CN112557143B - A soil sample pretreatment device for lead-zinc slay heavy metal content detects - Google Patents
A soil sample pretreatment device for lead-zinc slay heavy metal content detects Download PDFInfo
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- CN112557143B CN112557143B CN202011551444.6A CN202011551444A CN112557143B CN 112557143 B CN112557143 B CN 112557143B CN 202011551444 A CN202011551444 A CN 202011551444A CN 112557143 B CN112557143 B CN 112557143B
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Abstract
The invention discloses a soil sample pretreatment device for detecting heavy metal content in lead-zinc slag, which relates to the technical field of soil detection and comprises a microwave digestion device, a reagent adding device and an acid removing device, wherein the reagent adding device is fixedly arranged at the upper right part of the microwave digestion device, and the acid removing device is fixedly arranged at the left side of the microwave digestion device.
Description
Technical Field
The invention relates to the technical field of soil detection, in particular to a soil sample pretreatment device for detecting the heavy metal content of lead-zinc slag.
Background
Soil environment monitoring means that the environment quality (or pollution degree) and the change trend thereof are determined by measuring representative values of factors affecting the soil environment quality. Soil monitoring generally refers to soil environment monitoring, and generally comprises technical contents of distribution sampling, sample preparation, analysis methods, result characterization, data statistics, quality evaluation and the like.
The total lead and zinc yield of China in 2013 is 978 million tons, which accounts for 41 percent of the total lead and zinc yield of the world, and lead and zinc respectively live in the first production kingdom of the world for 12 years and 22 years continuously. However, the rapid development of the lead-zinc industry for many years also causes certain influence and damage to the ecological environment, and the serious prevention of heavy metal pollution becomes an insurmountable red line in the lead-zinc industry.
Along with social development, the exploitation of lead and zinc mineral products leads to environmental pollution, the soil in mining area can receive the pollution of different materials according to the difference of the mineral of adopting, heavy metal is the main form of soil pollution, nevertheless need carry out the preliminary treatment to soil when soil heavy metal detects, get rid of the interference that does not receive the testing substance as far as possible, often adopt among the prior art to clear up after the soil acidizing, nevertheless clear up and often can not integrate with dispelling sour device, lead to examining time measuring efficiency not high, consequently need an integrated device who is convenient for add reagent and dispelling sour.
Disclosure of Invention
In order to solve the technical problems, the invention provides a soil sample pretreatment device for detecting the heavy metal content of lead-zinc slag, which comprises a microwave digestion device, a reagent adding device and an acid removing device, wherein the reagent adding device is fixedly arranged at the upper right part of the microwave digestion device, the acid removing device is fixedly arranged at the left side of the microwave digestion device, the microwave digestion device comprises a digestion shell, a lifting mechanism, a stirrer, a digestion tank, a magnetron, a connecting channel, a high-voltage rectifier, a transformer, a PLC (programmable logic controller), a control panel, a digestion bin and a fixing frame, the digestion bin is fixedly connected above the lifting mechanism, the bottom of the lifting mechanism is fixedly connected with the bottom of the digestion shell, a lifting disc is hinged above the lifting mechanism, the center of the lifting disc is rotatably connected with a rotating disc, and the bottom of the rotating disc is provided with a rotating motor, the two sides of the rotating motor are fixedly connected with the bottom of the lifting disc through the fixing frame, the chuck is arranged above the rotating disc, the digesting tank is movably embedded above the chuck, the digesting tank is provided with a digesting plug, the top of the digesting shell is provided with a cover plate, the cover plate is positioned at the top of the digesting plug, a connecting pipe is vertically inserted in the cover plate, the lower end of the connecting pipe is movably inserted into the digesting tank, the stirrer is fixedly arranged on the inner wall at the rear side of the digesting bin, the magnetron is fixedly arranged above the right side of the digesting bin and is communicated with the stirrer through the connecting channel, the high-voltage rectifier is electrically connected below the magnetron, the control panel is embedded and arranged on the outer wall of the digesting shell in front of the high-voltage rectifier, the PLC controller is electrically connected below the high-voltage rectifier and is electrically connected with the control panel, and the transformer is electrically connected below the PLC controller, and is electrically connected with the high-voltage rectifier.
Further, the lifting mechanism comprises a lifting motor, a fixed disc, a screw rod and four supporting claws, the bottom of the fixed disc is fixedly connected with the digestion shell, the lifting motor is fixedly connected inside the fixed disc, the screw rod is rotatably connected above the fixed disc, the lower end of the supporting claw is in transmission connection with the lifting motor, the four supporting claws are uniformly arranged around the screw rod, each supporting claw comprises a hinged frame, a gear shaft, a bent rod and a straight rod, the bottom of the hinged frame is fixedly connected with the fixed disc, the gear shaft horizontally penetrates through the hinged frame, the gear is arranged at the center of the gear shaft and is in screw rod transmission connection with the screw rod, the near end of the bent rod is fixedly connected outside the gear shaft, the far end of the bent rod is rotatably connected with the lower end of the straight rod, the upper end of the straight rod is hinged with the bottom of the lifting disc, and after the digestion tank is lifted upwards through the lifting mechanism, an acidic reagent is added.
Further, catch up with sour device and include coupling hose, sour gas displacer, absorption tower, aspirator pump, pump machine connecting pipe, catch up with sour shell, coupling hose with the top of connecting pipe communicates with each other, the absorption tower is placed catch up with the top of sour shell, sour gas displacer fixed mounting is in the absorption tower bottom, and the upper end communicates with each other with coupling hose, aspirator pump fixed mounting catches up with the bottom of sour shell, pump machine connecting pipe lower extreme communicates with each other with the aspirator pump, and the upper end is inserted in the top of absorption tower, and communicates with each other with the absorption tower is inside, will clear up the interior acid gas of jar and shift to the absorption tower in through the aspirator pump.
Furthermore, a transparent window for replacing the absorption tower is arranged on the front surface above the acid dispelling shell, and alkaline solution in the absorption tower is replaced through the transparent window.
Further, the reagent adding device comprises a fixed rod, a rotating frame and a plurality of reagent bottles, the lower end of the fixed rod is fixedly connected with the top of the digestion shell, the center of the rotating frame is rotatably connected with the upper end of the fixed rod, the plurality of reagent bottles are placed on the outer side of the rotating frame, and samples in the digestion tank are acidified through the reagent adding device.
Furthermore, the lower end of the reagent bottle is provided with a valve for controlling the flow and the flow rate, and the speed and the dosage of the acid solution are controlled by the valve.
Furthermore, the outer side of the connecting pipe is sleeved with a plastic ring, the plastic ring is abutted to the upper surface of the digestion plug, and the plastic ring prevents acid gas from entering the digestion bin.
Furthermore, the lifting disc, the rotating disc, the digestion tank and the digestion plug are all made of high-temperature-resistant ceramic materials, and the ceramic materials can pass through microwaves and are not easy to heat.
Further, the high-temperature resistant ceramic material comprises the following components in parts by weight: 20-50 parts of fused quartz silica powder, 8-9 parts of cordierite, 3-4 parts of spodumene, 2-3 parts of clay, 2-3 parts of calcined talc, 0.5-1 part of silicon nitride, 0.2-0.5 part of tetramethylethylenediamine, 5-9 parts of zirconium dioxide powder and 2-5 parts of tungsten trioxide powder.
The preparation method of the high-temperature resistant ceramic comprises the following steps:
s1: weighing the raw materials for preparing the high-temperature resistant ceramics according to the weight parts;
s2: mixing fused quartz silica micro powder, cordierite, spodumene, clay, calcined talc, silicon nitride, zirconium dioxide powder and tungsten trioxide powder, and then putting the mixture into a ball mill to perform grinding and mixing at the speed of 30-50 r/min for 30 min;
s3: sieving the mixed powder with a 200-mesh sieve, taking undersize products, adding tetramethylethylenediamine and water, and stirring to form mud;
s4: and (3) molding the mud-shaped ceramic raw material into a mud blank with a fixed shape, and then firing at the high temperature of 1550 ℃ for 12h to obtain the high-temperature-resistant ceramic.
Further, the absorption tower is filled with alkaline absorption liquid, the alkaline absorption liquid adopts a NaOH solution with the mass fraction of 20%, and the NaOH solution and the acid gas are neutralized to further purify the acid gas.
The invention has the beneficial effects that:
(1) according to the invention, the soil sample is subjected to early treatment, the soil sample can be subjected to microwave drying, an acidic reagent is added after the soil sample is dried for acidification, the acidified soil sample is digested by microwaves, the digested gas enters the acid dispelling device for acid gas treatment, the device integrates multiple functions, and the treatment efficiency can be improved in the early treatment of the soil sample.
(2) Compared with other traditional digestion modes, the microwave digestion device has the advantages of higher microwave digestion efficiency, good digestion effect, capability of improving the accuracy of detection of the heavy metal content of the soil sample in the later period, simplicity in use and convenience in operation.
Drawings
Fig. 1 is a schematic structural view of the present invention.
Fig. 2 is a partially enlarged view of fig. 1 a according to the present invention.
Fig. 3 is a top view of the driving relationship of the support jaw and the lead screw of the present invention.
Wherein, 1-microwave digestion device, 2-reagent adding device, 3-acid removing device, 11-digestion shell, 12-lifting mechanism, 13-stirrer, 14-digestion tank, 15-magnetron, 16-connecting channel, 17-high voltage rectifier, 18-transformer, 19-PLC controller, 191-control panel, 192-digestion bin, 193-fixing frame, 121-lifting disk, 122-rotating disk, 123-rotating motor, 124-chuck, 125-lifting motor, 126-fixing disk, 127-screw rod, 128-supporting claw, 141-digestion plug, 111-cover plate, 112-connecting tube, 1121-plastic ring, 1281-hinging frame, 1282-gear, 1283-gear shaft, 1121-acid removing device, etc, 1284-bent rod, 1285-straight rod, 31-connecting hose, 32-acid gas displacer, 33-absorption tower, 34-air suction pump, 35-pump connecting pipe, 36-acid removing shell, 37-transparent window, 21-fixed rod, 22-rotating frame, 23-reagent bottle and 231-valve.
Detailed Description
Example 1: as shown in figure 1, a soil sample pretreatment device for detecting heavy metal content in lead-zinc slag comprises a microwave digestion device 1, a reagent adding device 2 and an acid removing device 3, wherein the reagent adding device 2 is fixedly arranged at the upper right side of the microwave digestion device 1, the acid removing device 3 is fixedly arranged at the left side of the microwave digestion device 1, the microwave digestion device 1 comprises a digestion shell 11, a lifting mechanism 12, a stirrer 13, a digestion tank 14, a magnetron 15, a connecting channel 16, a high-voltage rectifier 17, a transformer 18, a PLC (programmable logic controller) 19, a control panel 191, a digestion bin 192 and a fixing frame 193, the digestion bin 192 is fixedly connected above the lifting mechanism 12, the bottom of the lifting mechanism 12 is fixedly connected with the bottom of the digestion shell 11, a lifting disc 121 is hinged above the lifting mechanism 12, a rotating disc 122 is rotatably connected with the center of the lifting disc 121, a rotating motor 123 is arranged at the bottom of the rotating disc 122, the two sides of a rotating motor 123 are fixedly connected with the bottom of a lifting disc 121 through a fixing frame 193, a chuck 124 is arranged above a rotating disc 122, a digestion tank 14 is movably embedded above the chuck 124, a digestion plug 141 is arranged on the digestion tank 14, a cover plate 111 is arranged at the top of a digestion shell 11, the cover plate 111 is positioned at the top of the digestion plug 141, a connecting pipe 112 is vertically inserted in the cover plate 111, the lower end of the connecting pipe 112 is movably inserted into the digestion tank 14, a stirrer 13 is fixedly arranged on the inner wall of the rear side of the digestion tank 192, a magnetron 15 is fixedly arranged above the right side of the digestion tank 192 and is communicated with the stirrer 13 through a connecting channel 16, a high-voltage rectifier 17 is electrically connected below the magnetron 15, a control panel 191 is embedded on the outer wall of the digestion shell 11 in front of the high-voltage rectifier 17, a PLC controller 19 is electrically connected below the high-voltage rectifier 17 and is electrically connected with the control panel 191, a transformer 18 is electrically connected below the PLC controller 19, and is electrically connected with the high-voltage rectifier 17, and the lifting mechanism 12 adopts a telescopic air pressure rod for lifting.
The acid removing device 3 comprises a connecting hose 31, an acid gas displacer 32, an absorption tower 33, an air suction pump 34, a pump machine connecting pipe 35 and an acid removing shell 36, wherein the connecting hose 31 is communicated with the top of the connecting pipe 112, the absorption tower 33 is placed above the acid removing shell 36, the acid gas displacer 32 is fixedly arranged at the bottom of the absorption tower 33, the upper end of the acid gas displacer 32 is communicated with the connecting hose 31, the air suction pump 34 is fixedly arranged at the bottom of the acid removing shell 36, the lower end of the pump machine connecting pipe 35 is communicated with the air suction pump 34, the upper end of the pump machine connecting pipe 35 is inserted above the absorption tower 33 and is communicated with the inside of the absorption tower 33, and acid gas in the digestion tank 14 is transferred into the absorption tower 33 through the air suction pump 34; the front surface above the acid-removing shell 36 is provided with a transparent window 37 for replacing the absorption tower 33, and the alkaline solution in the absorption tower 33 is replaced through the transparent window 37.
Example 2:
as shown in figure 1, a soil sample pretreatment device for detecting heavy metal content in lead-zinc slag comprises a microwave digestion device 1, a reagent adding device 2 and an acid removing device 3, wherein the reagent adding device 2 is fixedly arranged at the upper right side of the microwave digestion device 1, the acid removing device 3 is fixedly arranged at the left side of the microwave digestion device 1, the microwave digestion device 1 comprises a digestion shell 11, a lifting mechanism 12, a stirrer 13, a digestion tank 14, a magnetron 15, a connecting channel 16, a high-voltage rectifier 17, a transformer 18, a PLC (programmable logic controller) 19, a control panel 191, a digestion bin 192 and a fixing frame 193, the digestion bin 192 is fixedly connected above the lifting mechanism 12, the bottom of the lifting mechanism 12 is fixedly connected with the bottom of the digestion shell 11, a lifting disc 121 is hinged above the lifting mechanism 12, a rotating disc 122 is rotatably connected with the center of the lifting disc 121, a rotating motor 123 is arranged at the bottom of the rotating disc 122, the two sides of a rotating motor 123 are fixedly connected with the bottom of a lifting disc 121 through a fixing frame 193, a chuck 124 is arranged above a rotating disc 122, a digestion tank 14 is movably embedded above the chuck 124, a digestion plug 141 is arranged on the digestion tank 14, a cover plate 111 is arranged at the top of a digestion shell 11, the cover plate 111 is positioned at the top of the digestion plug 141, a connecting pipe 112 is vertically inserted in the cover plate 111, the lower end of the connecting pipe 112 is movably inserted into the digestion tank 14, a stirrer 13 is fixedly arranged on the inner wall of the rear side of the digestion tank 192, a magnetron 15 is fixedly arranged above the right side of the digestion tank 192 and is communicated with the stirrer 13 through a connecting channel 16, a high-voltage rectifier 17 is electrically connected below the magnetron 15, a control panel 191 is embedded on the outer wall of the digestion shell 11 in front of the high-voltage rectifier 17, a PLC controller 19 is electrically connected below the high-voltage rectifier 17 and is electrically connected with the control panel 191, a transformer 18 is electrically connected below the PLC controller 19, and is electrically connected to the high voltage rectifier 17.
As shown in fig. 2-3, the lifting mechanism 12 includes a lifting motor 125, a fixed plate 126, a lead screw 127, four support claws 128, the bottom of the fixed plate 126 is fixedly connected with the digestion shell 11, the lifting motor 125 is fixedly connected inside the fixed plate 126, the lead screw 127 is rotatably connected above the fixed plate 126, and the lower end of the lead screw is in transmission connection with the lifting motor 125, four support claws 128 are uniformly installed around the lead screw 127, each support claw 128 includes a hinge frame 1281, a gear 1282, a gear shaft 1283, a bent rod 1284 and a straight rod 1285, the bottom of the hinge frame 1281 is fixedly connected with the fixed plate 126, the gear 1283 horizontally passes through the hinge frame 1281, the gear 1282 is installed at the center of the gear 1283 and is in transmission connection with the lead screw 127, the proximal end of the bent rod 1284 is fixedly connected outside the gear 1283, the distal end of the bent rod 1284 is rotatably connected with the lower end of the straight rod 1285, the upper end of the straight rod 1285 is hinged with the bottom of the lifting plate 121, after the digestion tank 14 is lifted up by the elevator mechanism 12, an acidic reagent is added.
The acid removing device 3 comprises a connecting hose 31, an acid gas displacer 32, an absorption tower 33, an air suction pump 34, a pump machine connecting pipe 35 and an acid removing shell 36, wherein the connecting hose 31 is communicated with the top of the connecting pipe 112, the absorption tower 33 is placed above the acid removing shell 36, the acid gas displacer 32 is fixedly arranged at the bottom of the absorption tower 33, the upper end of the acid gas displacer 32 is communicated with the connecting hose 31, the air suction pump 34 is fixedly arranged at the bottom of the acid removing shell 36, the lower end of the pump machine connecting pipe 35 is communicated with the air suction pump 34, the upper end of the pump machine connecting pipe 35 is inserted above the absorption tower 33 and is communicated with the inside of the absorption tower 33, and acid gas in the digestion tank 14 is transferred into the absorption tower 33 through the air suction pump 34; the front surface above the acid-removing shell 36 is provided with a transparent window 37 for replacing the absorption tower 33, and the alkaline solution in the absorption tower 33 is replaced through the transparent window 37.
Embodiment 1 compares with embodiment 2, and embodiment 1's elevating system 12 adopts pneumatic lifter to go up and down, needs the air pump cooperation to use, and occupation space, and embodiment 1 is more steady in the elevating system 12 lift process among embodiment 2, and does not need the air pump cooperation to use, and occupation space is little.
Example 3:
as shown in figure 1, a soil sample pretreatment device for detecting heavy metal content in lead-zinc slag comprises a microwave digestion device 1, a reagent adding device 2 and an acid removing device 3, wherein the reagent adding device 2 is fixedly arranged at the upper right side of the microwave digestion device 1, the acid removing device 3 is fixedly arranged at the left side of the microwave digestion device 1, the microwave digestion device 1 comprises a digestion shell 11, a lifting mechanism 12, a stirrer 13, a digestion tank 14, a magnetron 15, a connecting channel 16, a high-voltage rectifier 17, a transformer 18, a PLC (programmable logic controller) 19, a control panel 191, a digestion bin 192 and a fixing frame 193, the digestion bin 192 is fixedly connected above the lifting mechanism 12, the bottom of the lifting mechanism 12 is fixedly connected with the bottom of the digestion shell 11, a lifting disc 121 is hinged above the lifting mechanism 12, a rotating disc 122 is rotatably connected with the center of the lifting disc 121, a rotating motor 123 is arranged at the bottom of the rotating disc 122, the two sides of a rotating motor 123 are fixedly connected with the bottom of a lifting disc 121 through a fixing frame 193, a chuck 124 is arranged above a rotating disc 122, a digestion tank 14 is movably embedded above the chuck 124, a digestion plug 141 is arranged on the digestion tank 14, a cover plate 111 is arranged at the top of a digestion shell 11, the cover plate 111 is positioned at the top of the digestion plug 141, a connecting pipe 112 is vertically inserted in the cover plate 111, the lower end of the connecting pipe 112 is movably inserted into the digestion tank 14, a plastic ring 1121 is sleeved outside the connecting pipe 112, the plastic ring 1121 is abutted against the upper surface of the digestion plug 141, the plastic ring 1121 prevents acid gas from entering the digestion bin 192, a stirrer 13 is fixedly arranged on the inner wall at the rear side of the digestion bin 192, a magnetron 15 is fixedly arranged above the right side of the digestion bin 192 and communicated with the stirrer 13 through a connecting channel 16, a high-voltage rectifier 17 is electrically connected below the magnetron 15, and a control panel 191 is embedded on the outer wall of the digestion shell 11 in front of the high-voltage rectifier 17, the PLC controller 19 is electrically connected to the lower portion of the high voltage rectifier 17 and electrically connected to the control panel 191, and the transformer 18 is electrically connected to the lower portion of the PLC controller 19 and electrically connected to the high voltage rectifier 17.
As shown in fig. 2-3, the lifting mechanism 12 includes a lifting motor 125, a fixed plate 126, a lead screw 127, four support claws 128, the bottom of the fixed plate 126 is fixedly connected with the digestion shell 11, the lifting motor 125 is fixedly connected inside the fixed plate 126, the lead screw 127 is rotatably connected above the fixed plate 126, and the lower end of the lead screw is in transmission connection with the lifting motor 125, four support claws 128 are uniformly installed around the lead screw 127, each support claw 128 includes a hinge frame 1281, a gear 1282, a gear shaft 1283, a bent rod 1284 and a straight rod 1285, the bottom of the hinge frame 1281 is fixedly connected with the fixed plate 126, the gear 1283 horizontally passes through the hinge frame 1281, the gear 1282 is installed at the center of the gear 1283 and is in transmission connection with the lead screw 127, the proximal end of the bent rod 1284 is fixedly connected outside the gear 1283, the distal end of the bent rod 1284 is rotatably connected with the lower end of the straight rod 1285, the upper end of the straight rod 1285 is hinged with the bottom of the lifting plate 121, after the digestion tank 14 is lifted up by the elevator mechanism 12, an acidic reagent is added.
The acid removing device 3 comprises a connecting hose 31, an acid gas displacer 32, an absorption tower 33, an air suction pump 34, a pump machine connecting pipe 35 and an acid removing shell 36, wherein the connecting hose 31 is communicated with the top of the connecting pipe 112, the absorption tower 33 is placed above the acid removing shell 36, the acid gas displacer 32 is fixedly arranged at the bottom of the absorption tower 33, the upper end of the acid gas displacer 32 is communicated with the connecting hose 31, the air suction pump 34 is fixedly arranged at the bottom of the acid removing shell 36, the lower end of the pump machine connecting pipe 35 is communicated with the air suction pump 34, the upper end of the pump machine connecting pipe 35 is inserted above the absorption tower 33 and is communicated with the inside of the absorption tower 33, and acid gas in the digestion tank 14 is transferred into the absorption tower 33 through the air suction pump 34; the front surface above the acid-removing shell 36 is provided with a transparent window 37 for replacing the absorption tower 33, and the alkaline solution in the absorption tower 33 is replaced through the transparent window 37.
Compared with embodiment 3, in embodiment 2, the air leakage prevention plastic ring 1121 is added to the outer side of the connecting pipe 112, so that the acid gas can be effectively prevented from entering the digestion chamber 192.
Example 4:
as shown in figure 1, a soil sample pretreatment device for detecting heavy metal content in lead-zinc slag comprises a microwave digestion device 1, a reagent adding device 2 and an acid removing device 3, wherein the reagent adding device 2 is fixedly arranged at the upper right side of the microwave digestion device 1, the acid removing device 3 is fixedly arranged at the left side of the microwave digestion device 1, the microwave digestion device 1 comprises a digestion shell 11, a lifting mechanism 12, a stirrer 13, a digestion tank 14, a magnetron 15, a connecting channel 16, a high-voltage rectifier 17, a transformer 18, a PLC (programmable logic controller) 19, a control panel 191, a digestion bin 192 and a fixing frame 193, the digestion bin 192 is fixedly connected above the lifting mechanism 12, the bottom of the lifting mechanism 12 is fixedly connected with the bottom of the digestion shell 11, a lifting disc 121 is hinged above the lifting mechanism 12, a rotating disc 122 is rotatably connected with the center of the lifting disc 121, a rotating motor 123 is arranged at the bottom of the rotating disc 122, the two sides of a rotating motor 123 are fixedly connected with the bottom of a lifting disc 121 through a fixing frame 193, a chuck 124 is arranged above a rotating disc 122, a digestion tank 14 is movably embedded above the chuck 124, a digestion plug 141 is arranged on the digestion tank 14, a cover plate 111 is arranged at the top of a digestion shell 11, the cover plate 111 is positioned at the top of the digestion plug 141, a connecting pipe 112 is vertically inserted in the cover plate 111, the lower end of the connecting pipe 112 is movably inserted into the digestion tank 14, a plastic ring 1121 is sleeved outside the connecting pipe 112, the plastic ring 1121 is abutted against the upper surface of the digestion plug 141, the plastic ring 1121 prevents acid gas from entering the digestion bin 192, a stirrer 13 is fixedly arranged on the inner wall at the rear side of the digestion bin 192, a magnetron 15 is fixedly arranged above the right side of the digestion bin 192 and communicated with the stirrer 13 through a connecting channel 16, a high-voltage rectifier 17 is electrically connected below the magnetron 15, and a control panel 191 is embedded on the outer wall of the digestion shell 11 in front of the high-voltage rectifier 17, the PLC controller 19 is electrically connected to the lower portion of the high voltage rectifier 17 and electrically connected to the control panel 191, and the transformer 18 is electrically connected to the lower portion of the PLC controller 19 and electrically connected to the high voltage rectifier 17.
As shown in fig. 2-3, the lifting mechanism 12 includes a lifting motor 125, a fixed plate 126, a lead screw 127, four support claws 128, the bottom of the fixed plate 126 is fixedly connected with the digestion shell 11, the lifting motor 125 is fixedly connected inside the fixed plate 126, the lead screw 127 is rotatably connected above the fixed plate 126, and the lower end of the lead screw is in transmission connection with the lifting motor 125, four support claws 128 are uniformly installed around the lead screw 127, each support claw 128 includes a hinge frame 1281, a gear 1282, a gear shaft 1283, a bent rod 1284 and a straight rod 1285, the bottom of the hinge frame 1281 is fixedly connected with the fixed plate 126, the gear 1283 horizontally passes through the hinge frame 1281, the gear 1282 is installed at the center of the gear 1283 and is in transmission connection with the lead screw 127, the proximal end of the bent rod 1284 is fixedly connected outside the gear 1283, the distal end of the bent rod 1284 is rotatably connected with the lower end of the straight rod 1285, the upper end of the straight rod 1285 is hinged with the bottom of the lifting plate 121, after the digestion tank 14 is lifted up by the elevator mechanism 12, an acidic reagent is added.
The acid removing device 3 comprises a connecting hose 31, an acid gas displacer 32, an absorption tower 33, an air suction pump 34, a pump machine connecting pipe 35 and an acid removing shell 36, wherein the connecting hose 31 is communicated with the top of the connecting pipe 112, the absorption tower 33 is placed above the acid removing shell 36, the acid gas displacer 32 is fixedly arranged at the bottom of the absorption tower 33, the upper end of the acid gas displacer 32 is communicated with the connecting hose 31, the air suction pump 34 is fixedly arranged at the bottom of the acid removing shell 36, the lower end of the pump machine connecting pipe 35 is communicated with the air suction pump 34, the upper end of the pump machine connecting pipe 35 is inserted above the absorption tower 33 and is communicated with the inside of the absorption tower 33, and acid gas in the digestion tank 14 is transferred into the absorption tower 33 through the air suction pump 34; the front surface above the acid removing shell 36 is provided with a transparent window 37 for replacing the absorption tower 33, the alkaline solution in the absorption tower 33 is replaced through the transparent window 37, the absorption tower 33 is filled with the alkaline absorption liquid, the alkaline absorption liquid adopts a NaOH solution with the mass fraction of 20%, and the NaOH solution and the acid gas are neutralized to purify the acid gas.
In example 3, compared with example 4, the alkaline solution filled in the absorption tower 33 of example 4 is a 20% NaOH solution, and the reaction with the acid gas is stronger with the 20% NaOH solution than with other alkaline solutions, thereby increasing the purification rate of the acid gas.
Example 5:
as shown in figure 1, a soil sample pretreatment device for detecting heavy metal content in lead-zinc slag comprises a microwave digestion device 1, a reagent adding device 2 and an acid removing device 3, wherein the reagent adding device 2 is fixedly arranged at the upper right side of the microwave digestion device 1, the acid removing device 3 is fixedly arranged at the left side of the microwave digestion device 1, the microwave digestion device 1 comprises a digestion shell 11, a lifting mechanism 12, a stirrer 13, a digestion tank 14, a magnetron 15, a connecting channel 16, a high-voltage rectifier 17, a transformer 18, a PLC (programmable logic controller) 19, a control panel 191, a digestion bin 192 and a fixing frame 193, the digestion bin 192 is fixedly connected above the lifting mechanism 12, the bottom of the lifting mechanism 12 is fixedly connected with the bottom of the digestion shell 11, a lifting disc 121 is hinged above the lifting mechanism 12, a rotating disc 122 is rotatably connected with the center of the lifting disc 121, a rotating motor 123 is arranged at the bottom of the rotating disc 122, the two sides of a rotating motor 123 are fixedly connected with the bottom of a lifting disc 121 through a fixing frame 193, a chuck 124 is arranged above a rotating disc 122, a digestion tank 14 is movably embedded above the chuck 124, a digestion plug 141 is arranged on the digestion tank 14, a cover plate 111 is arranged at the top of a digestion shell 11, the cover plate 111 is positioned at the top of the digestion plug 141, a connecting pipe 112 is vertically inserted in the cover plate 111, the lower end of the connecting pipe 112 is movably inserted into the digestion tank 14, a plastic ring 1121 is sleeved outside the connecting pipe 112, the plastic ring 1121 is abutted against the upper surface of the digestion plug 141, the plastic ring 1121 prevents acid gas from entering the digestion bin 192, a stirrer 13 is fixedly arranged on the inner wall at the rear side of the digestion bin 192, a magnetron 15 is fixedly arranged above the right side of the digestion bin 192 and communicated with the stirrer 13 through a connecting channel 16, a high-voltage rectifier 17 is electrically connected below the magnetron 15, and a control panel 191 is embedded on the outer wall of the digestion shell 11 in front of the high-voltage rectifier 17, the PLC controller 19 is electrically connected to the lower portion of the high voltage rectifier 17 and electrically connected to the control panel 191, and the transformer 18 is electrically connected to the lower portion of the PLC controller 19 and electrically connected to the high voltage rectifier 17.
As shown in fig. 2-3, the lifting mechanism 12 includes a lifting motor 125, a fixed plate 126, a lead screw 127, four support claws 128, the bottom of the fixed plate 126 is fixedly connected with the digestion shell 11, the lifting motor 125 is fixedly connected inside the fixed plate 126, the lead screw 127 is rotatably connected above the fixed plate 126, and the lower end of the lead screw is in transmission connection with the lifting motor 125, four support claws 128 are uniformly installed around the lead screw 127, each support claw 128 includes a hinge frame 1281, a gear 1282, a gear shaft 1283, a bent rod 1284 and a straight rod 1285, the bottom of the hinge frame 1281 is fixedly connected with the fixed plate 126, the gear 1283 horizontally passes through the hinge frame 1281, the gear 1282 is installed at the center of the gear 1283 and is in transmission connection with the lead screw 127, the proximal end of the bent rod 1284 is fixedly connected outside the gear 1283, the distal end of the bent rod 1284 is rotatably connected with the lower end of the straight rod 1285, the upper end of the straight rod 1285 is hinged with the bottom of the lifting plate 121, after the digestion tank 14 is lifted up by the elevator mechanism 12, an acidic reagent is added.
The acid removing device 3 comprises a connecting hose 31, an acid gas displacer 32, an absorption tower 33, an air suction pump 34, a pump machine connecting pipe 35 and an acid removing shell 36, wherein the connecting hose 31 is communicated with the top of the connecting pipe 112, the absorption tower 33 is placed above the acid removing shell 36, the acid gas displacer 32 is fixedly arranged at the bottom of the absorption tower 33, the upper end of the acid gas displacer 32 is communicated with the connecting hose 31, the air suction pump 34 is fixedly arranged at the bottom of the acid removing shell 36, the lower end of the pump machine connecting pipe 35 is communicated with the air suction pump 34, the upper end of the pump machine connecting pipe 35 is inserted above the absorption tower 33 and is communicated with the inside of the absorption tower 33, and acid gas in the digestion tank 14 is transferred into the absorption tower 33 through the air suction pump 34; the front surface above the acid removing shell 36 is provided with a transparent window 37 for replacing the absorption tower 33, the alkaline solution in the absorption tower 33 is replaced through the transparent window 37, the absorption tower 33 is filled with the alkaline absorption liquid, the alkaline absorption liquid adopts a NaOH solution with the mass fraction of 20%, and the NaOH solution and the acid gas are neutralized to purify the acid gas.
The reagent adding device 2 comprises a fixed rod 21, a rotating frame 22 and a plurality of reagent bottles 23, the lower end of the fixed rod 21 is fixedly connected with the top of the digestion shell 11, the center of the rotating frame 22 is rotatably connected with the upper end of the fixed rod 21, the plurality of reagent bottles 23 are arranged on the outer side of the rotating frame 22, and the reagent adding device 2 is used for acidifying the samples in the digestion tank 14; the lower end of the reagent bottle 23 is provided with a valve 231 for controlling the flow rate and flow rate, and the speed and dosage of the acid solution is controlled by the valve 231.
Example 4 compared with example 5, in example 5, the valve 231 is added to the bottom of the reagent bottle 23, and the speed and the amount of the acid solution to be dropped are controlled and controlled by the valve 231, so that compared with example 4, the time and the labor are saved when the acid reagent is added.
Example 6:
as shown in figure 1, a soil sample pretreatment device for detecting heavy metal content in lead-zinc slag comprises a microwave digestion device 1, a reagent adding device 2 and an acid removing device 3, wherein the reagent adding device 2 is fixedly arranged at the upper right side of the microwave digestion device 1, the acid removing device 3 is fixedly arranged at the left side of the microwave digestion device 1, the microwave digestion device 1 comprises a digestion shell 11, a lifting mechanism 12, a stirrer 13, a digestion tank 14, a magnetron 15, a connecting channel 16, a high-voltage rectifier 17, a transformer 18, a PLC (programmable logic controller) 19, a control panel 191, a digestion bin 192 and a fixing frame 193, the digestion bin 192 is fixedly connected above the lifting mechanism 12, the bottom of the lifting mechanism 12 is fixedly connected with the bottom of the digestion shell 11, a lifting disc 121 is hinged above the lifting mechanism 12, a rotating disc 122 is rotatably connected with the center of the lifting disc 121, a rotating motor 123 is arranged at the bottom of the rotating disc 122, the two sides of a rotating motor 123 are fixedly connected with the bottom of a lifting disc 121 through a fixing frame 193, a chuck 124 is arranged above a rotating disc 122, a digestion tank 14 is movably embedded above the chuck 124, a digestion plug 141 is arranged on the digestion tank 14, a cover plate 111 is arranged at the top of a digestion shell 11, the cover plate 111 is positioned at the top of the digestion plug 141, a connecting pipe 112 is vertically inserted in the cover plate 111, the lower end of the connecting pipe 112 is movably inserted into the digestion tank 14, a plastic ring 1121 is sleeved outside the connecting pipe 112, the plastic ring 1121 is abutted against the upper surface of the digestion plug 141, the plastic ring 1121 prevents acid gas from entering the digestion bin 192, a stirrer 13 is fixedly arranged on the inner wall at the rear side of the digestion bin 192, a magnetron 15 is fixedly arranged above the right side of the digestion bin 192 and communicated with the stirrer 13 through a connecting channel 16, a high-voltage rectifier 17 is electrically connected below the magnetron 15, and a control panel 191 is embedded on the outer wall of the digestion shell 11 in front of the high-voltage rectifier 17, the PLC controller 19 is electrically connected to the lower portion of the high voltage rectifier 17 and electrically connected to the control panel 191, and the transformer 18 is electrically connected to the lower portion of the PLC controller 19 and electrically connected to the high voltage rectifier 17.
As shown in fig. 2-3, the lifting mechanism 12 includes a lifting motor 125, a fixed plate 126, a lead screw 127, four support claws 128, the bottom of the fixed plate 126 is fixedly connected with the digestion shell 11, the lifting motor 125 is fixedly connected inside the fixed plate 126, the lead screw 127 is rotatably connected above the fixed plate 126, and the lower end of the lead screw is in transmission connection with the lifting motor 125, four support claws 128 are uniformly installed around the lead screw 127, each support claw 128 includes a hinge frame 1281, a gear 1282, a gear shaft 1283, a bent rod 1284 and a straight rod 1285, the bottom of the hinge frame 1281 is fixedly connected with the fixed plate 126, the gear 1283 horizontally passes through the hinge frame 1281, the gear 1282 is installed at the center of the gear 1283 and is in transmission connection with the lead screw 127, the proximal end of the bent rod 1284 is fixedly connected outside the gear 1283, the distal end of the bent rod 1284 is rotatably connected with the lower end of the straight rod 1285, the upper end of the straight rod 1285 is hinged with the bottom of the lifting plate 121, after the digestion tank 14 is lifted up by the elevator mechanism 12, an acidic reagent is added.
The lifting disc 121, the rotating disc 122, the digestion tank 14 and the digestion plug 141 are all made of high-temperature-resistant ceramic materials, the ceramic materials can pass through microwaves and are not prone to heating, and the high-temperature-resistant ceramic materials are composed of the following components in parts by weight: the ceramic material comprises 20 parts of fused silica micropowder, 8 parts of cordierite, 3 parts of spodumene, 2 parts of clay, 2 parts of calcined talc, 0.5 part of silicon nitride, 0.2 part of tetramethylethylenediamine, 5 parts of zirconium dioxide powder and 2 parts of tungsten trioxide powder, and has high temperature resistance, can pass microwaves and is not easy to generate heat in a microwave environment;
the preparation method of the high-temperature resistant ceramic comprises the following steps:
s1: weighing the raw materials for preparing the high-temperature resistant ceramics according to the weight parts;
s2: mixing fused quartz silica micropowder, cordierite, spodumene, clay, calcined talc, silicon nitride, zirconium dioxide powder and tungsten trioxide powder, and putting the mixture into a ball mill for grinding and mixing at 30r/min for 30 min;
s3: sieving the mixed powder with a 200-mesh sieve, taking undersize products, adding tetramethylethylenediamine and water, and stirring to form mud;
s4: and (3) molding the mud-shaped ceramic raw material into a mud blank with a fixed shape, and then firing at the high temperature of 1550 ℃ for 12h to obtain the high-temperature-resistant ceramic.
The acid removing device 3 comprises a connecting hose 31, an acid gas displacer 32, an absorption tower 33, an air suction pump 34, a pump machine connecting pipe 35 and an acid removing shell 36, wherein the connecting hose 31 is communicated with the top of the connecting pipe 112, the absorption tower 33 is placed above the acid removing shell 36, the acid gas displacer 32 is fixedly arranged at the bottom of the absorption tower 33, the upper end of the acid gas displacer 32 is communicated with the connecting hose 31, the air suction pump 34 is fixedly arranged at the bottom of the acid removing shell 36, the lower end of the pump machine connecting pipe 35 is communicated with the air suction pump 34, the upper end of the pump machine connecting pipe 35 is inserted above the absorption tower 33 and is communicated with the inside of the absorption tower 33, and acid gas in the digestion tank 14 is transferred into the absorption tower 33 through the air suction pump 34; the front surface above the acid removing shell 36 is provided with a transparent window 37 for replacing the absorption tower 33, the alkaline solution in the absorption tower 33 is replaced through the transparent window 37, the absorption tower 33 is filled with the alkaline absorption liquid, the alkaline absorption liquid adopts a NaOH solution with the mass fraction of 20%, and the NaOH solution and the acid gas are neutralized to purify the acid gas.
The reagent adding device 2 comprises a fixed rod 21, a rotating frame 22 and a plurality of reagent bottles 23, the lower end of the fixed rod 21 is fixedly connected with the top of the digestion shell 11, the center of the rotating frame 22 is rotatably connected with the upper end of the fixed rod 21, the plurality of reagent bottles 23 are arranged on the outer side of the rotating frame 22, and the reagent adding device 2 is used for acidifying the samples in the digestion tank 14; the lower end of the reagent bottle 23 is provided with a valve 231 for controlling the flow rate and flow rate, and the speed and dosage of the acid solution is controlled by the valve 231.
Example 7:
as shown in figure 1, a soil sample pretreatment device for detecting heavy metal content in lead-zinc slag comprises a microwave digestion device 1, a reagent adding device 2 and an acid removing device 3, wherein the reagent adding device 2 is fixedly arranged at the upper right side of the microwave digestion device 1, the acid removing device 3 is fixedly arranged at the left side of the microwave digestion device 1, the microwave digestion device 1 comprises a digestion shell 11, a lifting mechanism 12, a stirrer 13, a digestion tank 14, a magnetron 15, a connecting channel 16, a high-voltage rectifier 17, a transformer 18, a PLC (programmable logic controller) 19, a control panel 191, a digestion bin 192 and a fixing frame 193, the digestion bin 192 is fixedly connected above the lifting mechanism 12, the bottom of the lifting mechanism 12 is fixedly connected with the bottom of the digestion shell 11, a lifting disc 121 is hinged above the lifting mechanism 12, a rotating disc 122 is rotatably connected with the center of the lifting disc 121, a rotating motor 123 is arranged at the bottom of the rotating disc 122, the two sides of a rotating motor 123 are fixedly connected with the bottom of a lifting disc 121 through a fixing frame 193, a chuck 124 is arranged above a rotating disc 122, a digestion tank 14 is movably embedded above the chuck 124, a digestion plug 141 is arranged on the digestion tank 14, a cover plate 111 is arranged at the top of a digestion shell 11, the cover plate 111 is positioned at the top of the digestion plug 141, a connecting pipe 112 is vertically inserted in the cover plate 111, the lower end of the connecting pipe 112 is movably inserted into the digestion tank 14, a plastic ring 1121 is sleeved outside the connecting pipe 112, the plastic ring 1121 is abutted against the upper surface of the digestion plug 141, the plastic ring 1121 prevents acid gas from entering the digestion bin 192, a stirrer 13 is fixedly arranged on the inner wall at the rear side of the digestion bin 192, a magnetron 15 is fixedly arranged above the right side of the digestion bin 192 and communicated with the stirrer 13 through a connecting channel 16, a high-voltage rectifier 17 is electrically connected below the magnetron 15, and a control panel 191 is embedded on the outer wall of the digestion shell 11 in front of the high-voltage rectifier 17, the PLC controller 19 is electrically connected to the lower portion of the high voltage rectifier 17 and electrically connected to the control panel 191, and the transformer 18 is electrically connected to the lower portion of the PLC controller 19 and electrically connected to the high voltage rectifier 17.
As shown in fig. 2-3, the lifting mechanism 12 includes a lifting motor 125, a fixed plate 126, a lead screw 127, four support claws 128, the bottom of the fixed plate 126 is fixedly connected with the digestion shell 11, the lifting motor 125 is fixedly connected inside the fixed plate 126, the lead screw 127 is rotatably connected above the fixed plate 126, and the lower end of the lead screw is in transmission connection with the lifting motor 125, four support claws 128 are uniformly installed around the lead screw 127, each support claw 128 includes a hinge frame 1281, a gear 1282, a gear shaft 1283, a bent rod 1284 and a straight rod 1285, the bottom of the hinge frame 1281 is fixedly connected with the fixed plate 126, the gear 1283 horizontally passes through the hinge frame 1281, the gear 1282 is installed at the center of the gear 1283 and is in transmission connection with the lead screw 127, the proximal end of the bent rod 1284 is fixedly connected outside the gear 1283, the distal end of the bent rod 1284 is rotatably connected with the lower end of the straight rod 1285, the upper end of the straight rod 1285 is hinged with the bottom of the lifting plate 121, after the digestion tank 14 is lifted up by the elevator mechanism 12, an acidic reagent is added.
The lifting disc 121, the rotating disc 122, the digestion tank 14 and the digestion plug 141 are all made of high-temperature-resistant ceramic materials, the ceramic materials can pass through microwaves and are not prone to heating, and the high-temperature-resistant ceramic materials are composed of the following components in parts by weight: the ceramic material comprises 40 parts of fused quartz silica micropowder, 8.5 parts of cordierite, 3.5 parts of spodumene, 2.5 parts of clay, 2.5 parts of calcined talc, 0.8 part of silicon nitride, 0.3 part of tetramethyl ethylenediamine, 7 parts of zirconium dioxide powder and 3 parts of tungsten trioxide powder, and has the advantages of high temperature resistance, microwave passing capability and difficult heating in a microwave environment;
the preparation method of the high-temperature resistant ceramic comprises the following steps:
s1: weighing the raw materials for preparing the high-temperature resistant ceramics according to the weight parts;
s2: mixing fused quartz silica micropowder, cordierite, spodumene, clay, calcined talc, silicon nitride, zirconium dioxide powder and tungsten trioxide powder, and putting the mixture into a ball mill for grinding and mixing at the speed of 40r/min for 30 min;
s3: sieving the mixed powder with a 200-mesh sieve, taking undersize products, adding tetramethylethylenediamine and water, and stirring to form mud;
s4: and (3) molding the mud-shaped ceramic raw material into a mud blank with a fixed shape, and then firing at the high temperature of 1550 ℃ for 12h to obtain the high-temperature-resistant ceramic.
The acid removing device 3 comprises a connecting hose 31, an acid gas displacer 32, an absorption tower 33, an air suction pump 34, a pump machine connecting pipe 35 and an acid removing shell 36, wherein the connecting hose 31 is communicated with the top of the connecting pipe 112, the absorption tower 33 is placed above the acid removing shell 36, the acid gas displacer 32 is fixedly arranged at the bottom of the absorption tower 33, the upper end of the acid gas displacer 32 is communicated with the connecting hose 31, the air suction pump 34 is fixedly arranged at the bottom of the acid removing shell 36, the lower end of the pump machine connecting pipe 35 is communicated with the air suction pump 34, the upper end of the pump machine connecting pipe 35 is inserted above the absorption tower 33 and is communicated with the inside of the absorption tower 33, and acid gas in the digestion tank 14 is transferred into the absorption tower 33 through the air suction pump 34; the front surface above the acid removing shell 36 is provided with a transparent window 37 for replacing the absorption tower 33, the alkaline solution in the absorption tower 33 is replaced through the transparent window 37, the absorption tower 33 is filled with the alkaline absorption liquid, the alkaline absorption liquid adopts a NaOH solution with the mass fraction of 20%, and the NaOH solution and the acid gas are neutralized to purify the acid gas.
The reagent adding device 2 comprises a fixed rod 21, a rotating frame 22 and a plurality of reagent bottles 23, the lower end of the fixed rod 21 is fixedly connected with the top of the digestion shell 11, the center of the rotating frame 22 is rotatably connected with the upper end of the fixed rod 21, the plurality of reagent bottles 23 are arranged on the outer side of the rotating frame 22, and the reagent adding device 2 is used for acidifying the samples in the digestion tank 14; the lower end of the reagent bottle 23 is provided with a valve 231 for controlling the flow rate and flow rate, and the speed and dosage of the acid solution is controlled by the valve 231.
Example 8:
as shown in figure 1, a soil sample pretreatment device for detecting heavy metal content in lead-zinc slag comprises a microwave digestion device 1, a reagent adding device 2 and an acid removing device 3, wherein the reagent adding device 2 is fixedly arranged at the upper right side of the microwave digestion device 1, the acid removing device 3 is fixedly arranged at the left side of the microwave digestion device 1, the microwave digestion device 1 comprises a digestion shell 11, a lifting mechanism 12, a stirrer 13, a digestion tank 14, a magnetron 15, a connecting channel 16, a high-voltage rectifier 17, a transformer 18, a PLC (programmable logic controller) 19, a control panel 191, a digestion bin 192 and a fixing frame 193, the digestion bin 192 is fixedly connected above the lifting mechanism 12, the bottom of the lifting mechanism 12 is fixedly connected with the bottom of the digestion shell 11, a lifting disc 121 is hinged above the lifting mechanism 12, a rotating disc 122 is rotatably connected with the center of the lifting disc 121, a rotating motor 123 is arranged at the bottom of the rotating disc 122, the two sides of a rotating motor 123 are fixedly connected with the bottom of a lifting disc 121 through a fixing frame 193, a chuck 124 is arranged above a rotating disc 122, a digestion tank 14 is movably embedded above the chuck 124, a digestion plug 141 is arranged on the digestion tank 14, a cover plate 111 is arranged at the top of a digestion shell 11, the cover plate 111 is positioned at the top of the digestion plug 141, a connecting pipe 112 is vertically inserted in the cover plate 111, the lower end of the connecting pipe 112 is movably inserted into the digestion tank 14, a plastic ring 1121 is sleeved outside the connecting pipe 112, the plastic ring 1121 is abutted against the upper surface of the digestion plug 141, the plastic ring 1121 prevents acid gas from entering the digestion bin 192, a stirrer 13 is fixedly arranged on the inner wall at the rear side of the digestion bin 192, a magnetron 15 is fixedly arranged above the right side of the digestion bin 192 and communicated with the stirrer 13 through a connecting channel 16, a high-voltage rectifier 17 is electrically connected below the magnetron 15, and a control panel 191 is embedded on the outer wall of the digestion shell 11 in front of the high-voltage rectifier 17, the PLC controller 19 is electrically connected to the lower portion of the high voltage rectifier 17 and electrically connected to the control panel 191, and the transformer 18 is electrically connected to the lower portion of the PLC controller 19 and electrically connected to the high voltage rectifier 17.
As shown in fig. 2-3, the lifting mechanism 12 includes a lifting motor 125, a fixed plate 126, a lead screw 127, four support claws 128, the bottom of the fixed plate 126 is fixedly connected with the digestion shell 11, the lifting motor 125 is fixedly connected inside the fixed plate 126, the lead screw 127 is rotatably connected above the fixed plate 126, and the lower end of the lead screw is in transmission connection with the lifting motor 125, four support claws 128 are uniformly installed around the lead screw 127, each support claw 128 includes a hinge frame 1281, a gear 1282, a gear shaft 1283, a bent rod 1284 and a straight rod 1285, the bottom of the hinge frame 1281 is fixedly connected with the fixed plate 126, the gear 1283 horizontally passes through the hinge frame 1281, the gear 1282 is installed at the center of the gear 1283 and is in transmission connection with the lead screw 127, the proximal end of the bent rod 1284 is fixedly connected outside the gear 1283, the distal end of the bent rod 1284 is rotatably connected with the lower end of the straight rod 1285, the upper end of the straight rod 1285 is hinged with the bottom of the lifting plate 121, after the digestion tank 14 is lifted up by the elevator mechanism 12, an acidic reagent is added.
The lifting disc 121, the rotating disc 122, the digestion tank 14 and the digestion plug 141 are all made of high-temperature-resistant ceramic materials, the ceramic materials can pass through microwaves and are not prone to heating, and the high-temperature-resistant ceramic materials are composed of the following components in parts by weight: the ceramic material comprises 50 parts of fused quartz silica micropowder, 9 parts of cordierite, 4 parts of spodumene, 3 parts of clay, 3 parts of calcined talc, 1 part of silicon nitride, 0.5 part of tetramethylethylenediamine, 9 parts of zirconium dioxide powder and 5 parts of tungsten trioxide powder, and has high temperature resistance, can pass microwaves and is not easy to generate heat in a microwave environment;
the preparation method of the high-temperature resistant ceramic comprises the following steps:
s1: weighing the raw materials for preparing the high-temperature resistant ceramics according to the weight parts;
s2: mixing fused quartz silica micropowder, cordierite, spodumene, clay, calcined talc, silicon nitride, zirconium dioxide powder and tungsten trioxide powder, and putting the mixture into a ball mill for grinding and mixing at the speed of 50r/min for 30 min;
s3: sieving the mixed powder with a 200-mesh sieve, taking undersize products, adding tetramethylethylenediamine and water, and stirring to form mud;
s4: and (3) molding the mud-shaped ceramic raw material into a mud blank with a fixed shape, and then firing at the high temperature of 1550 ℃ for 12h to obtain the high-temperature-resistant ceramic.
The acid removing device 3 comprises a connecting hose 31, an acid gas displacer 32, an absorption tower 33, an air suction pump 34, a pump machine connecting pipe 35 and an acid removing shell 36, wherein the connecting hose 31 is communicated with the top of the connecting pipe 112, the absorption tower 33 is placed above the acid removing shell 36, the acid gas displacer 32 is fixedly arranged at the bottom of the absorption tower 33, the upper end of the acid gas displacer 32 is communicated with the connecting hose 31, the air suction pump 34 is fixedly arranged at the bottom of the acid removing shell 36, the lower end of the pump machine connecting pipe 35 is communicated with the air suction pump 34, the upper end of the pump machine connecting pipe 35 is inserted above the absorption tower 33 and is communicated with the inside of the absorption tower 33, and acid gas in the digestion tank 14 is transferred into the absorption tower 33 through the air suction pump 34; the front surface above the acid removing shell 36 is provided with a transparent window 37 for replacing the absorption tower 33, the alkaline solution in the absorption tower 33 is replaced through the transparent window 37, the absorption tower 33 is filled with the alkaline absorption liquid, the alkaline absorption liquid adopts a NaOH solution with the mass fraction of 20%, and the NaOH solution and the acid gas are neutralized to purify the acid gas.
The reagent adding device 2 comprises a fixed rod 21, a rotating frame 22 and a plurality of reagent bottles 23, the lower end of the fixed rod 21 is fixedly connected with the top of the digestion shell 11, the center of the rotating frame 22 is rotatably connected with the upper end of the fixed rod 21, the plurality of reagent bottles 23 are arranged on the outer side of the rotating frame 22, and the reagent adding device 2 is used for acidifying the samples in the digestion tank 14; the lower end of the reagent bottle 23 is provided with a valve 231 for controlling the flow rate and flow rate, and the speed and dosage of the acid solution is controlled by the valve 231.
Compared with other materials, the high-temperature resistant ceramics used in the embodiments 6, 7 and 8 have the lowest temperature in the same microwave heating environment.
In the above embodiments, the rotating motor 123, the lifting motor 125, the PLC controller 19, the control panel 191, the magnetron 15, the high voltage rectifier 17, the transformer 18, the stirrer 13, and the getter pump 34 are all commercially available products as long as the functions of the present invention can be realized, and those skilled in the art can select and use the components according to the general knowledge, and are not limited herein.
The working method of example 8 is as follows:
s1: after sample soil is filled into the digestion tank 14, the lifting motor 125 is controlled to rotate through the control panel 191, so that the bent rod 1284 and the straight rod 1285 are driven to lift the lifting disc 121, the digestion tank 14 is placed into the chuck 124 after the lifting disc 121 is lifted, the lifting disc 121 is controlled to descend through the control panel 191, and after the cover plate 11 is covered, the soil sample in the digestion tank 14 is dried;
s2: after the sample is dried, the cover plate 11 is taken down, after the lifting disc 121 is lifted again, the reagent adding device 2 is used for adding an acidic reagent into the digestion tank 14, after the addition is completed, the lifting disc 121 is lowered, the cover plate 11 is covered to digest the soil sample, the acid gas enters the acid gas displacer 32 through the connecting hose 31 and then enters the absorption tower 33, the acid gas is neutralized through an alkaline solution in the absorption tower 33, and the neutralized neutral gas is discharged from the device through the suction pump 34.
Claims (8)
1. The utility model provides a soil sample pretreatment device for lead zinc slay heavy metal content detects, its characterized in that, includes microwave digestion device (1), reagent adds device (2), catches up with sour device (3), reagent adds device (2) fixed mounting in the upper right side of microwave digestion device (1), catch up with sour device (3) fixed mounting in the left side of microwave digestion device (1), microwave digestion device (1) including clear up shell (11), elevating system (12), agitator (13), clear up jar (14), magnetron (15), connecting channel (16), high-voltage rectifier (17), transformer (18), PLC controller (19), control panel (191), clear up storehouse (192), mount (193), clear up storehouse (192) fixed connection in the top of elevating system (12), the bottom of elevating system (12) with clear up the bottom fixed connection of shell (11), a lifting disc (121) is hinged above the lifting mechanism (12), the center of the lifting disc (121) is rotatably connected with a rotating disc (122), a rotating motor (123) is arranged at the bottom of the rotating disc (122), two sides of the rotating motor (123) are fixedly connected with the bottom of the lifting disc (121) through a fixing frame (193), a chuck (124) is arranged above the rotating disc (122), a digestion tank (14) is movably embedded above the chuck (124), a digestion plug (141) is arranged on the digestion tank (14), a cover plate (111) is arranged at the top of the digestion shell (11), the cover plate (111) is positioned at the top of the digestion plug (141), a connecting pipe (112) is vertically inserted in the cover plate (111), the lower end of the connecting pipe (112) is movably inserted in the digestion tank (14), and a stirrer (13) is fixedly installed on the inner wall of the rear side of the digestion bin (192), the magnetron (15) is fixedly installed above the right side of the digestion bin (192) and communicated with the stirrer (13) through the connecting channel (16), the high-voltage rectifier (17) is electrically connected below the magnetron (15), the control panel (191) is installed on the outer wall of the digestion shell (11) in front of the high-voltage rectifier (17) in an embedded mode, the PLC (19) is electrically connected below the high-voltage rectifier (17) and electrically connected with the control panel (191), and the transformer (18) is electrically connected below the PLC (19) and electrically connected with the high-voltage rectifier (17);
the lifting mechanism (12) comprises a lifting motor (125), a fixed disc (126), a screw rod (127) and support claws (128), the bottom of the fixed disc (126) is fixedly connected with the digestion shell (11), the lifting motor (125) is fixedly connected inside the fixed disc (126), the screw rod (127) is rotatably connected above the fixed disc (126), the lower end of the screw rod is in transmission connection with the lifting motor (125), the number of the support claws (128) is four, the four support claws (128) are uniformly arranged around the screw rod (127), each support claw (128) comprises a hinged frame (1281), a gear (1282), a gear shaft (1283), a bent rod (1284) and a straight rod (1285), the bottom of the hinged frame (1281) is fixedly connected with the fixed disc (126), the gear shaft (1283) horizontally penetrates through the hinged frame (1281), and the gear (1282) is arranged at the center of the gear shaft (1283), the lifting disc is in screw rod transmission connection with a screw rod (127), the near end of the bent rod (1284) is fixedly connected to the outer side of the gear shaft (1283), the far end of the bent rod (1284) is rotatably connected with the lower end of the straight rod (1285), and the upper end of the straight rod (1285) is hinged with the bottom of the lifting disc (121);
catch up with sour device (3) including coupling hose (31), sour gas displacer (32), absorption tower (33), aspirator pump (34), pump machine connecting pipe (35), catch up with sour shell (36), coupling hose (31) with the top of connecting pipe (112) communicates with each other, absorption tower (33) are placed catch up with the top of sour shell (36), sour gas displacer (32) fixed mounting is in absorption tower (33) bottom, and the upper end communicates with each other with coupling hose (31), aspirator pump (34) fixed mounting is in the bottom of catching up with sour shell (36), pump machine connecting pipe (35) lower extreme communicates with each other with aspirator pump (34), and the upper end inserts in the top of absorption tower (33), and communicates with each other with absorption tower (33) inside.
2. The soil sample pretreatment device for lead-zinc slag heavy metal content detection according to claim 1, wherein a transparent window (37) for replacing the absorption tower (33) is provided on the upper front surface of the acid-removing housing (36).
3. The soil sample pretreatment device for lead-zinc slag heavy metal content detection according to claim 1, wherein the reagent adding device (2) comprises a fixed rod (21), a rotating frame (22) and a plurality of reagent bottles (23), the lower end of the fixed rod (21) is fixedly connected with the top of the digestion shell (11), the center of the rotating frame (22) is rotatably connected with the upper end of the fixed rod (21), and the plurality of reagent bottles (23) are arranged outside the rotating frame (22).
4. The soil sample pretreatment device for lead-zinc slag heavy metal content detection according to claim 3, wherein a valve (231) for controlling flow rate and flow velocity is provided at a lower end of the reagent bottle (23).
5. The soil sample pretreatment device for lead-zinc slag heavy metal content detection according to claim 1, wherein a plastic ring (1121) is sleeved outside the connecting pipe (112), and the plastic ring (1121) abuts against the upper surface of the digestion plug (141).
6. The soil sample pretreatment device for lead-zinc slag heavy metal content detection according to claim 1, wherein the lifting disc (121), the rotating disc (122), the digestion tank (14) and the digestion plug (141) are made of high-temperature-resistant ceramic materials.
7. The soil sample pretreatment device for detecting the heavy metal content in lead-zinc slag according to claim 6, wherein the high-temperature resistant ceramic material comprises the following components in parts by weight: 20-50 parts of fused quartz silica powder, 8-9 parts of cordierite, 3-4 parts of spodumene, 2-3 parts of clay, 2-3 parts of calcined talc, 0.5-1 part of silicon nitride, 0.2-0.5 part of tetramethyl ethylenediamine, 5-9 parts of zirconium dioxide powder and 2-5 parts of tungsten trioxide powder.
8. The soil sample pretreatment device for lead-zinc slag heavy metal content detection according to claim 6, wherein a plastic ring (1121) is sleeved outside the connecting pipe (112).
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