CN107311121A - A kind of system for preparing nano lead-selenide - Google Patents
A kind of system for preparing nano lead-selenide Download PDFInfo
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- CN107311121A CN107311121A CN201710599189.4A CN201710599189A CN107311121A CN 107311121 A CN107311121 A CN 107311121A CN 201710599189 A CN201710599189 A CN 201710599189A CN 107311121 A CN107311121 A CN 107311121A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0046—Sequential or parallel reactions, e.g. for the synthesis of polypeptides or polynucleotides; Apparatus and devices for combinatorial chemistry or for making molecular arrays
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
- B01J19/1862—Stationary reactors having moving elements inside placed in series
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00054—Controlling or regulating the heat exchange system
- B01J2219/00056—Controlling or regulating the heat exchange system involving measured parameters
- B01J2219/00058—Temperature measurement
- B01J2219/00063—Temperature measurement of the reactants
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00177—Controlling or regulating processes controlling the pH
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
- B01J2219/00277—Apparatus
- B01J2219/00479—Means for mixing reactants or products in the reaction vessels
- B01J2219/00481—Means for mixing reactants or products in the reaction vessels by the use of moving stirrers within the reaction vessels
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
- B01J2219/00718—Type of compounds synthesised
- B01J2219/00745—Inorganic compounds
- B01J2219/0075—Metal based compounds
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Abstract
The present invention provides a kind of system for preparing nano lead-selenide, and the system includes the first reactor, and it is used to prepare selenium precursor solution；Second reactor, it is used to prepare lead precursor solution and/or selenizing lead materials；Gas shield device, it is used to be passed through protective gas into the first reactor；PH adjusting meanss, it is used for the pH value for adjusting lead precursor solution；Heater, it is used to heat the first reactor and the second reactor；Conveying device, it is used to the selenium precursor solution in the first reactor being delivered in the first reactor, with lead precursor solution reaction generation selenizing lead materials；Filtration wash unit, it is used to filter and/or cleans selenizing lead materials；Hollander tub, it is used to that lead selenide slurry will to be broken into through selenizing lead materials；Spray dryer, it is used to dry lead selenide slurry, completes the preparation of nano lead-selenide, it is possible to increase prepare the success rate of Nano lead sulfide.
Description
Technical field
The present invention relates to nano lead-selenide preparing technical field, and in particular to a kind of system for preparing nano lead-selenide.
Background technology
Nano lead-selenide is a kind of semi-conducting material with cubic structure low energy gap, and it has the physical of many uniquenesses
Can, such as dielectric constant is high, high, the narrow band gap of carrier mobility, good photoconductive effect, to external world the influence reaction of condition
Compare sensitive, it is adaptable to manufacture sensor part.In recent years, scientist observed " many current-carrying in Nano lead sulfide
Sub- effect ", is commonly called as " avalanche effect ", becomes most promising high-efficiency photovoltaic converting material.
The preparation method of nano lead-selenide has a lot, and one way in which is to nano lead-selenide system based on Aqueous phase
Standby, it is usually to be prepared in laboratory or production that existing use Aqueous phase, which prepares nano lead-selenide, and behaviour by hand
Make frequent, once operation is lack of standardization nano lead-selenide can be caused to prepare failure, nowadays still without suitable automation equipment
The preparation to nano lead-selenide can be realized.
Therefore, this area needs a kind of system for preparing nano lead-selenide to solve the above problems.
The content of the invention
In order to solve the above-mentioned technical problem, the invention provides a kind of system for preparing nano lead-selenide, it is desirable to provide one
Plant automation Preparation equipment to prepare nano lead-selenide, nanometer vulcanization is improved on the premise of labour is saved so as to realize
The preparation efficiency of lead and it is prepared into power.
In order to realize above-mentioned technical purpose, the present invention provides following technical scheme：
A kind of system for preparing nano lead-selenide, system includes：First reactor, it is used to prepare selenium precursor solution；The
Two reactors, it is used to prepare lead precursor solution and/or selenizing lead materials；Gas shield device, it is used for anti-to first
Answer and protective gas is passed through in kettle；PH adjusting meanss, it is used for the pH value for adjusting lead precursor solution；Heater, it is used for
One reactor and/or the second reactor are heated；Conveying device, it is used for the selenium precursor solution conveying in the first reactor
To the first reactor, with lead precursor solution reaction generation selenizing lead materials；Filtration wash unit, its be used for filter and/or
Person cleans selenizing lead materials；Hollander tub, it is used to that lead selenide slurry will to be broken into through selenizing lead materials；Spray dryer, it is used for
Lead selenide slurry is dried, the preparation of nano lead-selenide is completed.
In the optimal technical scheme of said system, the first reactor includes having in the first kettle, the first kettle and is used for
The first chamber of selenium precursor solution is prepared, the top of first chamber is provided with the first agitator, and the first agitator can be to the first kettle
Internal selenium precursor solution is stirred；First kettle is provided with the first inlet for being used for that solution to be injected to first chamber, with
And for injecting the air inlet of protective gas into first chamber.
In the optimal technical scheme of said system, gas shield device includes multiple gas tanks in parallel, and each gas tank is equal
Protective gas can be injected into first chamber by air inlet.
In the optimal technical scheme of said system, protective gas is inert gas.
In the optimal technical scheme of said system, the second reactor includes having in the second kettle, the second kettle and is used for
The second chamber of lead precursor solution is prepared, the top of second chamber is provided with the second agitator, and the second agitator can be to the second kettle
Internal lead precursor solution or selenizing lead materials is stirred；Second kettle, which is provided with, to be used to inject solution to second chamber
At least three second inlets.
In the optimal technical scheme of said system, pH adjusting meanss include pH sensors, and pH sensors are arranged on second
In chamber, the pH value for detecting the lead precursor solution in the second kettle.
In the optimal technical scheme of said system, hollander tub includes having in cell body, cell body and is used to accommodate lead selenide thing
3rd chamber of material, the bottom of the 3rd chamber is provided with dynamic mixers, and the side wall of the 3rd chamber is provided with and dynamic mixers phase
The static mixer of cooperation.
In the optimal technical scheme of said system, static mixer includes the gear being arranged on the side wall of the 3rd chamber
Plate, baffle plate is provided with mashing tooth.
In the optimal technical scheme of said system, TEMP is respectively equipped with the first reactor and the second reactor
Device.
In the optimal technical scheme of said system, system also includes control device, and control device reacts with first respectively
Kettle, the second reactor, gas shield device, pH adjusting meanss, heater, conveying device, filtration wash unit, hollander tub,
Spray dryer and the connection of temperature sensing device signal.
The invention provides a kind of system for preparing nano lead-selenide, its advantage is：Pass through the first reactor system
Standby selenium precursor solution, the second reactor prepare lead precursor solution, generate nano lead-selenide under normal pressure or reaction under high pressure, the nanometer
Crystalline substance be able to can be dispersed stably in aqueous phase, can effectively control nanocrystalline pattern, and preparation method is simple, manufacturing cycle
It is short, the efficiency and success rate for preparing nano lead-selenide can be improved.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is the accompanying drawing used required in technology description to be briefly described, it should be apparent that, drawings in the following description are only this
Some embodiments of invention, for those of ordinary skill in the art, on the premise of not paying creative work, can be with
Other accompanying drawings are obtained according to these accompanying drawings.
Fig. 1 is the structural representation of the system for preparing nano lead-selenide of the present invention；
Fig. 2 is the structural representation of the first reactor of the present invention；
Fig. 3 is the structural representation of the second reactor of the present invention；
Fig. 4 is the structural representation of the hollander tub of the present invention.
In figure：1st, the first reactor；11st, the first kettle；12nd, the first agitator；13rd, the first inlet；14th, air inlet；
2nd, the second reactor；21st, the second kettle；22nd, the second agitator；23rd, the second inlet；3rd, gas shield device；4th, pH is adjusted
Device；5th, heater；6th, conveying device；7th, filtration wash unit；8th, hollander tub；81st, cell body；82nd, dynamic mixers；83、
Static mixer；831st, baffle plate；832nd, it is beaten tooth；9th, spray dryer.
Embodiment
To make the object, technical solutions and advantages of the present invention clearer, technical scheme will be carried out below
Detailed description.Obviously, described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Base
Embodiment in the present invention, those of ordinary skill in the art are resulting on the premise of creative work is not made to be owned
Other embodiment, belongs to the scope that the present invention is protected.
It should be noted that in the description of the invention, term " " center ", " on ", " under ", "left", "right", " vertical ",
The direction of instruction such as " level ", " interior ", " outer " or the term of position relationship are to be based on direction shown in the drawings or position relationship, this
Description is intended merely to facilitate, rather than indicates or imply that described device or element there must be specific orientation, with specific
Azimuth configuration and operation, therefore be not considered as limiting the invention.In addition, term " first ", " second ", " the 3rd " are only used
In description purpose, and it is not intended that indicating or implying relative importance.
In addition it is also necessary to explanation, in the description of the invention, unless otherwise clearly defined and limited, term " peace
Dress ", " connected ", " connection " should be interpreted broadly, for example, it may be fixedly connected or be detachably connected, or integratedly
Connection；Can be mechanical connection or electrical connection；Can be joined directly together, can also be indirectly connected to by intermediary,
It can be the connection of two element internals.To those skilled in the art, it can understand that above-mentioned term exists as the case may be
Concrete meaning in the present invention.
Referring to Fig. 1 to Fig. 4, Fig. 1 is the structural representation of the system for preparing nano lead-selenide of the present invention；Fig. 2 is this hair
The structural representation of the first bright reactor；Fig. 3 is the structural representation of the second reactor of the present invention；Fig. 4 is of the invention
The structural representation of hollander tub.As shown in figure 1, the invention provides a kind of system for preparing nano lead-selenide, system includes：The
One reactor 1, it is used to prepare selenium precursor solution；Second reactor 2, it is used to prepare lead precursor solution and/or selenizing
Lead materials；Gas shield device 3, it is used to be passed through protective gas into the first reactor 1；PH adjusting meanss 4, it is used to adjust
The pH value of lead precursor solution；Heater 5, it is used to heat the first reactor 1 and/or the second reactor 2；Conveying dress
6 are put, it is used to the selenium precursor solution in the first reactor 1 being delivered in the first reactor 1, react and generate with lead precursor solution
Selenizing lead materials；Filtration wash unit 7, it is used to filter and/or cleans selenizing lead materials；Hollander tub 8, it is used to pass through
Selenizing lead materials break into lead selenide slurry；Spray dryer 9, it is used to dry lead selenide slurry, completes nano lead-selenide
Prepare.
By the structure design of said system, the first reactor will be put into for the reactant and water that prepare selenium precursor solution
In 1, then by the first agitator 12 reactant and water are well mixed, are passed through inertia into the first reactor 1 in the process
Protective gas；It will be put into for preparing the reactant and water of lead precursor solution in the second reactor 2, then pass through the second agitator 22
Reactant and water are well mixed, and are passed through into the first reactor 1 pH adjusting agent regulation pH value, then by the selenium precursor prepared
Solution is added in lead precursor solution, is heated by heater 5, room temperature is cooled to after the completion of reaction, pass through filtration wash unit 7
Filter and filter cake is washed by ethanol solution, repeatedly filtration washing, untill pH value meets the requirements；Filter cake is sent
Mashing processing is carried out to hollander tub 8, it is to avoid material lumps in the drying process, the material for completing mashing is delivered into spray drying
Device 9 is dried, and produces nano lead-selenide, pass through the present invention automated system, it is possible to increase prepare nano lead-selenide efficiency and
Success rate.
In a kind of preferably embodiment, as shown in Fig. 2 the first reactor 1 includes the first kettle 11, the first kettle 11
Interior to have the first chamber for being used for preparing selenium precursor solution, the top of first chamber is provided with the first agitator 12, the first agitator
12 can be stirred to the selenium precursor solution in the first kettle 11；First kettle 11, which is provided with, to be used to inject molten to first chamber
First inlet 13 of liquid, and for injecting the air inlet 14 of protective gas into first chamber.
In a kind of preferably embodiment, gas shield device 3 includes multiple gas tanks in parallel, and each gas tank can
Protective gas is injected into first chamber by air inlet 14.
Preferably, protective gas is inert gas, such as nitrogen.
In a kind of preferably embodiment, as shown in figure 3, the second reactor 2 includes the second kettle 21, the second kettle 21
Interior to have the second chamber for being used for preparing lead precursor solution, the top of second chamber is provided with the second agitator 22, the second agitator
22 can be stirred to the lead precursor solution in the second kettle 21 or selenizing lead materials；Second kettle 21 be provided be used for
Second chamber injects at least three second inlets 23 of solution.
Preferably, the quantity of the second inlet 23 is three, respectively molten for preparing lead precursor to second chamber injection
The inlet of the reactant of liquid, for second chamber inject selenium precursor solution inlet, for second chamber inject pH
Adjust the inlet of liquid.
In a kind of preferably embodiment, pH adjusting meanss 4 include pH sensors, and pH sensors are arranged on second chamber
It is interior, the pH value for detecting the lead precursor solution in the second kettle 21.
PH adjusting meanss 4 also include being used to accommodate the regulation tank that pH adjusts liquid, and regulation tank injects pH regulations to second chamber
Liquid, the pH value for adjusting lead precursor solution.
Preferably, it is alkaline solution, such as sodium hydroxide solution, potassium hydroxide solution, ammoniacal liquor that pH, which adjusts liquid,.
In a kind of preferably embodiment, it is used to hold as shown in figure 4, hollander tub 8 includes having in cell body 81, cell body 81
Receive the 3rd chamber of selenizing lead materials, the bottom of the 3rd chamber is provided with dynamic mixers 82, the side wall of the 3rd chamber be provided with
The static mixer 83 that dynamic mixers 82 are engaged.
Preferably, static mixer 83 includes the baffle plate 831 being arranged on the side wall of the 3rd chamber, and baffle plate 831 is provided with
It is beaten tooth 832.
Preferably, dynamic agitation oar includes rotating shaft and the multiple blades being arranged in rotating shaft, and blade, which is provided with, to be used to be beaten
Mashing hole.
Preferably, the sensor for detecting lead selenide mud dispersivity degree is additionally provided with the side wall of the 3rd chamber.
In a kind of preferably embodiment, temperature sensor is respectively equipped with the first reactor 1 and the second reactor 2,
Lead precursor solution and/or lead selenide in temperature for detecting selenium precursor solution in the first reactor 1, the second reactor 2
The temperature of material, the temperature of reactant can be detected in real time, it is to avoid temperature occur improper and influence the preparation of nano lead-selenide
Situation.
In said structure, heater 5 is heated by the way of steam heating, electrical heating or heat-conducting oil heating.
In a kind of preferably embodiment, conveying device 6 is delivery pump.
In a kind of preferably embodiment, filtration wash unit 7 includes the filter for filtering, washing for washing
Kettle and the cleaning solution kettle for putting cleaning solution are washed, filter cake is put into washing kettle after the completion of filtering, washing is added into washing kettle
Liquid washs filter cake, filters, operates repeatedly, untill pH value meets the requirements after the completion of washing.
In order to realize the control to system, although not showing in figure, the system also includes control device, control device difference
With the first reactor 1, the second reactor 2, gas shield device 3, pH adjusting meanss 4, heater 5, conveying device 6, filtering
Wash mill 7, hollander tub 8, spray dryer 9 and the connection of temperature sensing device signal.It can be controlled in real time by control device
The progress of whole equipment, makes its full automation, improves the efficiency and success rate for preparing nano lead-selenide.
In a kind of embodiment of the present invention, first will be put into for the reactant and water that prepare selenium precursor solution
In reactor 1, then by the first agitator 12 reactant and water are well mixed, led in the process into the first reactor 1
Enter inert protective gas；It will be put into the second reactor 2, then stirred by second for preparing the reactant and water of lead precursor solution
Mix device 22 to be well mixed reactant and water, and pH adjusting agent is passed through into the first reactor 1 and adjust pH value to 10, then will prepare
Good selenium precursor solution is added in lead precursor solution, and room is cooled to after being heated to 120 DEG C, reaction 30min by heater 5
Temperature, is filtered by filtration wash unit 7 and filter cake is washed by ethanol solution, repeatedly filtration washing, until pH value is
8；Filter cake is delivered into hollander tub 8 carry out mashing processing, it is to avoid material lumps in the drying process, the material for completing mashing is sent
Dried to spray dryer 9, produce nano lead-selenide.
In above process, the selenium precursor solution in the first reactor 1 first can also be preheated to 80 DEG C, it is anti-by second
Answer the lead precursor solution in kettle 2 to be preheated to 80 DEG C, then the selenium precursor solution for being preheated to 80 DEG C is added be preheated to 80 DEG C of lead
In precursor solution, then the mixed solution is heated to 120 DEG C prepares nano lead-selenide.
More than, it is only the embodiment of the present invention, but protection scope of the present invention is not limited thereto, and it is any to be familiar with
Those skilled in the art the invention discloses technical scope in, change or replacement can be readily occurred in, should all be covered
Within protection scope of the present invention.Therefore, protection scope of the present invention should be defined by scope of the claims.
Claims (10)
1. a kind of system for preparing nano lead-selenide, it is characterised in that the system includes：
First reactor, it is used to prepare selenium precursor solution；
Second reactor, it is used to prepare lead precursor solution and/or selenizing lead materials；
Gas shield device, it is used to be passed through protective gas into first reactor；
PH adjusting meanss, it is used for the pH value for adjusting the lead precursor solution；
Heater, it is used to heat first reactor and/or second reactor；
Conveying device, it is used to the selenium precursor solution in first reactor being delivered in first reactor,
With the lead precursor solution reaction generation selenizing lead materials；
Filtration wash unit, it is used to filter and/or cleans the selenizing lead materials；
Hollander tub, it is used to that lead selenide slurry will to be broken into through the selenizing lead materials；
Spray dryer, it is used to dry the lead selenide slurry, completes the preparation of nano lead-selenide.
2. system according to claim 1, it is characterised in that first reactor includes the first kettle, described first
There is the first chamber for being used for preparing the selenium precursor solution, the top of the first chamber is provided with the first agitator in kettle,
First agitator can be stirred to the selenium precursor solution in first kettle；First kettle is provided with
The first inlet for injecting solution to the first chamber, and for injecting protective gas into the first chamber
Air inlet.
3. system according to claim 2, it is characterised in that the gas shield device includes multiple gas tanks in parallel,
Each gas tank can inject protective gas by the air inlet into the first chamber.
4. the system according to any one of claims 1 to 3, it is characterised in that the protective gas is inert gas.
5. system according to claim 1, it is characterised in that second reactor includes the second kettle, described second
There is the second chamber for being used for preparing the lead precursor solution, the top of the second chamber is provided with the second agitator in kettle,
Second agitator can be stirred to the lead precursor solution or the selenizing lead materials in second kettle；
Second kettle is provided with least three second inlets for being used for that solution to be injected to the second chamber.
6. system according to claim 5, it is characterised in that the pH adjusting meanss include pH sensors, the pH is passed
Sensor is arranged in the second chamber, the pH value for detecting the lead precursor solution in second kettle.
7. system according to claim 1, it is characterised in that the hollander tub, which includes having in cell body, the cell body, to be used
In the 3rd chamber for accommodating the selenizing lead materials, the bottom of the 3rd chamber is provided with dynamic mixers, the 3rd chamber
Side wall be provided with the static mixer that is engaged with the dynamic mixers.
8. system according to claim 7, it is characterised in that the static mixer includes being arranged on the 3rd chamber
Side wall on baffle plate, the baffle plate provided with mashing tooth.
9. system according to claim 1, it is characterised in that in first reactor and second reactor respectively
Provided with temperature sensor.
10. system according to claim 9, it is characterised in that the system also includes control device, the control device
Respectively with first reactor, second reactor, the gas shield device, the pH adjusting meanss, the heating
Device, the conveying device, the filtration wash unit, the hollander tub, the spray dryer and TEMP dress
Confidence number is connected.
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| CN201710599189.4A CN107311121A (en) | 2017-07-21 | 2017-07-21 | A kind of system for preparing nano lead-selenide |
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