CN104324520A - Ultrasonic separator for different forms of selenium - Google Patents

Ultrasonic separator for different forms of selenium Download PDF

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Publication number
CN104324520A
CN104324520A CN201410582902.0A CN201410582902A CN104324520A CN 104324520 A CN104324520 A CN 104324520A CN 201410582902 A CN201410582902 A CN 201410582902A CN 104324520 A CN104324520 A CN 104324520A
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resin column
ultrasonic wave
hopper
control system
liquid
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CN104324520B (en
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吴瑶庆
杜春霖
高友
孟昭荣
陈启凡
宫胜臣
邵应海
张兴悦
张凤雷
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Eastern Liaoning University
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Eastern Liaoning University
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Abstract

The invention relates to an ultrasonic separator for different forms of selenium. The ultrasonic separator for different forms of selenium comprises a computer controller, an automatic infusion control system, a high-frequency ultrasonic oscillation heating control system and a temperature and operation control system; the ultrasonic separator is characterized by comprising the structure that the center of an ultrasonic liquid storage tank is provided with a polytetrafluoroethylene resin column, a protective cover is arranged at the periphery of the ultrasonic liquid storage tank, and a high-frequency ultrasonic generator is arranged between the protective cover and the ultrasonic liquid storage tank; the bottom of the ultrasonic liquid storage tank is provided with a circulating cooling water inlet pipe and an electromagnetic valve; the ultrasonic liquid storage tank is provided with an overflow pipe and a liquid temperature sensor; the upper part of the resin column is provided with a raw material liquid inlet and an eluant inlet, and the resin column is internally provided with a liquid level sensor; the bottom of the resin column is provided with a drainage flow velocity sensor and a drainage adjustment electromagnetic valve; a raw material liquid storage tank and an eluant storage tank are respectively communicated with the resin column by a pipeline and are respectively provided with a liquid injection pump; the pump, the valves and sensor execution devices are connected with circuit modules of all the control systems respectively by a lead through the computer controller; the operation of electrical execution devices in the ultrasonic separator can be automatically controlled by operating procedures. The ultrasonic separator has the characteristics that the purity and the separation efficiency are high when the ultrasonic separator is used for separating different forms of selenium, the cost is lowered, and the environmental pollution is reduced.

Description

Ultrasonic wave form selenium separator
Technical field
The invention belongs to the equipment that chemical substance is separated, particularly teaching testing device, be applied to the ultrasonic wave form selenium separator that variform selenium [Organic Selenium: albumen selenium and polysaccharide selenium etc., inorganic selenium: Se (IV) and Se (VI)] is separated.
Background technology
Traditional form selenium is separated, and animal or plant sample treatment is become solution and adsorbent mix and blend to adsorb, and then, is placed on by adsorbent in closed container and is placed in constant temperature oscillation machine and vibrates the adsorbent selenium of wash-out, then obtain product to after eluent process.The method separation purity is not high, separative efficiency is low, eluent consumption large, and harmful substance is volatile causes environmental pollution.Operated in accordance with conventional methods process need apparatus amount is large, numerous and diverse, (adsorbent to be taken out in container and drench dry raw material waste liquid, to reload in closed container after constant temperature oscillation wash-out form selenium, drench again and dryly collect the operations such as eluent), equally also make this teaching testing device utensil consumption large, medicine waste is serious, because skilled operation degree is different, the yield difference of product is larger.
Summary of the invention
The object of the invention is to provide a kind of ultrasonic wave form selenium separator, and overcome the deficiency that conventional method separation purity and separative efficiency are in the past low, can meet teaching test requirement, contaminated solution problem also can be applicable to industrial-scale production.
Ultrasonic wave form selenium separator of the present invention, comprise computerized control system, automatic infusion system, high-frequency ultrasonic vibration heating, temperature control system and operation procedure control system, it is characterized in that cyclone separator arrangement: polyflon post is settled at ultrasonic wave hopper center, ultrasonic wave hopper periphery arranges protective cover, high frequency ultrasound wave producer is arranged between ultrasonic wave hopper outer wall and protective cover, water inlet pipe and the ultrasonic wave hopper recirculated water magnetic valve thereof of ultrasonic wave hopper recirculated cooling water are installed bottom ultrasonic wave hopper, fluid temperature sensor in the overflow pipe of ultrasonic wave hopper top configuration cycles cooling water and hopper, liquid level sensor in material liquid entrance, eluent entrance and resin column is settled on polyflon post top, and the configuration of polyflon column bottom controls resin column internal drainage flow sensor and resin column draining adjustable electromagnetic valve, material liquid basin, eluent basin by pipeline connection polyflon post, and arrange topping-up pump, pump on each equipment, valve, sensor and actor part are connected with the circuit module of each control system by wire by computer controller, operation procedure in hopper computerized control system comprises ultrasonic wave hopper temperature setting territory, high-frequency ultrasonic power setting territory, polyflon post draining flow rate set territory, after the programme-control of computerized control system initiating task, by form selenium contained by the sensor feedback information on facility, the liquid of being discharged by the outer instrument of body or desk checking, monitor eluted mass index, terminate operation after reaching requirement or repeat this automatic infusion system cloud gray model, automatically Operation control being implemented to the electric executive item in this device.
Ultrasonic wave form selenium separator of the present invention, has that the purity being separated different shape selenium is high, separative efficiency is high, cost-saving, the feature that reduces environmental pollution.This separator is compared with conventional method: add controllability, decrease adsorbent in container, to take out the dry raw material waste liquid of pouring, reload closed container constant temperature oscillation wash-out form selenium, drench again and dryly collect the operations such as eluent, decrease the working time, reduce eluent consumption and post processing sewage cost.To extract different shape selenium in certain Blueberry, raw material state is identical, the different shape selenium that legacy equipment extracts, and 1.0kg blueberry can extract Organic Selenium 53.68mg, and because of the difference in operation, general purity is about 65% ~ 85%; And using this equipment 1.0kg blueberry can extract Organic Selenium 67.22mg, purity can reach more than 80% ~ 95%.
Accompanying drawing explanation
Fig. 1 is the device structure schematic diagram of ultrasonic wave form selenium separator;
Fig. 2 is that the circuit module that described ultrasonic wave form selenium splitter circuit controls connects schematic block diagram;
Fig. 3 is described ultrasonic wave form selenium separator operation procedure FB(flow block).
Detailed description of the invention
Ultrasonic wave form selenium separator, comprise computerized control system, automatic infusion system, high-frequency ultrasonic vibration heating and temperaturel control system, see Fig. 1, it is characterized in that structure: polyflon post 1 is settled at ultrasonic wave hopper 2 center, periphery arranges protective cover 3, high frequency ultrasound wave producer 8 is arranged between ultrasonic wave hopper 2 outer wall and protective cover 3, overflow pipe 6 is installed on ultrasonic wave hopper 2 top, ultrasonic wave hopper temperature sensor 7, hopper circulating water inlet 10 is installed bottom ultrasonic wave hopper 2, hopper recirculated water magnetic valve 9, resin column 1 top arranges liquid level sensor 5 in material liquid inlet pipe 4 and eluent inlet pipe 19 and resin column, the material liquid inlet pipe 4 of material liquid basin 15, the eluent inlet pipe 19 of eluent basin 16 arranges raw material liquid pump 18 respectively, wash-out liquid pump 17, configure configuration on the resin column draining flow sensor 12 of mensuration resin column draining flow velocity, pipeline in polyflon post 1 bottom discharge pipeline and control the resin column draining adjustable electromagnetic valve 11 of resin column internal drainage speed, the material liquid of the successively injection from resin column 1 upper end and eluent will share discharge outlet and discharge through resin column draining adjustable electromagnetic valve 11 in lower end, all electricity pieces are connected with computer operation table 14 by wire and sensor conductor 13.Magnetic valve is divided into complete folding type and adjustable type, all will use in this equipment different parts two kinds, if ultrasonic wave hopper recirculated water magnetic valve 9 and resin column draining adjustable electromagnetic valve 11 are exactly two kinds of different magnetic valves.
The electrical configurations of ultrasonic wave form selenium separator control system, as shown in Figure 2: the computerized control system in computer controller 14 comprises automatic infusion control system, high frequency ultrasound wave power, fluid temperature induction and automatic cycle water cooling control system in hopper, the measurement of rate of flow of resin column internal drainage and draining regulation and control system and operation procedure control system, it is characterized in that circuit connecting relation: the computerized control system circuit module in computer controller 14, computer controller 14 is called for short in block diagram 2, connect ultrasonic wave hopper temperature setting circuit and high-frequency ultrasonic power setting circuit respectively, computer controller 14 1 output is connected to the high frequency ultrasound wave producer 8 being fixed on ultrasonic wave hopper 2 outer wall, computer controller 14 1 output is connected to the resin column draining adjustable electromagnetic valve 11 on the discharge pipe line of resin column 1 lower end, computer controller 14 1 output is connected to cooling water and enters ultrasonic wave hopper recirculated water magnetic valve 9 in ultrasonic wave hopper 2 pipeline, computer controller 14 1 output is connected to the wash-out liquid pump 17 between eluent basin 16 outlet and resin column 1, computer controller 14 1 output is connected to the raw material liquid pump 18 between raw material receiver 15 outlet and resin column 1, computer controller 14 1 input connects the liquid level sensor 5 on resin column 1, computer controller 14 1 input connects the ultrasonic wave hopper temperature sensor 7 of ultrasonic wave hopper 2, computer controller 14 1 input connects the resin column draining flow sensor 12 in resin column 1 pipeline, all forms loop be connected electrical part.
See Fig. 3, operation procedure control system in computerized control system, comprise ultrasonic wave hopper temperature setting territory, high-frequency ultrasonic power setting territory, polyflon post draining flow rate set territory.Computer controller 14 starts after computerized control system enters operation procedure control system, according to the state that resin column liquid level sensor 5 in job control program is responded to without liquid level, automatic infusion system control state is entered: first ultrasonic wave hopper 2 is filled water under the mobility condition of resin column draining flow sensor 12 setting, close ultrasonic wave hopper recirculated water magnetic valve 9, and open resin column draining adjustable electromagnetic valve 11, start raw material liquid pump 18, material liquid (the form selenium solution containing Organic Selenium or inorganic selenium) is injected in resin column 1, enter adsorption process, when in resin column, liquid level sensor 5 feeds back to that in resin column 1, liquid level exceedes setting value, raw material liquid pump 18 cuts out.Form selenium contained from the material liquid that top adds in adsorption process is attracted to after on adsorbent, and remaining waste liquid is discharged from the lower end of resin column through resin column draining adjustable electromagnetic valve 11, what discharge under wash-out state is the eluent carrying form selenium.In adsorption process, this program injects material liquid by liquid level sensor in resin column 5 induction control raw material liquid pump 18: when in adsorption process resin column, liquid level sensor 5 senses that in resin column 1, liquid level is lower than setting value, raw material liquid pump 18 is again opened to supplement and injected material liquid.When the flow rate of liquid that resin column draining flow sensor 12 senses is zero, open high frequency ultrasound wave producer 8, the condition arranged by operation procedure carries out wash-out to form selenium adsorbent in resin column 1; After high frequency ultrasound wave producer 8 operation, start wash-out liquid pump 17 and inject eluent in resin column 1, whether automatic infusion system can constantly adjust wash-out liquid pump 17 according to the feedback states of receiving liquid level sensor 5 and continue to inject eluent; According to resin in resin column the absorption of various form selenium and elute effect, resin column draining flow sensor 12 fed back to control system and send instruction by the measurement of rate of flow of resin column internal drainage and draining regulation and control system and flow velocity adjustment is carried out to resin column draining adjustable electromagnetic valve 11, resin column draining adjustable electromagnetic valve 11 runs after starting always, according to the continuous regulating valve gap length of instruction received, can there is not the situation of closing and restarting.Set supersonic generator 8 in the vibration heating power set according to different material feature, the work of hopper temperature range in high-frequency ultrasonic vibration heating power system, and monitor high frequency ultrasound wave producer 8 operational factor.Wash-out needs to carry out at certain temperature and oscillating condition, before startup wash-out, open liquid in supersonic generator 8 pairs of ultrasonic wave hoppers 2 in Fig. 3 carry out vibration heating, the adsorbent of indirectly-acting in resin column 1, carry out auxiliary wash-out to the Organic Selenium of adsorbent different shape or inorganic selenium, marginal not enters limit and assists wash-out until adsorbent form selenium wash-out is complete.When in the ultrasonic wave hopper that in operation, ultrasonic wave hopper temperature sensor 7 senses, liquid temperature occurs exceeding design temperature situation, ultrasonic wave hopper recirculated water magnetic valve 9 is opened, by being connected to ultrasonic wave hopper circulating water inlet 10 flowing water of water supply pipe to the liquid cooling in ultrasonic wave hopper 2, the unnecessary water yield is discharged by overflow pipe 6; By opening, closing ultrasonic wave hopper recirculated water magnetic valve 9, control the fluid temperature in ultrasonic wave hopper, the temperature indirectly controlling eluent remains in the liquid temperature parameter area of setting.Form selenium concentration contained by the liquid of being discharged by the outer instrument of body or desk checking, is monitored eluted mass index, terminates operation or repeat this automatic infusion system cloud gray model after reaching requirement.To run after this device start always, operation procedure control system constantly can adjust according to the instruction received, when in post, flow rate of liquid is too low, computer controller increases resin column draining adjustable electromagnetic valve 11 gap automatically, increase flow rate of liquid in post, when in post, flow rate of liquid is too high, controller reduces adjustable electromagnetic valve clearance automatically, reduce flow rate of liquid in post, reach flow rate of liquid in post and automatically control.
Different shape selenium ability in above-mentioned adsorbent raw material, eluent is obtain data according to raw material is different through previous experiments to adsorbent different shape selenium elute effect, determine the material quantity that at every turn can inject and eluent consumption used again, discharged the state of liquid by inspection resin column draining adjustable electromagnetic valve 11 in running, assay is written in control system by computer controller and is adjusted by operation procedure control system and determine operation procedure, with the fixed value of internal memory: material liquid or eluate concentration, inject flow, flow velocity, material liquid or eluent inject complete index etc. and contrast, detection exudate concentration difference with reference to new write injects duration by adjustment, meet and inject or discharge rate requirement.In resin column, flow rate of liquid controls: load in polyflon post by the adsorbent chosen, according to the adsorption effect of the adsorbent selected to different shape selenium and the elute effect of eluent, flow rate of liquid in setting resin column, under absorption and washing steps state, in resin column, flow rate of liquid feeds back to controller by the draining flow sensor 12 in the drainage pipeline of resin column lower end.All should carry out lab scale early stage to different raw materials in production operation, after obtaining absorption, elute effect scope, set adsorbent amount, then according to adsorbent amount determination material liquid injection rate and eluent consumption.Flow rates value adjusts according to material characteristic, the flow velocity in post because of select adsorbent granule size, the consumption of adsorbent, adsorbent treatment effect in early stage relevant with factors such as the resin column diameters selected.
Resin column can select commercially available resin column as required, and the standard of resin column is produced according to national standard by manufacturer, needs to select according to actual experiment or production scale.Adsorbent is the resin, Sulfhydryl Cotton, thio chitosan, alundum (Al2O3) etc. that need to select commercially available different size and purposes according to the form selenium of separating-purifying different cultivars, and according to the selenium that different shape exists, may select different adsorbents, be variable.The standard of adsorbent is produced according to national standard by manufacturer, selects according to actual needs.

Claims (4)

1. ultrasonic wave form selenium separator, comprise computerized control system, automatic infusion system, high-frequency ultrasonic vibration heating, temperature control system and operation procedure control system, it is characterized in that cyclone separator arrangement: polyflon post is settled at ultrasonic wave hopper center, ultrasonic wave hopper periphery arranges protective cover, high frequency ultrasound wave producer is arranged between ultrasonic wave hopper outer wall and protective cover, water inlet pipe and the ultrasonic wave hopper recirculated water magnetic valve thereof of ultrasonic wave hopper recirculated cooling water are installed bottom ultrasonic wave hopper, fluid temperature sensor in the overflow pipe of ultrasonic wave hopper top configuration cycles cooling water and hopper, liquid level sensor in material liquid entrance, eluent entrance and resin column is settled on polyflon post top, and the configuration of polyflon column bottom controls resin column internal drainage flow sensor and resin column draining adjustable electromagnetic valve, material liquid basin, eluent basin by pipeline connection polyflon post, and arrange topping-up pump, pump on each equipment, valve, sensor and actor part are connected with the circuit module of each control system by wire by computer controller, operation procedure in hopper computerized control system comprises ultrasonic wave hopper temperature setting territory, high-frequency ultrasonic power setting territory, polyflon post draining flow rate set territory, after the programme-control of computerized control system initiating task, by form selenium contained by the sensor feedback information on facility, the liquid of being discharged by the outer instrument of body or desk checking, monitor eluted mass index, terminate operation after reaching requirement or repeat this automatic infusion system cloud gray model, automatically Operation control being implemented to the electric executive item in this device.
2. ultrasonic wave form selenium separator according to claim 1, it is characterized in that structure: polyflon post (1) is settled at ultrasonic wave hopper (2) center, periphery arranges protective cover (3), high frequency ultrasound wave producer (8) is arranged between ultrasonic wave hopper (2) outer wall and protective cover (3), overflow pipe (6) is installed on ultrasonic wave hopper (2) top, ultrasonic wave hopper temperature sensor (7), hopper circulating water inlet (10) is installed in ultrasonic wave hopper (2) bottom, hopper recirculated water magnetic valve (9), resin column (1) top arranges liquid level sensor (5) in material liquid inlet pipe (4) and eluent inlet pipe (19) and resin column, the material liquid inlet pipe (4) of material liquid basin (15), the eluent inlet pipe (19) of eluent basin (16) arranges raw material liquid pump (18) respectively, wash-out liquid pump (17), configure configuration on the resin column draining flow sensor (12) of mensuration resin column draining flow velocity, pipeline in polyflon post (1) bottom discharge pipeline and control the resin column draining adjustable electromagnetic valve (11) of resin column internal drainage speed, the material liquid of the successively injection from resin column (1) upper end and eluent will share discharge outlet and discharge through resin column draining adjustable electromagnetic valve (11) in lower end, all electricity pieces are connected with computer operation table (14) by wire and sensor conductor (13).
3. ultrasonic wave form selenium separator according to claim 1, it is characterized in that the electrical configurations of control system, circuit connecting relation: the computerized control system in computer controller (14) comprises automatic infusion control system, high frequency ultrasound wave power, fluid temperature induction and automatic cycle water cooling control system in hopper, the measurement of rate of flow of resin column internal drainage and draining regulation and control system and operation procedure control system, it is characterized in that circuit connecting relation: the computerized control system circuit module in computer controller (14), be called for short computer controller (14), connect ultrasonic wave hopper temperature setting circuit and high-frequency ultrasonic power setting circuit respectively, computer controller (14) one output is connected to the high frequency ultrasound wave producer (8) being fixed on ultrasonic wave hopper (2) outer wall, computer controller (14) one output is connected to the resin column draining adjustable electromagnetic valve (11) on the discharge pipe line of resin column (1) lower end, computer controller (14) one output is connected to cooling water and enters ultrasonic wave hopper recirculated water magnetic valve (9) in ultrasonic wave hopper (2) pipeline, computer controller (14) one output is connected to the wash-out liquid pump (17) between eluent basin (16) outlet and resin column (1), computer controller (14) one output is connected to the raw material liquid pump (18) between raw material receiver (15) outlet and resin column (1), computer controller (14) one input connects the liquid level sensor (5) on resin column (1), computer controller (14) one input connects the ultrasonic wave hopper temperature sensor (7) of ultrasonic wave hopper (2), computer controller (14) one input connects the resin column draining flow sensor (12) in resin column (1) pipeline, all forms loop be connected electrical part.
4. ultrasonic wave form selenium separator according to claim 1, it is characterized in that operation procedure control system: the state responded to without liquid level according to resin column liquid level sensor (5) in job control program, automatic infusion system control state is entered: first ultrasonic wave hopper (2) is filled water under the mobility condition that resin column draining flow sensor (12) sets, close ultrasonic wave hopper recirculated water magnetic valve (9), and open resin column draining adjustable electromagnetic valve (11), start raw material liquid pump (18), material liquid is injected in resin column (1), enter adsorption process, in resin column, liquid level sensor (5) feeds back to liquid level in resin column (1) when exceeding setting value, raw material liquid pump (18) cuts out, form selenium contained from the material liquid that top adds in adsorption process is attracted to after on adsorbent, and remaining waste liquid is discharged from the lower end of resin column through resin column draining adjustable electromagnetic valve (11), what discharge under wash-out state is the eluent carrying form selenium, in adsorption process, this program controls raw material liquid pump (18) injection material liquid by liquid level sensor in resin column (5) induction: when in adsorption process resin column, liquid level sensor (5) senses that in resin column (1), liquid level is lower than setting value, and raw material liquid pump (18) is again opened to supplement and injected material liquid, when the flow rate of liquid that resin column draining flow sensor (12) senses is zero, open high frequency ultrasound wave producer (8), the condition arranged by operation procedure carries out wash-out to form selenium adsorbent in resin column (1), after high frequency ultrasound wave producer (8) operation, start wash-out liquid pump (17) and inject eluent in resin column (1), whether automatic infusion system can constantly adjust wash-out liquid pump (17) according to the feedback states of receiving liquid level sensor (5) and continue to inject eluent, according to resin in resin column to the absorption of various form selenium and elute effect, resin column draining flow sensor (12) feeds back to control system, and send instruction by the measurement of rate of flow of resin column internal drainage and draining regulation and control system flow velocity adjustment is carried out to resin column draining adjustable electromagnetic valve (11), resin column draining adjustable electromagnetic valve (11) runs after starting always, can according to the continuous regulating valve gap length of instruction received, set supersonic generator (8) in high-frequency ultrasonic vibration heating power system in the vibration heating power set according to different material feature, the work of hopper temperature range, and monitor high frequency ultrasound wave producer (8) operational factor, wash-out needs to carry out at certain temperature and oscillating condition, before startup wash-out, open supersonic generator (8) vibration heating has been carried out to liquid in ultrasonic wave hopper (2), the adsorbent of indirectly-acting in resin column (1), carry out auxiliary wash-out to the Organic Selenium of adsorbent different shape or inorganic selenium, marginal not enters limit and assists wash-out until adsorbent form selenium wash-out is complete, when in the ultrasonic wave hopper that in operation, ultrasonic wave hopper temperature sensor (7) senses, liquid temperature occurs exceeding design temperature situation, ultrasonic wave hopper recirculated water magnetic valve (9) is opened, by being connected to ultrasonic wave hopper circulating water inlet (10) flowing water of water supply pipe to the liquid cooling in ultrasonic wave hopper (2), the unnecessary water yield is discharged by overflow pipe (6), by opening, closing ultrasound waves hopper recirculated water magnetic valve (9), control the fluid temperature in ultrasonic wave hopper, the temperature indirectly controlling eluent remains in the liquid temperature parameter area of setting, form selenium concentration contained by the liquid of being discharged by the outer instrument of body or desk checking, is monitored eluted mass index, terminates operation or repeat this automatic infusion system cloud gray model after reaching requirement.
CN201410582902.0A 2014-10-27 2014-10-27 Ultrasonic wave form selenium separator Active CN104324520B (en)

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CN107024375A (en) * 2017-06-05 2017-08-08 辽东学院 A kind of portable sample analyzer front processor and application method
CN108777179A (en) * 2018-06-13 2018-11-09 清华大学 Gel ball room temperature aging device

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CN107024375A (en) * 2017-06-05 2017-08-08 辽东学院 A kind of portable sample analyzer front processor and application method
CN108777179A (en) * 2018-06-13 2018-11-09 清华大学 Gel ball room temperature aging device

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