of macromolecular humic acid from small molecule humic acid:
在氮气保护条件下,用NaOH将步骤d中得到的纯化腐殖酸样品溶解,加入去离子水使溶液腐殖酸浓度=10—100g/L,用HCl和NaOH调节pH==6—8,得到腐殖酸溶液;Under nitrogen protection conditions, the purified humic acid sample obtained in step d is dissolved with NaOH, deionized water is added to make the solution humic acid concentration=10-100 g/L, and pH==6-8 is adjusted with HCl and NaOH. Obtaining a humic acid solution;
将腐殖酸溶液移入10000道尔顿透析袋,并将透析袋置于超纯水中,组成透析体系,搅拌20—40h,小分子腐殖酸通过透析袋进入超纯水,形成小分子腐殖酸溶液;Transfer the humic acid solution into a 10,000 Dalton dialysis bag, and place the dialysis bag in ultrapure water to form a dialysis system. Stir for 20-40 hours. Small molecule humic acid enters the ultrapure water through the dialysis bag to form a small molecule rot. Colonic acid solution;
步骤f:去除小分子腐殖酸中的含硅矿物质:Step f: Removal of silicon-containing minerals from small molecule humic acids:
用HCl酸化小分子腐殖酸溶液使其pH=1.0—3.0,加入HF,搅拌15—30min,静置20—40h;Acidify the small molecule humic acid solution with HCl to pH=1.0-3.0, add HF, stir for 15-30 min, let stand for 20-40 h;
步骤g:小分子腐殖酸的富集提取:Step g: Enrichment and extraction of small molecule humic acid:
用HCl和NaOH将步骤f中小分子腐殖酸溶液调节pH=1—3,以10—15倍柱体积/h速度通过XAD—8树脂柱;The small molecule humic acid solution in step f is adjusted to pH=1-3 with HCl and NaOH, and passed through the XAD-8 resin column at a rate of 10-15 column volumes/h;
然后用0.5—1倍柱体积超纯水以10—15倍柱体积/h的速度,淋洗XAD—8树脂柱,弃去流出液;Then, using 0.5-1 column volume ultrapure water at a speed of 10-15 column volumes/h, the XAD-8 resin column is rinsed, and the effluent is discarded;
再用1—2倍柱体积NaOH溶液和2—3倍柱体积超纯水依次以3—10倍柱体积/h的速度,淋洗XAD—8树脂柱,流出液以3—10倍柱体积/h的速度通过氢离子饱和的氢离子交换树脂去除钠离子,最终得到的流出液冷冻干燥得到土壤小分子腐殖酸组分。 Then use 1-2 times column volume NaOH solution and 2-3 times column volume ultrapure water to wash the XAD-8 resin column at a speed of 3-10 column volume/h, and the effluent is 3-10 column volumes. The velocity of /h is removed by hydrogen ion-saturated hydrogen ion exchange resin, and the finally obtained effluent is freeze-dried to obtain a small molecule humic acid component of the soil.
上述发明公开的土壤腐殖酸提取方法,主要是利用XAD-8树脂的吸附特性,将小分子腐殖酸在特定pH值条件下吸附到XAD-8树枝上,再通过解析、离子交换、冷冻干燥,最终获得小分子的腐殖酸,此方法依赖于实验室和大量的人工操作条件下进行的,操作过程复杂、自动化程度低,腐殖酸的提取量少,且方法也不适合大规模样品采集;另外,本论文公开的腐殖酸提取方法受人为影响操作影响较大,不能大量的提取土壤中的腐殖酸,可实施性不佳。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; In addition, 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.
发明内容Summary of the invention
为了有效提取并获取高浓度的土壤憎水腐殖酸组分,本发明提供了一种用于提取土壤腐殖酸的装置,可以实现高效的提取土壤腐殖酸,操作方便,自动化程度高。In order to effectively extract and obtain a high concentration of soil humic acid component, 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.
为了解决上述技术问题,本发明提供了一种用于提取土壤腐殖酸的装置,包括反应釜、pH调节单元、过滤净化单元、第一酸化箱、第一酸碱度调节单元、腐殖酸提取单元和总控制单元;In order to solve the above technical problems, 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;
所述反应釜的入口与所述pH调节单元的出口连接,反应釜的出口与所述过滤净化单元的入口连接,所述过滤净化单元的出口与所述第一酸化箱的入口连接,所述第一酸化箱的入口与所述第一酸碱度调节单元的出口连接;所述第一酸化箱的出口与所述腐殖酸提取单元的入口连接;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;
所述腐殖酸提取单元包括憎水腐殖酸提取单元和腐殖酸全组分提取单元;The humic acid extraction unit includes a hydrophobic humic acid extraction unit and a humic acid full component extraction unit;
所述pH调节单元、第一酸碱度调节单元均与所述总控制单元控制连接。The pH adjusting unit and the first pH adjusting unit are all connected to the overall control unit.
优选地,所述憎水腐殖酸提取单元包括吸附富集单元、第二酸化箱、第二酸碱度调节单元、淋洗装置、第二过滤器和液体储存器;所述吸附富集单元的入口与所述第一酸化箱的出口连接,所述吸附富集单元的出口与所述第二酸化箱的入口连接;所述第二酸化箱的入口还与所述第二酸碱度调节单元的出口连接,所述第二酸碱度调节单元与所述总控制单元连接;所述第二酸化箱的出口与所述第二过滤器的入口连接,所述第二过滤器的入口还与所述淋洗装置的出口连接,所述第二过滤器的出口与所述液体储存器的入口连接,所述液体储存器的底部设有废液排出阀。Preferably, 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.
优选地,所述第二过滤器包括样品室、滤膜和砂芯,所述滤膜设于所述样品室内,并由砂芯支撑,所述滤膜的孔径取值范围为0.1-0.7μm。Preferably, 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, and the filter membrane has a pore diameter ranging from 0.1 to 0.7 μm. .
优选地,所述吸附富集单元包括第一淋洗装置、第二加药装置和吸附富集装置,所述第一淋洗装置的出口、第二加药装置的出口均与所述吸附富集装置的入口连接,所述吸附富集 装置的入口还与所述第一酸化箱的出口连接,所述吸附富集装置的出口与所述第二酸化箱的入口连接,所述吸附富集装置的底部设有废液排出阀。Preferably, 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.
优选地,所述吸附富集装置包括吸附柱和填料,所述填料设于所述吸附柱内,所述填料为XAD-8树脂、DAX-8树脂和XAD-7树脂的一种或多种。Preferably, 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. .
优选地,所述第二酸碱度调节单元包括第三酸液药剂箱、第四酸液药剂箱和第三计量加药泵;所述第三计量加药泵的入口分别与所述第三酸液药剂箱的出口、第四酸液药剂箱的出口连接,所述第三计量加药泵的出口与所述第二酸化箱的入口连接;所述第三酸液药剂箱与所述第四酸液药剂箱并列布置。Preferably, 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.
优选地,所述腐殖酸全组分提取单元包括淋洗装置、第二过滤器和液体储存器;所述淋洗装置的出口与所述第二过滤器的入口连接,所述第二过滤器的出口与所述液体储存器的入口连接;所述第二过滤器包括样品室、滤膜和砂芯,所述滤膜设于所述样品室内,并由砂芯支撑,所述滤膜的孔径取值范围为0.1-0.7μm。Preferably, 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 μm.
优选地,所述pH调节单元包括第一计量加药泵和第一加药装置,第一计量加药泵设于所述第一加药装置与所述反应釜之间,所述第一计量加药泵的入口与所述第一加药装置的出口连接,所述第一计量加药泵的出口与所述反应釜的入口连接。Preferably, 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.
优选地,所述反应釜内设有土壤储存室,所述土壤储存室由支架支撑并设于反应釜内;所述土壤储存室的外壁上设有多个孔径小于1mm的孔。Preferably, 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.
优选地,所述过滤净化单元包括第一过滤器和真空泵,所述第一过滤器的入口通过管道与所述反应釜的出口连接,所述第一过滤器的出口与所述第一酸化箱的入口连接;所述真空泵与所述第一酸化箱连接。Preferably, 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.
优选地,所述反应釜与所述第一过滤器之间的管道伸入反应釜,所述伸入反应釜的管道高度取值为反应釜高度的1/20-1/10,且其外设有保护罩,所述保护罩上设有多个孔径为1mm的孔。Preferably, 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.
优选地,所述反应釜采用耐碱材料,其上面设有密封盖,下端为漏斗形状,反应釜内还设有搅拌器、液位传感器和pH传感器;所述密封盖的端面设有至少5个通孔。Preferably, 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.
优选地,所述第一过滤器与所述第一酸化箱之间的管道伸入第一酸化箱内,所述伸入第一酸化箱的管道位于所述第一酸化箱中液面之上;所述真空泵的吸气口分别位于所述第一酸化箱中液面之上和所述液体储存器中液面之上。 Preferably, 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.
优选地,所述第一酸碱度调节单元包括pH传感器、搅拌器、第一酸液药剂箱、第二酸液药剂箱和第二计量加药泵;所述pH传感器和搅拌器设于所述第一酸化箱内;所述第一酸液药剂箱和第二酸液药剂箱并列布置;所述第二计量加药泵的入口分别与第一酸液药剂箱的出口、第二酸液药剂箱的出口连接,第二计量加药泵的出口与所述第一酸化箱的入口连接。Preferably, 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.
优选地,所述总控制系统包括控制单元和触屏器,所述控制单元均与所述反应釜内的pH传感器、搅拌器、液位传感器、第一计量加药泵、第二计量加药泵、第三计量加药泵、真空泵、第一酸化箱和第二酸化箱内的pH传感器、搅拌器控制连接;所述pH传感器设有升降台。Preferably, 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. The pump, the third metering dosing pump, the vacuum pump, the pH sensor in the first acidification tank and the second acidification tank, and the agitator control connection; the pH sensor is provided with a lifting platform.
采用提取土壤腐殖酸的装置进行土壤憎水腐殖酸提取的方法,其包括如下步骤:A method for extracting soil humic acid by using a device for extracting soil humic acid, comprising the following steps:
(1)土壤加入到土壤储存室中,并向反应釜中注入纯水;(1) the soil is added to the soil storage chamber, and pure water is injected into the reaction kettle;
(2)启动pH调节单元,第一计量加药泵接收位于反应釜中pH传感器信号启动碱液加入程序,第一加药装置通过第一耐强碱管道向反应釜中注入碱液,同时启动反应釜中的搅拌马达,使碱液均匀分散,直到达到预设的pH值,第一计量加药泵停止工作;(2) starting the pH adjusting unit, 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;
(3)打开反应釜的出口阀门,同时启动真空泵,通过真空泵施压,反应釜中的溶液经第一过滤器流入第一酸化箱,碱不溶杂质被滤膜截留而去除,去除杂质后的液体通过滤膜流入第一酸化箱;(3) Opening the outlet valve of the reaction kettle, simultaneously starting the vacuum pump, applying pressure through the vacuum pump, and the solution in the reaction tank flows into the first acidification tank through the first filter, and the alkali-insoluble impurities are removed by the filter membrane to remove the liquid after the impurities are removed. Flowing through the filter membrane into the first acidification tank;
(4)启动第一酸碱度调节单元进行酸碱度的初次调节,第二计量加药泵接收位于酸化箱中的pH传感器信号启动酸液加入程序,第二计量加药泵通过第一通道从第一酸液药剂箱抽取酸液通过第一耐酸管道向酸化箱中注入非氧化性酸液,同时启动酸化箱中搅拌马达,使得酸液均匀分散,直至达到预设的pH值,第二计量加药泵第一通道加酸液程序停止工作,传感器升降台升起pH传感器探头;(4) starting the first pH adjustment unit to perform the initial adjustment of the pH, 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;
第二计量加药泵通过第二通道从第二酸液药剂箱抽取氢氟酸通过第二耐酸管道注入酸化箱中,直到达到预设的氢氟酸浓度,第二计量加药泵停止工作;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;
(5)完成初次的pH值调节后,打开第一酸化箱的出口阀门,同时打开第一酸化箱与吸附富集装置之间的连通阀门,关闭第一酸化箱与第二过滤器之间的连通阀门,第一酸化箱内液体通过管道流入吸附富集装置,吸附完成后,打开第一淋洗装置与吸附富集装置之间的开关,第一淋洗装置中的纯水通过管道冲洗吸附富集装置,并打开吸附富集装置底部的废液排出阀,冲洗废液通过管道排出,完成吸附富集装置的冲洗,并关闭废液排出阀; (5) After the initial pH adjustment is completed, 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. When 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;
完成吸附富集装置冲洗后,关闭淋洗装置的出口阀门,打开第二加药装置的出口阀门,第二加药装置通过第二耐碱管道向吸附富集装置中注入碱液,被树脂吸附的天然溶解有机质在碱液的作用下发生解吸,解吸后的液体经管道流入第二酸化箱;After the immersion and concentration device is flushed, 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;
(6)启动第二酸碱度调节单元进行酸碱度的再次调节,第三计量加药泵接收位于酸化箱中的pH传感器信号启动酸液加入程序,第三计量加药泵通过第三通道从第三酸液药剂箱抽取酸液通过第三耐酸管道向酸化箱中注入非氧化性酸液,同时启动酸化箱中搅拌马达,使得酸液均匀分散,直至达到预设的pH值,第三计量加药泵第三通道加酸液程序停止工作,传感器升降台升起pH传感器探头;(6) starting a second pH adjustment unit for re-adjusting the pH, 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;
第三计量加药泵通过第四通道从第四酸液药剂箱抽取氢氟酸通过第四耐酸管道注入酸化箱中,直到达到预设的氢氟酸浓度,第三计量加药泵停止工作;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;
(7)完成二次的pH值调节后,打开第二酸化箱的出口阀门,同时启动真空泵,通过真空泵施压,第二酸化箱中的有机质溶液通过第二过滤器中的滤膜过滤,憎水腐殖酸被截留在滤膜上面,杂质流入液体储存器中;(7) After the second pH adjustment is completed, the outlet valve of the second acidification tank is opened, and the vacuum pump is started at the same time, and the pressure is applied by the vacuum pump, and the organic matter solution in the second acidification tank is filtered through the filter membrane in the second filter, and the water is rotted. The acid is trapped on the membrane and the impurities flow into the liquid reservoir;
(8)有机质完成过滤后,关闭第二酸化箱的出口阀门,打开淋洗装置的出口阀门,淋洗装置中的纯水通过管道流入第二过滤器,对滤膜进行冲洗,冲洗液直接流入液体储存器中,液体储存器中的液体通过排出阀直接排放掉,留在滤膜上的有机质为所需提取的土壤憎水腐殖酸。(8) After the organic matter is filtered, 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. In the 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 soil humic acid to be extracted.
优选地,所述第一加药装置中的碱液为饱和或近饱和强碱溶液,所述第一耐强碱管道要求能承受饱和强碱,所述耐强碱管道要求能承受0.001-0.5mol/L的强碱;所述反应釜中液体的pH预设值为10-14;所述第二加药装置中的碱液为0.1mol/L的强碱溶液,所述第二耐碱管道要求能承受0.5mol/L的强碱。Preferably, the lye in the first dosing device is a saturated or near-saturated strong alkali solution, and the first alkali-resistant pipeline is required to withstand a saturated strong alkali, and 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.
优选地,所述第一耐酸管道要求能承受10mol/L的非氧化性强酸;所述第二耐酸管道要求能承受6mol/L的氢氟酸;所述第一酸化箱中氢氟酸的预设浓度为0.01-1mol/L;所述第一酸化箱中液体的pH预设值为0.5-1.5。Preferably, 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 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.
优选地,所述第三耐酸管道要求能承受10mol/L的非氧化性强酸;所述第二耐酸管道要求能承受6mol/L的氢氟酸;所述第一酸化箱中氢氟酸的预设浓度为0.01-1mol/L;所述第一酸化箱中液体的pH预设值为0.5-1.5。Preferably, 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.
采用提取土壤腐殖酸的装置进行土壤腐殖酸全组分提取的方法,其包括如下步骤: A method for extracting whole components of soil humic acid by using a device for extracting soil humic acid, comprising the following steps:
(1)土壤加入到土壤储存室中,并向反应釜中注入纯水;(1) the soil is added to the soil storage chamber, and pure water is injected into the reaction kettle;
(2)启动pH调节单元,第一计量加药泵接收位于反应釜中pH传感器信号启动碱液加入程序,加药装置通过耐强碱管道向反应釜中注入碱液,同时启动反应釜中的搅拌马达,使碱液均匀分散,直到达到预设的pH值,第一计量加药泵停止工作;(2) starting the pH adjusting unit, 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;
(3)打开反应釜的出口阀门,同时启动真空泵,反应釜中的液体经真空泵施压通过第一过滤器流入酸化箱内,碱不溶杂质被滤膜截留而去除,去除杂质后的液体通过滤膜流入酸化箱内;(3) Opening the outlet valve of the reaction kettle, and starting the vacuum pump at the same time, the liquid in the reaction kettle is pressurized by the vacuum pump and flows into the acidification tank through the first filter, and the alkali-insoluble impurities are removed by the filter membrane, and the liquid after removing the impurities passes through the filter. The membrane flows into the acidification tank;
(4)启动酸碱度调节单元,第二计量加药泵接收位于第一酸化箱中的pH传感器信号启动酸液加入程序,第二计量加药泵通过第一通道从第一酸液药剂箱抽取酸液通过第一耐酸管道向酸化箱中注入非氧化性酸液,同时启动第一酸化箱中搅拌马达,使得酸液均匀分散,直至达到预设的pH值,第二计量加药泵第一通道加酸液程序停止工作,传感器升降台升起pH传感器探头;(4) starting the pH adjustment unit, 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;
第二计量加药泵通过第二通道从第二酸液药剂箱抽取氢氟酸通过第二耐酸管道注入第一酸化箱中,直到达到预设的氢氟酸浓度,第二计量加药泵停止工作;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;
(5)完成pH值调节后,打开第一酸化箱的出口阀门,同时打开第一酸化箱与第二过滤器之间的连通阀门,关闭第一酸化箱与吸附富集装置之间的连通阀门,启动真空泵,通过真空泵施压,酸化箱中的有机质溶液通过第二过滤器中的滤膜过滤,腐殖酸全组分被截留在滤膜上面,杂质流入液体储存器中;(5) After the pH adjustment is completed, 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;
(6)有机质完成过滤后,关闭第一酸化箱的出口阀门,打开淋洗装置的出口阀门,淋洗装置中的纯水通过管道流入第二过滤器,对滤膜进行冲洗,冲洗液直接流入液体储存器中,液体储存器中的液体通过排出阀直接排放掉,留在滤膜上的有机质为所需提取的土壤腐殖酸全组分。(6) After the organic matter is filtered, 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.
优选地,所述第一加药装置中的碱液为饱和或近饱和强碱溶液,所述第一耐强碱管道要求能承受饱和强碱,所述第一耐强碱管道要求能承受0.001-0.5mol/L的强碱;所述反应釜中液体的pH预设值为10-14;所述第一耐酸管道要求能承受10mol/L的非氧化性强酸;所述第二耐酸管道要求能承受6mol/L的氢氟酸;所述第一酸化箱中氢氟酸的预设浓度为0.01-1mol/L;所述第一酸化箱中液体的pH预设值为0.5-1.5。Preferably, 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, and 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.
与现有技术相比,本发明产生的有益效果是: Compared with the prior art, the beneficial effects produced by the present invention are:
(1)本发明提供的用于提取土壤腐殖酸的装置,结构简单,操作方便,自动化程度高,可以方便有效地将憎水腐殖酸和其它杂质分离,既可以提取大量的土壤憎水溶解性腐殖酸,还可以提取大量的土壤腐殖酸全组分,在很大程度上满足了客户对不同土壤腐殖酸组分的需求;(1) The device for extracting soil humic acid provided by the invention 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;
(2)反应釜、第一酸化箱、第二酸化箱底部均为漏斗形状,伸入反应釜、第一酸化箱的管道外设有过滤罩,伸入反应釜管道的高度取值为反应釜的高度的1/20-1/10,伸入第一酸化箱管道的高度取值为第一酸化箱高度的1/30-1/20,伸入第一酸化箱的管道外设有过滤罩,既可以保证最大限度的收集腐殖酸,提高了装置效率,又可以有效的阻止杂质颗粒混入样品中,保证了提取液的纯度;(2) 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;
(3)pH值调节、第一酸碱度调节单元、第二酸碱度调节单元均是全自动的,节省了劳动力,调节的pH值的准确率比较高;第一酸液药剂箱和第二酸液药剂箱共用一个计量加药泵,第三酸液药剂箱和第四酸液药剂箱共用一个计量加药泵,经过进一步优化pH值调节单元、第一酸碱度调节单元和第二酸碱度调节单元可共用一个多通道的计量加药泵,进一步降低生产成本;第一酸化箱、第二酸化箱、液体储存器共用一个真空泵,降低了生产成本;(3) 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;
(4)反应釜预留了惰性气体入口和出口,在生产中通过通入氮气、氦气等惰性气体,可以有效抑制强碱性条件下土壤腐殖酸全组分氧化。(4) 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.
附图说明DRAWINGS
图1是本发明提供的一种用于提取土壤腐殖酸的装置的工艺流程图。1 is a process flow diagram of an apparatus for extracting soil humic acid provided by the present invention.
具体实施方式detailed description
下面结合附图,对本发明的具体实施方式作详细的说明。The specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
参图1所示,图1是本发明提供的一种用于提取土壤腐殖酸的装置的工艺流程图。本发明提供的提取土壤腐殖酸全组分的设备,包括反应釜1、pH调节单元、过滤净化单元、第一酸化箱8、第一酸碱度调节单元、腐殖酸提取单元和总控制单元6,腐殖酸提取单元包括憎水腐殖酸提取单元和腐殖酸全组分提取单元;其中,反应釜1内设有土壤储存室2、支架3、搅拌器、液位传感器和pH传感器,土壤储存室2由支架3支撑并位于反应釜1内,土壤储存室2的外壁设有多个孔径小于1mm的孔;pH调节单元包括第一计量加药泵4和第一加药装置5;过滤净化单元包括第一过滤器7和真空泵12,其中第一过滤器7内包括样品室71、滤膜72和砂芯73,滤膜72设于样品室71内,并由砂芯73支撑;第一酸碱度调节单元包括第 二计量加药泵9、第一酸液药剂箱10和第二酸液药剂箱11;憎水腐殖酸提取单元包括吸附富集单元、第二酸碱度调节单元、第二酸化箱22、淋洗装置13、第二过滤器14和液体储存器15,吸附富集单元包括第一淋洗装置16、第二加药装置17、吸附富集装置18;第二酸碱度调节单元包括第三酸液药剂箱20、第四酸液药剂箱21和第三计量加药泵19;腐殖酸全组分提取单元包括淋洗装置13、第二过滤器14和液体储存器15;其中,第二过滤器14包括样品室141、滤膜142和砂芯143,滤膜142设于样品室141内,并由砂芯143支撑;总控制单元6主要采用自动控制,其中的集控操作在控制柜中统一进行,可使整个系统实现自动控制操作和手动操作。Referring to Figure 1, Figure 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. A fourth acid solution tank 21 and a third metering dosing pump 19; 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.
其中,第一加药装置5通过第一计量加药泵4与反应釜1连接,第一计量加药泵4的入口与第一加药装置5连接,其出口与反应釜1连接;反应釜1的出口与第一过滤器7的入口连接,反应釜1与第一过滤器7之间的连接管道伸入反应釜1中,伸入反应釜管道的高度取值为反应釜1高度的1/20-1/10,且其外设有保护罩,所述保护罩上设有多个孔径为1mm的孔;第一过滤器7的出口与第一酸化箱8连接,真空泵12的出口置于第一酸化箱8的腔体内;第一酸液药剂箱10和第二酸液药剂箱11并列布置,第二计量加药泵9设于第一酸液药剂箱10和第二酸液药剂箱11之间,第二计量加药泵9的入口与第一酸液药剂箱10的出口、第二酸液药剂箱11的出口连接,第二计量加药泵9的出口与第一酸化箱8的入口连接,第一酸化箱8的出口分别与吸附富集装置18的入口、第二过滤器14的入口连接;吸附富集装置18的入口还与第一淋洗装置16的出口、第二加药装置17的出口连接,吸附富集装置18的出口与第二酸化箱22的入口连接;,吸附富集装置的底部设有废液排出阀;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. /20-1/10, and a 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 Between the tanks 11, 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. Liquid discharge valve
第三酸液药剂箱20的出口、第四酸液药剂箱21的出口均与第三计量加药泵19的入口连接,第三计量加药泵19的出口与第二酸化箱22的入口连接;第二酸化箱22的出口与第二过滤器14的入口连接;第二过滤器14的入口还与淋洗装置13的出口连接,第二过滤器14的出口与液体储存器15的入口连接;真空泵12的出口分别置于第一酸化箱8的腔体内和液体储存器15的腔体内;液体储存器15的底部设有废液排出阀。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.
总控制系统6包括控制单元和触屏器,控制单元与触屏器连接,控制单元与搅拌器、液位传感器、pH传感器、第一计量加药泵4、第二计量加药泵9、真空泵12连接。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.
总控制系统采用低压配电,供配电设备的电压等级为220VAC,且设低压配电柜,向工艺系统动力设备供电。另外,控制系统中配备独立操作的控制柜,以及电器开关和电气元件 都集中在控制柜内,电源开关与电控柜门联锁保护,可以达到防尘、散热快且易于安装的效果。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. In addition, 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.
实施例一Embodiment 1
首先开启总电源和启动按钮,使整个系统处于工作状态,启动注水程序,向土壤储存室2中加入一定量研磨后的土壤样品,并关闭土壤储存室2;启动注水程序,向土壤储存室2中加入纯水,反应釜1中的液位传感器对反应釜1中的水位进行检测,当水位达到反应釜总体积的4/5时,液位传感器向总控制系统发送液位信号,停止注水过程。First turn on the main power and start button, make the whole system in working state, start the water injection program, add a certain amount of ground soil sample to the soil storage room 2, and close the soil storage room 2; start the water injection program to the soil storage room 2 The pure water is added, and the liquid level sensor in the reaction tank 1 detects the water level in the reaction kettle 1. When the water level reaches 4/5 of the total volume of the reaction kettle, the liquid level sensor sends a liquid level signal to the total control system to stop the water injection. process.
向反应釜1中通入惰性气体,在惰性气体的保护下,启动pH调节单元,第一计量加药泵4接收位于反应釜1中的pH传感器信号启动碱液加入程序,第一加药装置5通过耐强碱管道向反应釜1中注入碱液,同时启动反应釜1中的搅拌马达,使得碱液均匀分散,直到达到预设的pH值,第一计量加药泵4停止工作。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.
持续搅拌,土壤储存室2中的土壤样品浸取液通过土壤储存室外壁上的孔流入反应釜1中。土壤储存室2外壁上设有多个孔径小于1mm的孔,可以有效地阻止土壤中的杂质进入到反应釜1的液体中;其中反应釜1采用耐碱材料,其上面设有密封盖,下端为漏斗形状,其内设有搅拌器、液位传感器和pH传感器,所述密封盖的端面设有至少5个通孔。With continuous stirring, 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.
打开反应釜1的出口阀门,同时启动真空泵12,通过真空泵12施压,反应釜1中的溶液经第一过滤器7流入第一酸化箱8,碱不溶杂质被滤膜截留而去除,去除杂质后的液体通过滤膜流入第一酸化箱8;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;
启动第一酸碱度调节单元进行酸碱度的初次调节,第二计量加药泵9接收位于第一酸化箱8中的pH传感器信号启动酸液加入程序,第二计量加药泵9通过第一通道从第一酸液药剂箱10抽取酸液通过第一耐酸管道向第一酸化箱8中注入非氧化性酸液,同时启动第一酸化箱中搅拌马达,使得酸液均匀分散,直至达到预设的pH值,第二计量加药泵9第一通道加酸液程序停止工作,传感器升降台升起pH传感器探头;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, and 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;
第二计量加药泵9通过第二通道从第二酸液药剂箱11抽取氢氟酸通过第二耐酸管道注入酸化箱中,直到达到预设的氢氟酸浓度,第二计量加药泵9停止工作;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;
完成初次的pH值调节后,打开第一酸化箱8的出口阀门,同时打开第一酸化箱8与吸附富集装置18之间的连通阀,关闭第一酸化箱8与第二过滤器14之间的连通阀,第一酸化箱8内液体通过管道流入吸附富集装置18,吸附完成后,打开第一淋洗装置16与吸附富集 装置18之间的开关,第一淋洗装置16中的纯水通过管道冲洗吸附富集装置18,并打开吸附富集装置18底部的废液排出阀,冲洗废液通过管道排出,完成吸附富集装置18的冲洗,并关闭废液排出阀;After the initial pH adjustment is completed, 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. After the adsorption is completed, the first rinse device 16 is opened and the adsorption is enriched. The switch between the devices 18, the pure water in the first eluent device 16 flushes the adsorption enrichment device 18 through the pipeline, and opens the waste liquid discharge valve at the bottom of the adsorption enrichment device 18, and the flushing waste liquid is discharged through the pipeline to complete the adsorption rich Flushing the device 18 and closing the waste liquid discharge valve;
完成吸附富集装置18冲洗后,关闭第一淋洗装置16与吸附富集装置18之间的开关,打开第二加药装置17与吸附富集装置18之间的开关,第二加药装置17通过第二耐碱管道向吸附富集装置18中注入碱液,被树脂吸附的天然溶解有机质在碱液的作用下发生解吸,解吸后的液体经管道流入第二酸化箱22;After the immersion of the concentrating and accumulating device 18 is completed, 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;
启动第二酸碱度调节单元进行酸碱度的再次调节,第三计量加药泵19接收位于第二酸化箱22中的pH传感器信号启动酸液加入程序,第三计量加药泵19通过第三通道从第三酸液药剂箱20抽取酸液通过第三耐酸管道向酸化箱中注入非氧化性酸液,同时启动酸化箱中搅拌马达,使得酸液均匀分散,直至达到预设的pH值,第三计量加药泵19第三通道加酸液程序停止工作,传感器升降台升起pH传感器探头;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, and 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;
第三计量加药泵19通过第四通道从第四酸液药剂箱21抽取氢氟酸通过第四耐酸管道注入酸化箱中,直到达到预设的氢氟酸浓度,第三计量加药泵19停止工作;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;
完成二次的pH值调节后,打开第二酸化箱22的出口阀门,同时启动真空泵12,通过真空泵12施压,第二酸化箱22中的有机质溶液通过第二过滤器中的滤膜过滤,憎水腐殖酸被截留在滤膜上面,杂质流入液体储存器中;After the second pH adjustment is completed, 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;
有机质完成过滤后,关闭第二酸化箱22的出口阀门,打开第二淋洗装置13的出口阀门,第二淋洗装置13中的纯水通过管道流入第二过滤器14,对滤膜142进行冲洗,冲洗液直接流入液体储存器15中,液体储存器15中的液体通过排出阀直接排放掉,留在滤膜142上的有机质为所需提取的土壤憎水腐殖酸,完成了土壤憎水腐殖酸的提取。After the organic matter is filtered, 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.
pH值调节单元、第一酸碱度调节单元、第二酸碱度调节单元中的pH值调节的过程均为全自动的过程,节省了劳动力,降低了生产成本,并且调制的pH值的精确度比较高,配制的过程效率也较高。在pH调节过程中,开启搅拌器马达使搅拌器搅拌反应釜1、第一酸化箱8、第二酸化箱22中的液体,使得流入其中的酸液药剂均匀溶入水中,可避免局部的pH值偏高或偏低。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. During the pH adjustment process, 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.
实施例二 Embodiment 2
完成初次的pH值调节后,打开第一酸化箱8的出口阀门,同时打开第一酸化箱8与第二过滤器14之间的连通阀,关闭第一酸化箱8与吸附富集装置18之间的连通阀,启动真空泵12,通过真空泵12施压,第一酸化箱8中的溶液通过第二过滤器8中的滤膜142过滤,腐殖酸全组分被截留在滤膜上,杂质流入液体储存器15内;After the initial pH adjustment is completed, 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;
过滤完成后,关闭第一酸化箱8的出口阀门,打开淋洗装置13的出口阀门,淋洗装置13内的纯水通过管道注入第二过滤器14,对第二过滤器14内的粗品腐殖酸进行冲洗,冲洗液直接流入液体储存器15中,液体储存器中的液体通过排出阀直接排放掉,土壤腐殖酸全组分留在滤膜上,完成土壤腐殖酸全组分的提取。After the filtration is completed, 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.
所述第一过滤器中使用的滤膜为一次性滤膜,滤膜需要能耐受1mol/L强碱,滤膜按要求存储及使用,但不可使用玻璃纤维滤膜等含硅滤膜;所述第二过滤器中使用的滤膜为一次性滤膜,滤膜需要能耐受0.5mol/L强酸,滤膜按要求存储及使用,但不可使用玻璃纤维滤膜等含硅滤膜。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.
上文所述的一系列的详细说明仅仅是针对本发明的可行性实施方式的具体说明,它们并不是用以限制本发明的保护范围,在所述技术领域普通技术人员所具备的知识范围内,在不脱离本发明宗旨的前提下作出的各种变化均属于本发明的保护范围。 The detailed descriptions of the foregoing are merely illustrative of the possible embodiments of the present invention, and are not intended to limit the scope of the present invention, which is within the knowledge of those skilled in the art Various changes made without departing from the spirit of the invention are within the scope of the invention.

Claims (13)

  1. 一种用于提取土壤腐殖酸的装置,包括反应釜、pH调节单元、过滤净化单元、第一酸化箱、第一酸碱度调节单元、腐殖酸提取单元和总控制单元;其特征在于,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, a humic acid extraction unit, and a total control unit;
    所述反应釜的入口与所述pH调节单元的出口连接,反应釜的出口与所述过滤净化单元的入口连接,所述过滤净化单元的出口与所述第一酸化箱的入口连接,所述第一酸化箱的入口与所述第一酸碱度调节单元的出口连接;所述第一酸化箱的出口与所述腐殖酸提取单元的入口连接;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;
    所述腐殖酸提取单元包括憎水腐殖酸提取单元和腐殖酸全组分提取单元;The humic acid extraction unit includes a hydrophobic humic acid extraction unit and a humic acid full component extraction unit;
    所述pH调节单元、第一酸碱度调节单元均与所述总控制单元控制连接。The pH adjusting unit and the first pH adjusting unit are all connected to the overall control unit.
  2. 如权利要求1所述的用于提取土壤腐殖酸的装置,其特征在于,所述憎水腐殖酸提取单元包括吸附富集单元、第二酸化箱、第二酸碱度调节单元、淋洗装置、第二过滤器和液体储存器;所述吸附富集单元的入口与所述第一酸化箱的出口连接,所述吸附富集单元的出口与所述第二酸化箱的入口连接;所述第二酸化箱的入口还与所述第二酸碱度调节单元的出口连接,所述第二酸碱度调节单元与所述总控制单元连接;所述第二酸化箱的出口与所述第二过滤器的入口连接,所述第二过滤器的入口还与所述淋洗装置的出口连接,所述第二过滤器的出口与所述液体储存器的入口连接,所述液体储存器的底部设有废液排出阀;The apparatus for extracting soil humic acid according to claim 1, wherein 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 is connected to an outlet of the first acidification tank, an outlet of the adsorption-enrichment unit is connected to an inlet of the second acidification tank; the second acidification An inlet of the tank is further connected to an outlet of the second pH adjusting unit, the second pH adjusting unit is connected to the total control unit; an outlet of the second acidifying tank is connected to an inlet of the second filter, The inlet of the second filter is also connected to the outlet of the rinsing device, the outlet of the second filter is connected to the inlet of the liquid reservoir, and the bottom of the liquid reservoir is provided with a waste liquid discharge valve;
    所述第二过滤器包括样品室、滤膜和砂芯,所述滤膜设于所述样品室内,并由砂芯支撑,所述滤膜的孔径取值范围为0.1-0.7μm。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, and the filter membrane has a pore diameter ranging from 0.1 to 0.7 μm.
  3. 如权利要求2所述的用于提取土壤憎水腐殖酸的装置,其特征在于,所述吸附富集单元包括第一淋洗装置、第二加药装置和吸附富集装置,所述第一淋洗装置的出口、第二加药装置的出口均与所述吸附富集装置的入口连接,所述吸附富集装置的入口还与所述第一酸化箱的出口连接,所述吸附富集装置的出口与所述第二酸化箱的入口连接,所述吸附富集装置的底部设有废液排出阀;The apparatus for extracting soil hydrophobic humic acid according to claim 2, wherein the adsorption and enrichment unit comprises a first rinsing device, a second medicating device, and an adsorption and enrichment device, An outlet of a rinsing device and an outlet of the second medicating device are both connected to an inlet of the concentrating and accumulating device, and an inlet of the concentrating and enriching device is further connected to an outlet of the first acidification tank, the absorbing rich An outlet of the collecting device is connected to an inlet of the second acidification tank, and a bottom of the adsorption and enrichment device is provided with a waste liquid discharge valve;
    所述第二酸碱度调节单元包括第三酸液药剂箱、第四酸液药剂箱和第三计量加药泵;所述第三计量加药泵的入口分别与所述第三酸液药剂箱的出口、第四酸液药剂箱的出口连接,所述第三计量加药泵的出口与所述第二酸化箱的入口连接;所述第三酸液药剂箱与所述第四酸液药剂箱并列布置。 The second pH adjustment unit includes a third acid solution tank, a fourth acid solution tank, and a third metering dosing pump; the inlet of the third metering dosing pump and the third acid solution tank respectively An outlet, 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 is juxtaposed with the fourth acid liquid medicine tank Arrangement.
  4. 如权利要求1所述的用于提取土壤腐植酸的装置,其特征在于,所述腐殖酸全组分提取单元包括淋洗装置、第二过滤器和液体储存器;所述淋洗装置的出口与所述第二过滤器的入口连接,所述第二过滤器的出口与所述液体储存器的入口连接;所述第二过滤器包括样品室、滤膜和砂芯,所述滤膜设于所述样品室内,并由砂芯支撑,所述滤膜的孔径取值范围为0.1-0.7μm。The apparatus for extracting soil humic acid according to claim 1, wherein said humic acid component extracting unit comprises a rinsing device, a second filter and a liquid reservoir; and said rinsing device An outlet is connected to the inlet of the second filter, an outlet of the second filter is connected to an inlet of the liquid reservoir; the second filter comprises a sample chamber, a filter membrane and a sand core, the filter It is disposed in the sample chamber and supported by a sand core, and the filter membrane has a pore diameter ranging from 0.1 to 0.7 μm.
  5. 如权利要求1所述的用于提取土壤腐殖酸的装置,其特征在于,所述pH调节单元包括第一计量加药泵和第一加药装置,第一计量加药泵设于所述第一加药装置与所述反应釜之间,所述第一计量加药泵的入口与所述第一加药装置的出口连接,所述第一计量加药泵的出口与所述反应釜的入口连接;The apparatus for extracting soil humic acid according to claim 1, wherein the pH adjusting unit comprises a first metering dosing pump and a first dosing device, and the first metering dosing pump is provided in the Between the first dosing device and the reaction kettle, an inlet of the first metering dosing pump is connected to an outlet of the first dosing device, an outlet of the first metering dosing pump and the reaction kettle Entrance connection
    所述反应釜内设有土壤储存室,所述土壤储存室由支架支撑并设于反应釜内;所述土壤储存室的外壁上设有多个孔径小于1mm的孔。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 diameter of less than 1 mm.
  6. 如权利要求1所述的用于提取土壤腐殖酸的装置,其特征在于,所述过滤净化单元包括第一过滤器和真空泵,所述第一过滤器的入口通过管道与所述反应釜的出口连接,所述第一过滤器的出口与所述第一酸化箱的入口连接;所述真空泵与所述第一酸化箱连接;The apparatus for extracting soil humic acid according to claim 1, wherein the filtration purification unit comprises a first filter and a vacuum pump, and an inlet of the first filter passes through a pipe and the reaction kettle An outlet connection, an outlet of the first filter is connected to an inlet of the first acidification tank; the vacuum pump is connected to the first acidification tank;
    所述反应釜与所述第一过滤器之间的管道伸入反应釜,所述伸入反应釜的管道高度取值为反应釜高度的1/20-1/10,且其外设有保护罩,所述保护罩上设有多个孔径为1mm的孔;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 the protection is externally provided. a cover, the protective cover is provided with a plurality of holes having a hole diameter of 1 mm;
    所述反应釜采用耐碱材料,其上面设有密封盖,下端为漏斗形状,反应釜内还设有搅拌器、液位传感器和pH传感器;所述密封盖的端面设有至少5个通孔;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. The reactor is further provided with a stirrer, a liquid level sensor and a pH sensor; the end surface of the sealing cover is provided with at least 5 through holes. ;
    所述第一过滤器与所述第一酸化箱之间的管道伸入第一酸化箱内,所述伸入第一酸化箱的管道位于所述第一酸化箱中液面之上;所述真空泵的吸气口分别位于所述第一酸化箱中液面之上和所述液体储存器中液面之上。a conduit 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.
  7. 如权利要求1所述的用于提取土壤腐殖酸的装置,其特征在于,所述第一酸碱度调节单元包括pH传感器、搅拌器、第一酸液药剂箱、第二酸液药剂箱和第二计量加药泵;所述pH传感器和搅拌器设于所述第一酸化箱内;所述第一酸液药剂箱和第二酸液药剂箱并列布置;所述第二计量加药泵的入口分别与第一酸液药剂箱的出口、第二酸液药剂箱的出口连接,第二计量加药泵的出口与所述第一酸化箱的入口连接。The apparatus for extracting soil humic acid according to claim 1, wherein the first pH adjusting unit comprises a pH sensor, a stirrer, a first acid solution tank, a second acid tank, and a a metering dosing pump; the pH sensor and the agitator are disposed in the first acidification tank; the first acid liquid medicine tank and the second acid liquid medicine tank are arranged side by side; the second metering dosing pump is The inlet is connected to the outlet of the first acid solution tank, the outlet of the second acid tank, and the outlet of the second metering pump is connected to the inlet of the first acid tank.
  8. 如权利要求1所述的用于提取土壤腐殖酸的装置,其特征在于,所述总控制系统包括控制单元和触屏器,所述控制单元均与所述反应釜内的pH传感器、搅拌器、液位传感器、 第一计量加药泵、第二计量加药泵、第三计量加药泵、真空泵、第一酸化箱和第二酸化箱内的pH传感器、搅拌器控制连接;所述pH传感器设有升降台。The apparatus for extracting soil humic acid according to claim 1, wherein the total control system comprises a control unit and a touch screen, and the control unit is coupled with a pH sensor and a stirring in the reaction kettle. , liquid level sensor, The first metering dosing pump, the second metering dosing pump, the third metering dosing pump, the vacuum pump, the pH sensor in the first acidification tank and the second acidification tank, and the agitator control connection; the pH sensor is provided with a lifting platform.
  9. 利用权利要求1-8任一所述的用于提取土壤腐殖酸的装置进行土壤憎水腐殖酸提取的方法,其特征在于,其包括如下步骤:A method for extracting soil humic acid by using the apparatus for extracting soil humic acid according to any one of claims 1-8, characterized in that it comprises the following steps:
    (1)土壤加入到土壤储存室中,并向反应釜中注入纯水;(1) the soil is added to the soil storage chamber, and pure water is injected into the reaction kettle;
    (2)启动pH调节单元,第一计量加药泵接收位于反应釜中pH传感器信号启动碱液加入程序,第一加药装置通过第一耐强碱管道向反应釜中注入碱液,同时启动反应釜中的搅拌马达,使碱液均匀分散,直到达到预设的pH值,第一计量加药泵停止工作;(2) starting the pH adjusting unit, 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;
    (3)打开反应釜的出口阀门,同时启动真空泵,通过真空泵施压,反应釜中的溶液经第一过滤器流入第一酸化箱,碱不溶杂质被滤膜截留而去除,去除杂质后的液体通过滤膜流入第一酸化箱;(3) Opening the outlet valve of the reaction kettle, simultaneously starting the vacuum pump, applying pressure through the vacuum pump, and the solution in the reaction tank flows into the first acidification tank through the first filter, and the alkali-insoluble impurities are removed by the filter membrane to remove the liquid after the impurities are removed. Flowing through the filter membrane into the first acidification tank;
    (4)启动第一酸碱度调节单元进行酸碱度的初次调节,第二计量加药泵接收位于酸化箱中的pH传感器信号启动酸液加入程序,第二计量加药泵通过第一通道从第一酸液药剂箱抽取酸液通过第一耐酸管道向酸化箱中注入非氧化性酸液,同时启动酸化箱中搅拌马达,使得酸液均匀分散,直至达到预设的pH值,第二计量加药泵第一通道加酸液程序停止工作,传感器升降台升起pH传感器探头;(4) starting the first pH adjustment unit to perform the initial adjustment of the pH, 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;
    第二计量加药泵通过第二通道从第二酸液药剂箱抽取氢氟酸通过第二耐酸管道注入酸化箱中,直到达到预设的氢氟酸浓度,第二计量加药泵停止工作;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;
    (5)完成初次的pH值调节后,打开第一酸化箱的出口阀门,同时打开第一酸化箱与吸附富集装置之间的连通阀门,关闭第一酸化箱与第二过滤器之间的连通阀门,第一酸化箱内液体通过管道流入吸附富集装置,吸附完成后,打开第一淋洗装置与吸附富集装置之间的开关,第一淋洗装置中的纯水通过管道冲洗吸附富集装置,并打开吸附富集装置底部的废液排出阀,冲洗废液通过管道排出,完成吸附富集装置的冲洗,并关闭废液排出阀;(5) After the initial pH adjustment is completed, 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. When 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;
    完成吸附富集装置冲洗后,关闭淋洗装置的出口阀门,打开第二加药装置的出口阀门,第二加药装置通过第二耐碱管道向吸附富集装置中注入碱液,被树脂吸附的天然溶解有机质在碱液的作用下发生解吸,解吸后的液体经管道流入第二酸化箱;After the immersion and concentration device is flushed, 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;
    (6)启动第二酸碱度调节单元进行酸碱度的再次调节,第三计量加药泵接收位于酸化箱中的pH传感器信号启动酸液加入程序,第三计量加药泵通过第三通道从第三酸液药剂箱抽 取酸液通过第三耐酸管道向酸化箱中注入非氧化性酸液,同时启动酸化箱中搅拌马达,使得酸液均匀分散,直至达到预设的pH值,第三计量加药泵第三通道加酸液程序停止工作,传感器升降台升起pH传感器探头;(6) starting a second pH adjustment unit for re-adjusting the pH, 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 Liquid medicine tank pumping The acid solution is injected into the acidification tank through the third acid-proof pipeline, and the stirring motor in the acidification tank is started, so that the acid liquid is evenly dispersed until the preset pH value is reached, and the third metering dosing pump third channel The acid solution program stops working, and the sensor lifter raises the pH sensor probe;
    第三计量加药泵通过第四通道从第四酸液药剂箱抽取氢氟酸通过第四耐酸管道注入酸化箱中,直到达到预设的氢氟酸浓度,第三计量加药泵停止工作;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;
    (7)完成二次的pH值调节后,打开第二酸化箱的出口阀门,同时启动真空泵,通过真空泵施压,第二酸化箱中的有机质溶液通过第二过滤器中的滤膜过滤,憎水腐殖酸被截留在滤膜上面,杂质流入液体储存器中;(7) After the second pH adjustment is completed, the outlet valve of the second acidification tank is opened, and the vacuum pump is started at the same time, and the pressure is applied by the vacuum pump, and the organic matter solution in the second acidification tank is filtered through the filter membrane in the second filter, and the water is rotted. The acid is trapped on the membrane and the impurities flow into the liquid reservoir;
    (8)有机质完成过滤后,关闭第二酸化箱的出口阀门,打开淋洗装置的出口阀门,淋洗装置中的纯水通过管道流入第二过滤器,对滤膜进行冲洗,冲洗液直接流入液体储存器中,液体储存器中的液体通过排出阀直接排放掉,留在滤膜上的有机质为所需提取的土壤憎水腐殖酸。(8) After the organic matter is filtered, 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. In the 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 soil humic acid to be extracted.
  10. 如权利要求9所述的土壤憎水腐殖酸提取方法,其特征在于,所述第一加药装置中的碱液为饱和或近饱和强碱溶液,所述第一耐强碱管道要求能承受饱和强碱,所述耐强碱管道要求能承受0.001-0.5mol/L的强碱;所述反应釜中液体的pH预设值为10-14;所述第二加药装置中的碱液为0.1mol/L的强碱溶液,所述第二耐碱管道要求能承受0.5mol/L的强碱。The method for extracting soil hydrophobic humic acid according to claim 9, wherein the alkali solution in the first dosing device is a saturated or near-saturated strong alkali solution, and the first alkali-resistant alkali pipeline requires energy. Sustaining a saturated alkali, the alkali-resistant pipeline is required to withstand a strong base of 0.001-0.5 mol/L; the pH of the liquid in the reactor is preset to 10-14; the alkali in the second dosing device The liquid is a 0.1 mol/L strong alkali solution, and the second alkali-resistant pipe is required to withstand a strong base of 0.5 mol/L.
  11. 如权利要求9所述的土壤憎水腐殖酸提取方法,其特征在于,所述第一耐酸管道要求能承受10mol/L的非氧化性强酸;所述第二耐酸管道要求能承受6mol/L的氢氟酸;所述第一酸化箱中氢氟酸的预设浓度为0.01-1mol/L;所述第一酸化箱中液体的pH预设值为0.5-1.5;The method for extracting soil hydrophobic humic acid according to claim 9, wherein the first acid-resistant pipe is required to withstand a non-oxidizing strong acid of 10 mol/L; and the second acid-resistant pipe is required to withstand 6 mol/L. Hydrofluoric acid; the first 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 be 0.5-1.5;
    所述第三耐酸管道要求能承受10mol/L的非氧化性强酸;所述第二耐酸管道要求能承受6mol/L的氢氟酸;所述第一酸化箱中氢氟酸的预设浓度为0.01-1mol/L;所述第一酸化箱中液体的pH预设值为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; 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 be 0.5-1.5.
  12. 利用权利要求1-8任一所述的用于提取土壤腐殖酸的装置进行土壤腐殖酸全组分提取的方法,其特征在于,其包括如下步骤:A method for extracting whole components of soil humic acid by using the apparatus for extracting soil humic acid according to any one of claims 1-8, characterized in that it comprises the following steps:
    (1)土壤加入到土壤储存室中,并向反应釜中注入纯水;(1) the soil is added to the soil storage chamber, and pure water is injected into the reaction kettle;
    (2)启动pH调节单元,第一计量加药泵接收位于反应釜中pH传感器信号启动碱液加入程序,加药装置通过耐强碱管道向反应釜中注入碱液,同时启动反应釜中的搅拌马达,使碱液均匀分散,直到达到预设的pH值,第一计量加药泵停止工作; (2) starting the pH adjusting unit, 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;
    (3)打开反应釜的出口阀门,同时启动真空泵,反应釜中的液体经真空泵施压通过第一过滤器流入酸化箱内,碱不溶杂质被滤膜截留而去除,去除杂质后的液体通过滤膜流入酸化箱内;(3) Opening the outlet valve of the reaction kettle, and starting the vacuum pump at the same time, the liquid in the reaction kettle is pressurized by the vacuum pump and flows into the acidification tank through the first filter, and the alkali-insoluble impurities are removed by the filter membrane, and the liquid after removing the impurities passes through the filter. The membrane flows into the acidification tank;
    (4)启动酸碱度调节单元,第二计量加药泵接收位于第一酸化箱中的pH传感器信号启动酸液加入程序,第二计量加药泵通过第一通道从第一酸液药剂箱抽取酸液通过第一耐酸管道向酸化箱中注入非氧化性酸液,同时启动第一酸化箱中搅拌马达,使得酸液均匀分散,直至达到预设的pH值,第二计量加药泵第一通道加酸液程序停止工作,传感器升降台升起pH传感器探头;(4) starting the pH adjustment unit, 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;
    第二计量加药泵通过第二通道从第二酸液药剂箱抽取氢氟酸通过第二耐酸管道注入第一酸化箱中,直到达到预设的氢氟酸浓度,第二计量加药泵停止工作;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;
    (5)完成pH值调节后,打开第一酸化箱的出口阀门,同时打开第一酸化箱与第二过滤器之间的连通阀门,关闭第一酸化箱与吸附富集装置之间的连通阀门,启动真空泵,通过真空泵施压,酸化箱中的有机质溶液通过第二过滤器中的滤膜过滤,腐殖酸全组分被截留在滤膜上面,杂质流入液体储存器中;(5) After the pH adjustment is completed, 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;
    (6)有机质完成过滤后,关闭第一酸化箱的出口阀门,打开淋洗装置的出口阀门,淋洗装置中的纯水通过管道流入第二过滤器,对滤膜进行冲洗,冲洗液直接流入液体储存器中,液体储存器中的液体通过排出阀直接排放掉,留在滤膜上的有机质为所需提取的土壤腐殖酸全组分。(6) After the organic matter is filtered, 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.
  13. 如权利要求12所述的土壤腐殖酸全组分提取方法,其特征在于,所述第一加药装置中的碱液为饱和或近饱和强碱溶液,所述第一耐强碱管道要求能承受饱和强碱,所述第一耐强碱管道要求能承受0.001-0.5mol/L的强碱;所述反应釜中液体的pH预设值为10-14;所述第一耐酸管道要求能承受10mol/L的非氧化性强酸;所述第二耐酸管道要求能承受6mol/L的氢氟酸;所述第一酸化箱中氢氟酸的预设浓度为0.01-1mol/L;所述第一酸化箱中液体的pH预设值为0.5-1.5。 The method for extracting whole components of soil humic acid according to claim 12, wherein the alkali solution in the first dosing device is a saturated or near-saturated strong alkali solution, and the first alkali-resistant alkali pipeline is required. Capable of withstanding saturated alkali, the first alkali-resistant pipeline is required to withstand 0.001-0.5 mol/L of strong alkali; the pH of the liquid in the reactor is preset to 10-14; the first acid-resistant pipeline requires Capable of withstanding 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 first acidification tank is 0.01-1 mol/L; The pH of the liquid in the first acidification tank is preset to be 0.5-1.5.
PCT/CN2017/101707 2017-02-08 2017-09-14 Equipment for use in extracting humic acid from soil and manufacturing method for equipment WO2018145458A1 (en)

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CN201710069441.0A CN106905382B (en) 2017-02-08 2017-02-08 A kind of device of extraction soil hydrophobic humic acid
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CN106893114A (en) * 2017-02-08 2017-06-27 中国环境科学研究院 A kind of equipment for extracting soil humic acid full constituent
CN106905382A (en) * 2017-02-08 2017-06-30 中国环境科学研究院 A kind of device for extracting soil hydrophobic humic acid

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JP2004325425A (en) * 2003-04-28 2004-11-18 Silk Kogei:Kk Method of manufacturing standard powder sample of in-water fulvic acid
CN101033241A (en) * 2007-04-29 2007-09-12 晋城市炬坤生物科技有限公司 Method of preparing high-purity humic acid
CN103131023A (en) * 2013-02-06 2013-06-05 何林 Humic acid extraction novel process
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