CN114887567A - Hydrogen selenide continuous synthesis equipment and method - Google Patents
Hydrogen selenide continuous synthesis equipment and method Download PDFInfo
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- CN114887567A CN114887567A CN202210526833.6A CN202210526833A CN114887567A CN 114887567 A CN114887567 A CN 114887567A CN 202210526833 A CN202210526833 A CN 202210526833A CN 114887567 A CN114887567 A CN 114887567A
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- 229910000058 selane Inorganic materials 0.000 title claims abstract description 115
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 32
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title abstract description 16
- SPVXKVOXSXTJOY-UHFFFAOYSA-N selane Chemical compound [SeH2] SPVXKVOXSXTJOY-UHFFFAOYSA-N 0.000 title 1
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims abstract description 197
- 239000001257 hydrogen Substances 0.000 claims abstract description 179
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 179
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 155
- 239000007788 liquid Substances 0.000 claims abstract description 147
- 238000006243 chemical reaction Methods 0.000 claims abstract description 141
- 229910052711 selenium Inorganic materials 0.000 claims abstract description 53
- 239000011669 selenium Substances 0.000 claims abstract description 53
- 238000000746 purification Methods 0.000 claims abstract description 40
- 150000002431 hydrogen Chemical class 0.000 claims abstract description 27
- 238000004519 manufacturing process Methods 0.000 claims abstract description 13
- 239000007787 solid Substances 0.000 claims description 28
- 238000003860 storage Methods 0.000 claims description 28
- 239000007789 gas Substances 0.000 claims description 24
- 238000002844 melting Methods 0.000 claims description 18
- 230000008018 melting Effects 0.000 claims description 18
- 238000007599 discharging Methods 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 12
- 238000009826 distribution Methods 0.000 claims description 10
- 238000001308 synthesis method Methods 0.000 claims description 10
- 230000000750 progressive effect Effects 0.000 claims description 9
- 230000005540 biological transmission Effects 0.000 claims description 7
- 238000005056 compaction Methods 0.000 claims description 7
- 238000000926 separation method Methods 0.000 claims description 7
- 239000003507 refrigerant Substances 0.000 claims description 5
- 230000000149 penetrating effect Effects 0.000 claims description 4
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- 239000000463 material Substances 0.000 description 5
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- 239000003595 mist Substances 0.000 description 4
- 230000001174 ascending effect Effects 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 230000002349 favourable effect Effects 0.000 description 3
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- 229910000831 Steel Inorganic materials 0.000 description 2
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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
-
- 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
- B01J10/00—Chemical processes in general for reacting liquid with gaseous media other than in the presence of solid particles, or apparatus specially adapted therefor
-
- 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
- B01J19/0053—Details of the reactor
-
- 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
- B01J19/0053—Details of the reactor
- B01J19/0066—Stirrers
-
- 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
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
-
- 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
- C01B19/04—Binary compounds including binary selenium-tellurium compounds
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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Abstract
The invention discloses a hydrogen selenide continuous synthesis device and a method thereof, wherein the hydrogen selenide continuous synthesis device comprises: the device comprises a feeder, a reaction kettle, a gas-liquid purification separator and a hydrogen circulation assembly, wherein the feeder is communicated with the reaction kettle through a pipeline and used for conveying liquid selenium to the reaction kettle; the reaction kettle is communicated with the gas-liquid purification separator through a pipeline and is used for realizing the gas-liquid reaction of the liquid selenium and the hydrogen to generate the hydrogen selenide; the gas-liquid purification separator is communicated with the hydrogen circulation assembly through a pipeline and is used for separating and purifying the hydrogen selenide and the unreacted hydrogen to form the separated unreacted hydrogen and liquid hydrogen selenide; the hydrogen circulation component is communicated with the reaction kettle through a pipeline and is used for inputting the separated unreacted hydrogen and the new hydrogen into the reaction kettle together. The invention can recycle the unreacted hydrogen, improve the utilization rate of the raw material, reduce the consumption of the raw material hydrogen and reduce the production cost. The invention can give consideration to multiple functions, has high integration degree and greatly reduces the industrial production investment.
Description
Technical Field
The invention belongs to the technical field of hydrogen selenide production, and particularly relates to hydrogen selenide continuous synthesis equipment and a hydrogen selenide continuous synthesis method.
Background
Hydrogen selenide electronic gas is widely used in the semiconductor industry, solar energy industry, laser industry and aerospace industry. Such as: hydrogen selenide can form a P-N protective layer and an isolation layer on the surface of a semiconductor, the hydrogen selenide is a necessary raw material for manufacturing an infrared optical material, the hydrogen selenide is a basic raw material of a novel photovoltaic solar cell, and the hydrogen selenide is doped gas in the manufacturing of an LED integrated circuit, and the like.
The existing hydrogen selenide production process is complex, has low integration degree and is easy to cause environmental pollution.
Disclosure of Invention
In order to solve the technical problems, the invention provides hydrogen selenide continuous synthesis equipment and a hydrogen selenide continuous synthesis method.
In order to achieve the purpose, the technical scheme of the invention is as follows:
in one aspect, the invention discloses a continuous synthesis device of hydrogen selenide, comprising:
the charging machine is communicated with the reaction kettle through a pipeline and is used for conveying liquid selenium to the reaction kettle;
the reaction kettle is communicated with the gas-liquid purification separator through a pipeline and is used for realizing gas-liquid reaction of the liquid selenium and the hydrogen to generate hydrogen selenide;
the gas-liquid purification separator is communicated with the hydrogen circulation assembly through a pipeline and is used for separating and purifying the hydrogen selenide and the unreacted hydrogen to form separated unreacted hydrogen and liquid hydrogen selenide;
and the hydrogen circulation component is communicated with the reaction kettle through a pipeline and is used for inputting the separated unreacted hydrogen and new hydrogen into the reaction kettle together.
The invention discloses a hydrogen selenide continuous synthesis device, which specifically comprises: feeder, reation kettle, gas-liquid purification separator and hydrogen circulation subassembly have following beneficial effect:
first, the invention can recycle unreacted hydrogen, improve the utilization rate of raw materials, reduce the consumption of raw material hydrogen and reduce the production cost.
Secondly, the invention can give consideration to multiple functions, has high integration degree and greatly reduces the industrial production investment.
On the basis of the technical scheme, the following improvements can be made:
as a preferred scheme, the charging machine comprises: the feeding shell is provided with a feeding hole for solid selenium powder to enter and a discharging hole for liquid selenium to flow out.
By adopting the preferable scheme, the continuous feeding is realized by using the feeding machine with a screw rod structure, the solid selenium powder can be effectively converted into liquid selenium, and the synthesis rate of hydrogen selenide in a subsequent reaction kettle is improved.
Preferably, the screw of the feeder is sequentially provided with a feeding metering section, a progressive compaction section and a discharging melting section along the selenium conveying direction;
the feeding metering section is used for metering and conveying solid selenium powder;
the progressive compaction section is used for compacting the solid selenium powder;
and the discharging melting section is used for melting the solid selenium powder into liquid selenium.
By adopting the preferable scheme, the feeder has the functions of metering, melting, continuously supplementing and the like of the solid selenium powder.
Preferably, the reaction kettle comprises: the reaction tank comprises a reaction tank body with an inner cavity, a heating sleeve arranged on the outer wall of the reaction tank body, a stirrer and a hydrogen distributor arranged at the bottom of the inner cavity of the reaction tank body;
the top of the reaction tank body is provided with a feeding port for liquid selenium to flow in, the top of the reaction tank body is also provided with a discharge port for hydrogen selenide and unreacted hydrogen to flow out, the reaction tank body is communicated with a hydrogen circulation assembly through a hydrogen conveying pipe, and the hydrogen conveying pipe is used for conveying hydrogen to the bottom of an inner cavity of the reaction tank body.
By adopting the preferable scheme, the reaction kettle has a skillful structure, the selenium and hydrogen react in an endothermic way, and the heat required by the reaction is provided by adopting a heating jacket mode.
Hydrogen enters from the bottom of the inner cavity of the reaction tank body through the hydrogen distributor, gas fully contacts with liquid selenium in the ascending process of the reaction kettle to react, generated hydrogen selenide gas and unreacted hydrogen are gathered on the upper part of the liquid level of the reaction kettle, and a discharge hole at the top of the reaction kettle continuously enters the gas-liquid purification separator through a pipeline in a gas form.
Preferably, the agitator includes: the stirring driving device and the multilayer downward pressing type stirring paddle are in transmission connection with the stirring driving device.
By adopting the preferable scheme, the hydrogen is further ensured to be fully contacted with the liquid selenium in the reaction kettle, the reaction is full, and the synthesis rate is improved.
Preferably, the hydrogen distributor is provided with a plurality of distribution holes penetrating through the hydrogen distributor in the thickness direction, and the distribution holes are inclined holes inclined downwards.
By adopting the preferable scheme, the hydrogen enters from the bottom of the inner cavity of the reaction tank body through the hydrogen distributor.
Preferably, the gas-liquid purification separator includes: the upper condenser, the lower liquid storage tank and a connecting piece for connecting the upper condenser and the lower liquid storage tank;
the top of the upper condenser is provided with a gas outlet for outflow of unreacted hydrogen after separation, the top of the lower liquid storage tank is provided with a material inlet for inflow of gaseous hydrogen selenide and unreacted hydrogen, and the bottom of the lower liquid storage tank is provided with a material outlet for outflow of liquid hydrogen selenide.
Adopt above-mentioned preferred scheme, the mist containing gaseous state hydrogen selenide and hydrogen gets into the top of lower part liquid storage pot from the reation kettle top, gaseous state hydrogen selenide in the mist is stored to the liquid hydrogen selenide in the liquid storage pot by the upper portion condenser cooling, in hydrogen that is not condensed gets into the storage tank through the condenser, gaseous state hydrogen selenide that gets into in the gas-liquid purification separator simultaneously reduces at the condensation in-process along with the volume, and pressure reduction is favorable to the gas at reation kettle top to get into the gas-liquid purification separator.
As the preferred scheme, the outer wall of the lower liquid storage tank is wrapped with a jacket, and the inner cavity of the jacket is provided with refrigerating fluid.
By adopting the preferable scheme, the stability of the performance of the liquid hydrogen selenide is further ensured.
Preferably, the hydrogen circulation module includes:
the feed inlet of the first buffer tank is communicated with the hydrogen outlet of the gas-liquid purification separator through a pipeline, and the discharge outlet of the first buffer tank is communicated with the first feed inlet of the second buffer tank through a pipeline provided with a hydrogen compressor;
and a first feeding port of the second buffer tank is communicated with a hydrogen outlet of the first buffer tank through a pipeline, a second feeding port of the second buffer tank inputs new hydrogen through a pipeline, and a discharge port of the second buffer tank is communicated with the reaction kettle through a pipeline.
With the above preferred aspect, the hydrogen circulation module includes: first buffer tank and second buffer tank through the tube coupling who installs the hydrogen compressor between two buffer tanks, get into unreacted hydrogen in the first buffer tank, compress to the second buffer tank through the hydrogen compressor in, the new hydrogen of raw materials also gets into the second buffer tank simultaneously, supplies the reaction needs.
On the other hand, the invention also discloses a hydrogen selenide continuous synthesis method, which prepares hydrogen selenide by using any one of the hydrogen selenide continuous synthesis devices, and specifically comprises the following steps:
s1: a feeder conveys liquid selenium to the reaction kettle;
s2: the liquid selenium and the hydrogen gas are subjected to gas-liquid reaction in the reaction kettle to generate gaseous hydrogen selenide;
s3: the gas-liquid purification separator separates and purifies the gas-liquid hydrogen selenide and the unreacted hydrogen to form separated unreacted hydrogen and liquid hydrogen selenide;
s4: inputting the unreacted hydrogen and the new hydrogen after separation into the reaction kettle through a hydrogen circulation component;
s5: and repeating the steps S1-S4 until the hydrogen selenide production meets the mass production.
The hydrogen selenide continuous synthesis method provided by the invention has the advantages of simple process and wide applicability.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
Fig. 1 is a schematic structural diagram of a hydrogen selenide continuous synthesis apparatus according to an embodiment of the present invention.
Fig. 2 is a schematic structural diagram of a feeding machine provided in an embodiment of the present invention.
Fig. 3 is a schematic structural diagram of a reaction kettle according to an embodiment of the present invention.
Fig. 4 is a schematic structural diagram of a gas-liquid purification separator provided in an embodiment of the present invention.
Wherein: 1-a feeder, 11-a feeding shell, 12-a screw, 13-a screw driving device, 2-a reaction kettle, 21-a reaction tank body, 22-a heating jacket, 23-a stirrer, 231-a stirring driving device, 232-a multilayer downward-pressing stirring paddle, 24-a hydrogen distributor, 25-a hydrogen conveying pipe, 3-a gas-liquid purification separator, 31-an upper condenser, 32-a lower liquid storage tank, 33-a connecting piece, 34-a jacket, 4-a hydrogen circulating component, 41-a first buffer tank, 42-a second buffer tank and 43-a hydrogen compressor.
Detailed Description
Preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The use of the ordinal terms "first," "second," "third," etc., to describe a common object merely indicate that different instances of like objects are being referred to, and are not intended to imply that the objects so described must be in a given sequence, either temporally, spatially, in ranking, or in any other manner.
Additionally, the expression "comprising" an element is an "open" expression that merely indicates the presence of a corresponding component or step and should not be interpreted as excluding additional components or steps.
In order to achieve the object of the present invention, in some embodiments of the apparatus and method for continuously synthesizing hydrogen selenide, as shown in fig. 1, the apparatus for continuously synthesizing hydrogen selenide comprises: the system comprises a feeder 1, a reaction kettle 2, a gas-liquid purification separator 3 and a hydrogen circulation component 4;
the feeder 1 is communicated with the reaction kettle 2 through a pipeline, and the feeder 1 is used for conveying liquid selenium to the reaction kettle 2;
the reaction kettle 2 is communicated with the gas-liquid purification separator 3 through a pipeline, and the reaction kettle 2 is used for realizing gas-liquid reaction of liquid selenium and hydrogen to generate hydrogen selenide;
the gas-liquid purification separator 3 is communicated with the hydrogen circulation component 4 through a pipeline, and the gas-liquid purification separator 3 is used for separating and purifying the hydrogen selenide and the unreacted hydrogen to form the separated unreacted hydrogen and liquid hydrogen selenide;
the hydrogen circulation component 4 is communicated with the reaction kettle 2 through a pipeline, and the hydrogen circulation component 4 is used for inputting the separated unreacted hydrogen and new hydrogen into the reaction kettle 2 together.
The invention discloses a hydrogen selenide continuous synthesis device, which specifically comprises: feeder 1, reation kettle 2, gas-liquid purification separator 3 and hydrogen circulation subassembly 4 have following beneficial effect:
first, the invention can recycle unreacted hydrogen, improve the utilization rate of raw materials, reduce the consumption of raw material hydrogen and reduce the production cost.
Secondly, the invention can give consideration to multiple functions, has high integration degree and greatly reduces the industrial production investment.
In order to further optimize the implementation effect of the present invention, in other embodiments of the hydrogen selenide continuous synthesis apparatus, the rest features are the same, except that, as shown in fig. 2, the feeder 1 includes: the feeding device comprises a feeding shell 11 with an inner cavity, a screw 12 arranged in the feeding shell 11 and a screw 12 driving device in transmission connection with the screw 12, wherein a feeding hole for solid selenium powder to enter and a discharging hole for liquid selenium to flow out are formed in the feeding shell 11.
By adopting the preferable scheme, the continuous feeding is realized by using the feeding machine 1 with the screw 12 structure, the solid selenium powder can be effectively converted into liquid selenium, and the synthesis rate of hydrogen selenide in the subsequent reaction kettle 2 is improved. It should be noted that the disclosed continuous hydrogen selenide synthesizing apparatus is not limited to a feeder with a screw, but may be other types of feeders.
Further, on the basis of the above embodiment, the screw 12 of the feeder 1 has a feeding metering section, a progressive compacting section and a discharging melting section in sequence along the selenium transportation direction;
the feeding metering section is used for metering and conveying solid selenium powder;
the progressive compaction section is used for compacting the solid selenium powder;
and the discharging melting section is used for melting the solid selenium powder into liquid selenium.
The feeder 1 has the functions of metering, melting, continuously supplementing and the like of solid selenium powder. A feeding metering section, which has the main function of metering and conveying solid selenium powder; the progressive compaction section has the main function of compacting the solid selenium powder conveyed to the progressive compaction section through the change of the screw pitch of the screw 12, so that gas-phase substances in the reaction kettle 2 are prevented from leaking; the discharging melting section has a main function of heating the solid selenium powder to a temperature above the melting point of selenium to melt the solid selenium powder into liquid selenium, and continuously enters the reaction kettle 2.
Further, on the basis of the above embodiment, the rotation speed of the screw 12 of the feeder 1 has a frequency conversion adjusting function, so that the purpose of adjusting the supplemented selenium powder is achieved.
Further, on the basis of the above embodiment, the solid selenium powder is heated to 250 ℃ to 300 ℃ in the advancing process in the discharging and melting section, and the selenium at the outlet enters the reaction kettle 2 in a liquid state.
In order to further optimize the implementation effect of the present invention, in other embodiments of the hydrogen selenide continuous synthesis apparatus, the rest features are the same, except that, as shown in fig. 3, the reaction kettle 2 includes: a reaction tank body 21 with an inner cavity, a heating jacket 22 arranged on the outer wall of the reaction tank body 21, a stirrer 23 and a hydrogen distributor 24 arranged at the bottom of the inner cavity of the reaction tank body 21;
the top of the reaction tank body 21 is provided with a feeding port for liquid selenium to flow in, the top of the reaction tank body is also provided with a discharging port for hydrogen selenide and unreacted hydrogen to flow out, the reaction tank body 21 is communicated with the hydrogen circulation component 4 through a hydrogen conveying pipe 25, and the hydrogen conveying pipe 25 is used for conveying hydrogen to the bottom of the inner cavity of the reaction tank body 21.
By adopting the preferable scheme, the reaction kettle 2 has a smart structure, the reaction of selenium and hydrogen is endothermic, and the heat required by the reaction is provided by adopting a heating jacket 22.
Hydrogen enters from the bottom of the inner cavity of the reaction tank body 21 through the hydrogen distributor 24, gas fully contacts with liquid selenium in the ascending process of the reaction kettle 2 to react, generated hydrogen selenide gas and unreacted hydrogen are gathered on the upper part of the liquid level of the reaction kettle 2, and the hydrogen selenide gas and the unreacted hydrogen continuously enter the gas-liquid purification separator 3 through a pipeline in a gas form from a discharge hole at the top of the reaction kettle 2.
The liquid level of the reaction kettle 2 is supplemented with liquid selenium through the feeder 1 to keep basic balance, and the charging coefficient is preferably 60-80%.
Further, on the basis of the above embodiment, the agitator 23 includes: stirring drive arrangement 231 and with stirring drive arrangement 231 transmission connection's multilayer down-pressure formula stirring rake 232, further guarantee that hydrogen fully contacts with liquid selenium inside reation kettle 2, the reaction is abundant, improves the synthetic rate.
Specifically, the diameter of the stirring paddle is 70% -85% of the inner diameter of the reaction tank body 21.
Further, on the basis of the above embodiment, the hydrogen distributor 24 is provided with a plurality of distribution holes penetrating through the thickness direction thereof, the distribution holes are inclined holes inclined downward, and hydrogen enters from the bottom of the inner cavity of the reaction tank body 21 through the hydrogen distributor 24.
Specifically, the central axis of the distribution holes is at an acute angle, in some embodiments, 60 ° from the end face or thickness direction of the hydrogen distributor 24.
Specifically, the hydrogen distributor 24 is circular ring-shaped, and the diameter of the circular ring is 40% -60% of the inner diameter of the reaction tank body 21.
Further, in the above embodiment, the ratio of the height of the reactor vessel 21 to the diameter thereof is 2.5 to 4, and the length-diameter ratio of the reactor vessel 2 is larger than that of the conventional apparatus.
Further, it is preferable that the ratio of the height of the reaction vessel body 21 to the diameter thereof is 3.
Further, on the basis of the above embodiment, the heating jacket 22 is a ceramic electric heating jacket 22, and the ceramic electric heating jacket 22 is used to provide the heat required for the reaction.
Specifically, the heating jacket 22 is automatically controlled to maintain the reaction temperature at 400 ℃ to 600 ℃. Further, the temperature is preferably 500 ℃.
Further, on the basis of the above embodiment, the hydrogen delivery pipe 25 is installed along the inner wall of the inner cavity of the reaction tank 21 from top to bottom, and can deliver hydrogen to the bottom of the inner cavity of the reaction tank 21.
Further, on the basis of the above embodiment, the reaction temperature in the reaction kettle 2 is 400-600 ℃, preferably 500 ℃, the reaction pressure is 0.2-0.6 MPa, and the molar ratio of selenium to hydrogen is more than 1: 3.
The reaction of selenium and hydrogen is endothermic, and the direct synthesis of hydrogen selenide by selenium and hydrogen has no side reaction and high yield. High-purity selenium powder and high-purity hydrogen are selected as raw materials, and 99.99 percent of high-purity hydrogen selenide can be produced without human impurities in the operations of equipment processing, installation, equipment cleaning, charging, conveying, reaction and filling.
Further, on the basis of the above embodiment, the top of the reaction vessel 2 is provided with one or more of the following components: safety valves, pressure gauges, thermometers, level gauges, etc.
In order to further optimize the implementation effect of the present invention, in other embodiments of the hydrogen selenide continuous synthesis apparatus, the rest features are the same, except that, as shown in fig. 4, the gas-liquid purification separator 3 includes: an upper condenser 31, a lower receiver 32, and a connecting member 33 for connecting the upper condenser 31 and the lower receiver 32;
the top of the upper condenser 31 is provided with a gas outlet for outflow of unreacted hydrogen after separation, the top of the lower liquid storage tank 32 is provided with a material inlet for inflow of gaseous hydrogen selenide and unreacted hydrogen, and the bottom of the lower liquid storage tank 32 is provided with a material outlet for outflow of liquid hydrogen selenide.
Adopt above-mentioned preferred scheme, the mist that contains gaseous state hydrogen selenide and hydrogen gets into the top of lower part liquid storage pot 32 from reation kettle 2 top, gaseous state hydrogen selenide in the mist is stored to lower part liquid storage pot 32 for liquid hydrogen selenide by upper portion condenser 31 cooling, hydrogen that is not condensed passes through the condenser and gets into in the storage tank, gaseous state hydrogen selenide that gets into in gas-liquid purification separator 3 simultaneously accompanies the volume reduction in the condensation process, pressure reduction, be favorable to the gas at reation kettle 2 top to get into gas-liquid purification separator 3.
Further, on the basis of the above embodiment, the outer wall of the lower liquid storage tank 32 is wrapped by the jacket 34, and the inner cavity of the jacket 34 is provided with the refrigerant, so as to further ensure the stability of the performance of the liquid hydrogen selenide.
In some embodiments, the upper condenser 31 is a shell and tube condenser through which a refrigerant fluid is passed, and the condenser is elongated.
In some embodiments, the lower reservoir 32 is a structure with a level gauge, a temperature gauge, and a baffle on the top.
Further, on the basis of the above embodiment, the mixed gas entering the gas-liquid purification separator 3 needs to be cooled to a temperature of-40 ℃ to-60 ℃, preferably to a temperature of-50 ℃, so that the hydrogen selenide is condensed into a liquid state.
Further, on the basis of the above embodiment, the bottom of the gas-liquid purification separator 3 is provided with a discharge valve, when the liquid level gauge of the lower liquid storage tank 32 displays that the liquid level reaches a certain value, the discharge valve at the bottom is opened, and the liquid enters the steel cylinder which is processed in advance through the precision filter.
In order to further optimize the implementation effect of the present invention, in other embodiments of the hydrogen selenide continuous synthesis apparatus, the remaining features are the same, except that the hydrogen circulation assembly 4 includes:
a first buffer tank 41, wherein the feeding port of the first buffer tank 41 is communicated with the hydrogen outlet of the gas-liquid purification separator 3 through a pipeline, and the discharging port of the first buffer tank 41 is communicated with the first feeding port of the second buffer tank 42 through a pipeline provided with a hydrogen compressor 43;
and a first feeding port of the second buffer tank 42 is communicated with a hydrogen outlet of the first buffer tank 41 through a pipeline, a second feeding port of the second buffer tank 42 inputs new hydrogen through a pipeline, and a discharge port of the second buffer tank is communicated with the reaction kettle 2 through a pipeline.
With the above preferred embodiment, the hydrogen circulation module 4 includes: the first buffer tank 41 and the second buffer tank 42 are connected through a pipeline provided with a hydrogen compressor 43, unreacted hydrogen entering the first buffer tank 41 is compressed to the second buffer tank 42 through the hydrogen compressor 43, and meanwhile, new hydrogen of the raw material also enters the second buffer tank 42 for reaction.
In addition, the invention also discloses a hydrogen selenide continuous synthesis method, which prepares hydrogen selenide by using the hydrogen selenide continuous synthesis equipment disclosed by any embodiment, and specifically comprises the following steps:
s1: the feeder 1 conveys liquid selenium to the reaction kettle 2;
s2: the liquid selenium and the hydrogen gas are subjected to gas-liquid reaction in the reaction kettle 2 to generate gaseous hydrogen selenide;
s3: the gaseous hydrogen selenide and the unreacted hydrogen enter the gas-liquid purification separator 3 through a pipeline, and the gas-liquid purification separator 3 separates and purifies the gaseous hydrogen selenide and the unreacted hydrogen to form separated unreacted hydrogen and liquid hydrogen selenide;
s4: the unreacted hydrogen and the new hydrogen after separation are input into the reaction kettle 2 through the hydrogen circulation component 4;
s5: and repeating the steps S1-S4 until the hydrogen selenide production meets the mass production.
In order to further optimize the implementation effect of the present invention, in other embodiments of the hydrogen selenide continuous synthesis method, the rest features are the same, except that the feeder 1 includes: the feeding device comprises a feeding shell 11 with an inner cavity, a screw 12 arranged in the feeding shell 11 and a screw 12 driving device in transmission connection with the screw 12, wherein a feeding hole for solid selenium powder to enter and a discharging hole for liquid selenium to flow out are formed in the feeding shell 11.
S1 specifically includes the contents: along the transportation direction of selenium, the solid selenium powder is metered and conveyed by a feeding metering section of a screw 12 of the feeder 1, the solid selenium powder is compacted by a progressive compacting section of the screw 12 of the feeder 1, and the solid selenium powder is fused into liquid selenium by a discharging melting section of the screw 12 of the feeder 1.
Further, on the basis of the above embodiment, the solid selenium powder is heated to 250-300 ℃ in the process of advancing in the discharging and melting section, and the selenium at the outlet enters the reaction kettle 2 in a liquid state.
In order to further optimize the implementation effect of the present invention, in other embodiments of the continuous synthesis method of hydrogen selenide, the rest features are the same, except that the reaction kettle 2 comprises: a reaction tank body 21 with an inner cavity, a heating jacket 22 arranged on the outer wall of the reaction tank body 21, a stirrer 23 and a hydrogen distributor 24 arranged at the bottom of the inner cavity of the reaction tank body 21;
the top of the reaction tank body 21 is provided with a feeding port for liquid selenium to flow in, the top of the reaction tank body is also provided with a discharging port for hydrogen selenide and unreacted hydrogen to flow out, the reaction tank body 21 is communicated with the hydrogen circulation component 4 through a hydrogen conveying pipe 25, and the hydrogen conveying pipe 25 is used for conveying hydrogen to the bottom of the inner cavity of the reaction tank body 21.
S2 specifically includes the contents: hydrogen enters from the bottom of the inner cavity of the reaction tank body 21 through the hydrogen distributor 24, gas fully contacts with liquid selenium in the ascending process of the reaction kettle 2 to react, generated hydrogen selenide gas and unreacted hydrogen are gathered on the upper part of the liquid level of the reaction kettle 2, and the hydrogen selenide gas and the unreacted hydrogen continuously enter the gas-liquid purification separator 3 through a pipeline in a gas form from a discharge hole at the top of the reaction kettle 2.
The liquid level of the reaction kettle 2 is supplemented with liquid selenium through the feeder 1 to keep basic balance, and the charging coefficient is preferably 60-80%.
Further, on the basis of the above embodiment, the agitator 23 includes: stirring drive arrangement 231 and with stirring drive arrangement 231 transmission connection's multilayer push down formula stirring rake 232, further guarantee that hydrogen is abundant contact with liquid selenium in reation kettle 2 inside, the reaction is abundant, improves the synthetic rate.
Specifically, the diameter of the stirring paddle is 70% -85% of the inner diameter of the reaction tank body 21.
Further, on the basis of the above embodiment, the hydrogen distributor 24 is provided with a plurality of distribution holes penetrating through the thickness direction thereof, the distribution holes are inclined holes inclined downward, and hydrogen enters from the bottom of the inner cavity of the reaction tank body 21 through the hydrogen distributor 24.
Specifically, the central axis of the distribution holes is at an acute angle, in some embodiments, 60 ° from the end face or thickness direction of the hydrogen distributor 24.
Specifically, the hydrogen distributor 24 is circular ring-shaped, and the diameter of the circular ring is 40% -60% of the inner diameter of the reaction tank body 21.
Further, in the above embodiment, the ratio of the height of the reactor vessel 21 to the diameter thereof is 2.5 to 4, and the length-diameter ratio of the reactor vessel 2 is larger than that of the conventional apparatus.
Further, it is preferable that the ratio of the height of the reaction vessel body 21 to the diameter thereof is 3.
Further, on the basis of the above embodiment, the heating jacket 22 is a ceramic electric heating jacket 22, and the way of the ceramic electric heating jacket 22 is adopted to provide the heat required by the reaction.
Specifically, the heating jacket 22 is automatically controlled to maintain the reaction temperature at 400 ℃ to 600 ℃. Further, the temperature is preferably 500 ℃.
Further, on the basis of the above embodiment, the hydrogen delivery pipe 25 is installed along the inner wall of the inner cavity of the reaction tank 21 from top to bottom, and can deliver hydrogen to the bottom of the inner cavity of the reaction tank 21.
Further, on the basis of the above embodiment, the reaction temperature in the reaction kettle 2 is 400-600 ℃, preferably 500 ℃, the reaction pressure is 0.2-0.6 MPa, and the molar ratio of selenium to hydrogen is more than 1: 3.
The reaction of selenium and hydrogen is endothermic, and the direct synthesis of hydrogen selenide by selenium and hydrogen has no side reaction and high yield. High-purity selenium powder and high-purity hydrogen are selected as raw materials, and 99.99 percent of high-purity hydrogen selenide can be produced without human impurities in the operations of equipment processing, installation, equipment cleaning, charging, conveying, reaction and filling.
Further, on the basis of the above embodiment, the top of the reaction vessel 2 is provided with one or more of the following components: safety valves, pressure gauges, thermometers, level gauges, etc.
In order to further optimize the implementation effect of the present invention, in other embodiments of the continuous synthesis method of hydrogen selenide, the rest features are the same, except that the gas-liquid purification separator 3 includes: an upper condenser 31, a lower receiver 32, and a connecting member 33 for connecting the upper condenser 31 and the lower receiver 32;
the top of the upper condenser 31 is provided with a gas outlet for outflow of unreacted hydrogen after separation, the top of the lower liquid storage tank 32 is provided with a feeding port for inflow of gaseous hydrogen selenide and unreacted hydrogen, and the bottom of the lower liquid storage tank 32 is provided with a discharge port for outflow of liquid hydrogen selenide.
S3 specifically includes the following: the top that contains gaseous state hydrogen selenide and hydrogen gets into lower part liquid storage pot 32 from reation kettle 2 top, gaseous state hydrogen selenide among the mixed gas is stored to lower part liquid storage pot 32 for liquid hydrogen selenide by upper portion condenser 31 cooling, in hydrogen that is not condensed gets into the storage pot through the condenser, gaseous state hydrogen selenide that gets into in gas-liquid purification separator 3 simultaneously reduces at the condensation in-process along with the volume, pressure reduction, be favorable to the gas at reation kettle 2 top to get into gas-liquid purification separator 3.
Further, on the basis of the above embodiment, the outer wall of the lower liquid storage tank 32 is wrapped by the jacket 34, and the inner cavity of the jacket 34 is provided with the refrigerant, so as to further ensure the stability of the performance of the liquid hydrogen selenide.
In some embodiments, the upper condenser 31 is a shell and tube condenser through which a refrigerant fluid is passed, and the condenser is of an elongated configuration.
In some embodiments, the lower reservoir 32 is a structure with a level gauge, a temperature gauge, and a baffle on the top.
Further, on the basis of the above embodiment, the mixed gas entering the gas-liquid purification separator 3 needs to be cooled to a temperature of-40 ℃ to-60 ℃, preferably to a temperature of-50 ℃, so that the hydrogen selenide is condensed into a liquid state.
Further, on the basis of the above embodiment, the bottom of the gas-liquid purification separator 3 is provided with a discharge valve, when the liquid level gauge of the lower liquid storage tank 32 displays that the liquid level reaches a certain value, the discharge valve at the bottom is opened, and the liquid enters the steel cylinder which is processed in advance through the precision filter.
In order to further optimize the implementation effect of the present invention, in other embodiments of the continuous synthesis method of hydrogen selenide, the rest features are the same, except that the hydrogen circulation module 4 includes:
a first buffer tank 41, wherein the feeding port of the first buffer tank 41 is communicated with the hydrogen outlet of the gas-liquid purification separator 3 through a pipeline, and the discharging port of the first buffer tank 41 is communicated with the first feeding port of the second buffer tank 42 through a pipeline provided with a hydrogen compressor 43;
a second buffer tank 42, a first feeding port of the second buffer tank 42 is communicated with a hydrogen outlet of the first buffer tank 41 through a pipeline, a second feeding port of the second buffer tank is fed with new hydrogen through a pipeline, and a discharge port of the second buffer tank is communicated with the reaction kettle 2 through a pipeline.
S4 specifically includes the following: the hydrogen circulation module 4 includes: the first buffer tank 41 and the second buffer tank 42 are connected through a pipeline provided with a hydrogen compressor 43, unreacted hydrogen entering the first buffer tank 41 is compressed to the second buffer tank 42 through the hydrogen compressor 43, and meanwhile, new hydrogen of the raw material also enters the second buffer tank 42 for reaction.
The various embodiments above may be implemented in cross-parallel.
To sum up, the invention discloses hydrogen selenide continuous synthesis equipment and a method, and the whole process comprises the following steps: 1) metering, melting and continuously replenishing solid selenium powder; 2) carrying out gas-liquid reaction on the liquid selenium and the hydrogen; 3) separating and purifying gaseous hydrogen selenide and raw material hydrogen; 4) the separated unreacted hydrogen is recycled, the process is simple, and the applicability is wide.
The equipment disclosed by the invention has multiple functions, is high in integration degree, and can greatly reduce the industrial production investment.
Meanwhile, the invention opens up a new engineering technical route for metering and conveying the high-melting-point solid and carrying out the melting gas-liquid reaction, and can be used as a demonstration of the reaction of other high-melting-point liquid and gas.
In the description of the present invention, it is to be understood that the terms "coaxial", "bottom", "one end", "top", "middle", "other end", "upper", "one side", "top", "inner", "front", "center", "both ends", and the like, indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplicity of description, and do not indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and thus, are not to be construed as limiting the present invention.
In the present invention, unless otherwise expressly specified or limited, the terms "mounted," "disposed," "connected," "secured," "screwed" and the like are to be construed broadly, e.g., as meaning fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; the terms may be directly connected or indirectly connected through an intermediate, and may be communication between two elements or interaction relationship between two elements, unless otherwise specifically limited, and the specific meaning of the terms in the present invention will be understood by those skilled in the art according to specific situations.
While there have been shown and described what are at present considered to be the fundamental principles of the invention and its essential features and advantages, it will be understood by those skilled in the art that the invention is not limited by the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the invention as defined by the appended claims and their equivalents.
The control mode of the invention is controlled by manually starting and closing the switch, the wiring diagram of the power element and the supply of the power supply belong to the common knowledge in the field, and the invention is mainly used for protecting mechanical devices, so the control mode and the wiring arrangement are not explained in detail in the invention.
Claims (10)
1. Continuous synthesis equipment of hydrogen selenide, which is characterized by comprising:
the charging machine is communicated with the reaction kettle through a pipeline and is used for conveying liquid selenium to the reaction kettle;
the reaction kettle is communicated with the gas-liquid purification separator through a pipeline and is used for realizing gas-liquid reaction of the liquid selenium and the hydrogen to generate gaseous hydrogen selenide;
the gas-liquid purification separator is communicated with the hydrogen circulation assembly through a pipeline and is used for separating and purifying the hydrogen selenide and the unreacted hydrogen to form separated unreacted hydrogen and liquid hydrogen selenide;
and the hydrogen circulation component is communicated with the reaction kettle through a pipeline and is used for inputting the separated unreacted hydrogen and new hydrogen into the reaction kettle together.
2. The continuous synthesis apparatus of hydrogen selenide according to claim 1, wherein the feeder comprises: the feeding device comprises a feeding shell with an inner cavity, a screw rod arranged in the feeding shell and a screw rod driving device in transmission connection with the screw rod, wherein a feeding hole for solid selenium powder to enter and a discharging hole for liquid selenium to flow out are formed in the feeding shell.
3. The continuous synthesis apparatus of hydrogen selenide according to claim 2, wherein the screw of the feeder has a feed metering section, a progressive compaction section and an exit melting section in this order along the transport direction of selenium;
the feeding metering section is used for metering and conveying solid selenium powder;
the progressive compaction section is used for compacting the solid selenium powder;
and the discharging melting section is used for melting the solid selenium powder into liquid selenium.
4. The continuous synthesis apparatus of hydrogen selenide according to claim 1, wherein the reaction kettle comprises: the reaction tank comprises a reaction tank body with an inner cavity, a heating sleeve arranged on the outer wall of the reaction tank body, a stirrer and a hydrogen distributor arranged at the bottom of the inner cavity of the reaction tank body;
the top of the reactor body is provided with a feeding port for liquid selenium to flow in, the top of the reactor body is also provided with a discharge port for hydrogen selenide and unreacted hydrogen to flow out, the reactor body is communicated with the hydrogen circulation assembly through a hydrogen conveying pipe, and the hydrogen conveying pipe is used for conveying hydrogen to the bottom of the inner cavity of the reactor body.
5. The continuous synthesis apparatus of hydrogen selenide according to claim 4, wherein the agitator comprises: the stirring driving device and the multilayer downward pressing type stirring paddle are in transmission connection with the stirring driving device.
6. The continuous synthesis apparatus of claim 4, wherein the hydrogen distributor is provided with a plurality of distribution holes penetrating through the thickness direction of the hydrogen distributor, and the distribution holes are inclined holes inclined downward.
7. The continuous synthesis apparatus of hydrogen selenide according to claim 1, wherein the gas-liquid purification separator comprises: the upper part condenser, the lower part liquid storage tank and a connecting piece for connecting the upper part condenser and the lower part liquid storage tank;
the top of upper portion condenser is equipped with the gas outlet that is used for the unreacted hydrogen after the separation to flow out the top of lower part liquid storage pot is equipped with the pan feeding mouth that is used for gaseous state hydrogen selenide and unreacted hydrogen to flow in the bottom of lower part liquid storage pot is equipped with the discharge gate that is used for liquid hydrogen selenide to flow out.
8. The continuous synthesis apparatus of hydrogen selenide according to claim 7, wherein the outer wall of the lower liquid storage tank is wrapped with a jacket, and the inner cavity of the jacket is provided with a refrigerant.
9. The continuous synthesis apparatus of hydrogen selenide according to claim 1, wherein the hydrogen circulation module comprises:
the feed inlet of the first buffer tank is communicated with the hydrogen outlet of the gas-liquid purification separator through a pipeline, and the discharge outlet of the first buffer tank is communicated with the first feed inlet of the second buffer tank through a pipeline provided with a hydrogen compressor;
and a first feeding port of the second buffer tank is communicated with a hydrogen outlet of the first buffer tank through a pipeline, a second feeding port of the second buffer tank inputs new hydrogen through a pipeline, and a discharge port of the second buffer tank is communicated with the reaction kettle through a pipeline.
10. A continuous synthesis method of hydrogen selenide, wherein hydrogen selenide is prepared by using the continuous synthesis apparatus of hydrogen selenide according to any one of claims 1 to 9, comprising the steps of:
s1: a feeder conveys liquid selenium to the reaction kettle;
s2: the liquid selenium and the hydrogen gas are subjected to gas-liquid reaction in the reaction kettle to generate gaseous hydrogen selenide;
s3: the gas-liquid purification separator separates and purifies the gas-liquid hydrogen selenide and the unreacted hydrogen to form separated unreacted hydrogen and liquid hydrogen selenide;
s4: inputting the unreacted hydrogen and the new hydrogen after separation into the reaction kettle through a hydrogen circulation component;
s5: and repeating the steps S1-S4 until the hydrogen selenide production meets the mass production.
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