CN206362178U - A kind of vacuum synthesis stove - Google Patents
A kind of vacuum synthesis stove Download PDFInfo
- Publication number
- CN206362178U CN206362178U CN201621388951.1U CN201621388951U CN206362178U CN 206362178 U CN206362178 U CN 206362178U CN 201621388951 U CN201621388951 U CN 201621388951U CN 206362178 U CN206362178 U CN 206362178U
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- CN
- China
- Prior art keywords
- vacuum
- boiler tube
- tube
- heater
- stove according
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 22
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 25
- 230000008676 import Effects 0.000 claims abstract description 20
- 238000007789 sealing Methods 0.000 claims abstract description 20
- 239000002826 coolant Substances 0.000 claims abstract description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 238000007599 discharging Methods 0.000 claims description 8
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 6
- 238000005259 measurement Methods 0.000 claims description 4
- 239000003708 ampul Substances 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 3
- 238000003780 insertion Methods 0.000 claims description 3
- 230000037431 insertion Effects 0.000 claims description 3
- -1 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 230000005611 electricity Effects 0.000 claims 1
- 239000000376 reactant Substances 0.000 abstract description 7
- 230000004044 response Effects 0.000 abstract description 6
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 14
- PSCMQHVBLHHWTO-UHFFFAOYSA-K Indium trichloride Inorganic materials Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 description 9
- 239000011261 inert gas Substances 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 3
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 229920000915 polyvinyl chloride Polymers 0.000 description 2
- 239000004800 polyvinyl chloride Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 229910002027 silica gel Inorganic materials 0.000 description 2
- 239000000741 silica gel Substances 0.000 description 2
- 229960001866 silicon dioxide Drugs 0.000 description 2
- MARUHZGHZWCEQU-UHFFFAOYSA-N 5-phenyl-2h-tetrazole Chemical compound C1=CC=CC=C1C1=NNN=N1 MARUHZGHZWCEQU-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 238000009533 lab test Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
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- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The utility model provides a kind of vacuum synthesis stove, including tube type high-temperature furnace, glove box, air-washer, tube type high-temperature furnace includes body of heater and boiler tube, the inwall of the body of heater is provided with electric heater unit, the boiler tube is made up of horizontal boiler tube with vertical boiler tube, the left end of the horizontal boiler tube is provided with import sealing flange, import coolant jacket, placing response boat in the horizontal boiler tube, the vertical boiler tube is provided with outlet coolant jacket, exit seal flange, and the exit seal flange lower end is connected with receiving flask sealing.The utility model can effectively carry out heating in vacuum to reactant, and the synthetic product of reaction collects convenient, can carry out situation by observing response at any time.
Description
Technical field
The utility model is related to a kind of vacuum synthesis stove, belongs to compound synthesis apparatus field.
Background technology
With the fast development of flat-panel monitor, the demand for the ito thin film material of transparency electrode therein drastically increases
Plus, and ito thin film material is to use anhydrous InCl3And SnCl4It is dissolved in after mixing by a certain percentage in ethanol and then using spraying heat
Made from solution.Wherein anhydrous InCl3As the important materials of ito thin film, its purity has decisive for the performance of ito thin film
Influence.Current anhydrous InCl3Mainly directly reacted to synthesize using hydrogen chloride and indium, but produce anhydrous InCl3
Legacy equipment there are problems that yield is small, cost is high, purity, and rely primarily on import equipment production, ensure yield,
On the premise of purity, security, the production domesticization of equipment is a major issue for needing to solve.
In utility model patent《The high―temperature nuclei furnace system and the application method of the system of compound, Publication No.
CN103438704A》A kind of synthesizer for producing cadmium telluride is proposed in one text, but the device, without equipment of crystallisation by cooling, nothing is washed
Device of air, body of heater can not be opened when reacting and be unable to observing response situation, it is impossible to for anhydrous InCl3Production.
Utility model content
The deficiency of the utility model regarding to the issue above proposes a kind of vacuum synthesis stove, effectively reactant can be carried out true
Sky is heated, and the synthetic product of reaction collects convenient, can carry out situation by observing response at any time, can use has with corrosive
Malicious reacting gas, and safety and environmental protection.
The utility model is achieved by the following technical programs：
A kind of vacuum synthesis stove, including tube type high-temperature furnace, air-washer, the tube type high-temperature furnace include body of heater and boiler tube,
The inwall of the body of heater is provided with electric heater unit, body of heater be divided into above and below two parts, lower volume right-hand member is provided with through body of heater
Circular hole, the boiler tube is perpendicular type bend pipe, is connected as one by horizontal boiler tube with vertical boiler tube, the horizontal boiler tube is positioned over stove
In vivo, and between electric heater unit, the vertical boiler tube runs through lower volume by circular hole；The left end of the horizontal boiler tube
It is provided with import sealing flange, import coolant jacket, the horizontal boiler tube and is placed with reaction boat；The lower end of the vertical boiler tube is set
Outlet coolant jacket, exit seal flange are equipped with, the exit seal flange lower end is provided with discharging opening, and the discharging opening passes through sealing
Circle is closely coupled with receiving flask, and the receiving flask has support.
The import sealing flange is provided with charging aperture, and the charging aperture is provided with end cap, the end cap and is provided with insertion
Two air inlets and a thermocouple port.
The exit seal flange is provided with gas outlet, and the gas outlet is connected to be provided with vacuum tube, the vacuum tube
Vacuum meter and vacuum valve, the vacuum tube connect air-washer, the air-washer and vacuum means after vacuum valve
Put connected.
Further, the temperature sensor of measurement in-furnace temperature is provided with the boiler tube, the temperature sensor is heat
Galvanic couple, the thermocouple is wrapped in a thin quartz ampoule, and the thermocouple is goed deep into boiler tube by thermocouple port, and is located at
React below boat.
Further, the air-washer includes surge flask, No. 1 Drexel bottle, No. 2 Drexel bottles, No. 1 Drexel bottle and 2
Number Drexel bottle is built with the NaOH solution that concentration is 5 ~ 15%.
Further, the exit seal flange is connected with glove box, and the receiving flask is located in glove box.
Further, the boiler tube and reaction boat are made using high temperature resistant quartz glass, and receiving flask is simple glass
Bottle.
Further, the import sealing flange, end cap, exit seal flange and vacuum valve use polytetrafluoroethylene (PTFE) system
Form.
Further, the electric heater unit is Elema electric heater unit.
Further, the vacuum meter is stainless steel diaphragm.
Further, in addition to temperature controller is connected with the electric heater unit.
According to a kind of vacuum synthesis stove of the present utility model, with it is existing be used to synthesize the device of anhydrous indium chloride compared with,
Have the advantages that：
（1）Boiler tube and reaction boat be all quartz glass, import sealing flange, exit seal flange, end cap are all polytetrafluoros
Ethene, connecting pipe is all polyvinyl chloride, vacuum meter, and valve etc. is all anticorrosive material, is had when reacting gas is that hydrogen chloride is this
During aggressive gas, it is also ensured that the normal of equipment is used, prevent from corroding the hydrogen chloride leakage caused, it is ensured that synthesis
The quality of product and the safety of production.
（2）Course of reaction is that the purity that can improve synthetic product carried out under the protection of vacuum and inert gas ensures
Product quality.
（3）Horizontal boiler tube is provided with temperature sensor, is placed in reacting the lower section of boat, this mode can be to reactant temperature
Degree carries out closely quickly measurement, true temperature numerical value of the measured temperature closer to reactant.
（4）Body of heater be divided into above and below two parts, can open observing response situation in reaction, control the process of reaction.
（5）Boiler tube is furnished with cooling device, can accelerate the crystallisation by cooling of anhydrous indium chloride, raising prepares anhydrous indium chloride
Efficiency.
（6）There is crystallization receiving flask in boiler tube, crystallized product is collected convenient.
（7）Synthetic furnace is connected with air-washer, for toxic gases such as absorbing hydrogen chlorides.Safe preparation process environmental protection.
Brief description of the drawings
Fig. 1 is the structural representation of the utility model synthetic furnace.
Fig. 2 is air-washer structural representation of the present utility model.
In accompanying drawing：1st, boiler tube；2nd, body of heater；3rd, electric heater unit；4 reaction boats；5th, reactant；61st, import coolant jacket；62、
Export coolant jacket；71st, silicagel pad；72nd, exit seal circle；73rd, receiving flask sealing ring；8th, vacuum valve；9th, escape pipe；101st, enter
Mouth sealing flange；102nd, exit seal flange；11st, end cap；12nd, reacting gas air inlet pipe；13 inert gas inleting pipes；14th, it is hot
Galvanic couple；15th, receiving flask；16th, glove box；17th, support；18th, vacuum meter；19th, airway tube；20th, surge flask；21st, No. 1 Drexel bottle；
22nd, No. 2 Drexel bottles；23rd, NaOH solution.
Embodiment
In order that technical problem, technical scheme and beneficial effect that the utility model is solved are more clearly understood, below
With reference to drawings and Examples, the utility model is described in further detail.It should be appreciated that specific reality described herein
Example is applied only to explain the utility model, is not used to limit the utility model.
Fig. 1 is refer to, the utility model specific embodiment provides a kind of vacuum synthesis stove, including tube type high-temperature furnace, gloves
Case 16, air-washer, tube type high-temperature furnace include body of heater 2 and boiler tube 1, and the inwall of the body of heater 2 is provided with electric heater unit 3.Institute
Electric heater unit 3 is stated, Resistant heating device or Elema heater can be used.The synthetic furnace also includes temperature control
Device processed, the temperature controller is connected with the electric heater unit, for controlling the heating-up temperature of body of heater 2.
2 points of body of heater is two parts of upper furnace body and lower volume, and lower volume right-hand member is provided with the circular hole through body of heater.Stove
Pipe 1 is perpendicular type bend pipe, is connected as one by horizontal boiler tube with vertical boiler tube, the horizontal boiler tube is positioned in body of heater 2, and by
Electric heater unit 3 is surrounded.The vertical boiler tube runs through lower volume by circular hole.
The left end of horizontal boiler tube is provided with import sealing flange 101, import coolant jacket 61, and import coolant jacket 61 is enclosed on transverse direction
The left end of the outside of boiler tube, import sealing flange 101 and horizontal boiler tube, which is adopted, to be inlayed or is glued or be interference fitted or screw connection
Mode seal connected.Reaction boat 4 is placed with the horizontal boiler tube.Charging aperture is provided with the import sealing flange 101, institute
State and end cap 11 is installed on charging aperture, two air inlets and a thermocouple port of insertion, the end are provided with the end cap 11
Has silicagel pad 71 in lid, so that it is sealed closely between import sealing flange 101；Reaction is respectively provided with two air inlets
Gas inlet pipe 12 and inert gas inleting pipe 13.The temperature sensor of measurement in-furnace temperature is provided with horizontal boiler tube, it is described
Temperature sensor is thermocouple 14, and the thermocouple 14 is wrapped in a thin quartz ampoule, and it is deep into by thermocouple port
In boiler tube 1, and positioned at the lower section of reaction boat 4, the boiler tube 1 and reaction boat 4 are made using high temperature resistant quartz glass.
The vertical boiler tube is provided with outlet coolant jacket 62, exit seal flange 102, and the outlet coolant jacket 62 is sleeved on
Outside the lower end of vertical boiler tube, the lower end of exit seal flange 102 and vertical boiler tube adopt inlay or be glued or be interference fitted or
The mode of screw connection seals connected.The lower end of exit seal flange 102 is provided with the discharging opening of back taper, the discharging opening band
There is sealing ring 73 to be sealed closely with receiving flask 15, the receiving flask 15 has the support 17 that can be lifted, support 17 is used for branch
Receiving flask 15 is supportted, receiving flask 15 is simple glass bottle.The support 17 and receiving flask 15 of the lifting are respectively positioned in glove box 16, institute
Glove box 16 is stated to be tightly connected with the lower end of exit seal flange 102.
Venthole is provided with the exit seal flange 101, the venthole is connected pacifies on vacuum tube 9, the vacuum tube 9
Equipped with vacuum meter 18 and vacuum valve 8, the vacuum meter 18 is stainless steel diaphragm.
The vacuum tube 18 connects air-washer after vacuum valve 8, and vacuum extractor is connected after air-washer,
Can be by the evacuating air in the boiler tube by vacuum extractor.The import sealing flange 101, end cap 11, exit seal
Flange 102 and vacuum valve 8 are made using polytetrafluoroethylene (PTFE), and connecting pipe is polyvinyl chloride pipe.
Fig. 2 is refer to, the air-washer includes the Drexel bottle 22 of Drexel bottle 21,2 of surge flask 20,1；The Drexel bottle
Built with the NaOH solution 23 that concentration is 5 ~ 15%, air-washer is connected by airway tube 19.
A kind of process of vacuum synthesis stove in the present embodiment, its operation principle is as follows；
The first step, opens charging aperture end cap 11, will be equipped with the reaction boat 4 of reactant 5, is put into the end of horizontal boiler tube, erects
To the anterior position of boiler tube upper opening, it is then shut off end cap 11 and seals close.
Second step, opens vacuum extractor and boiler tube 1 is vacuumized, after vacuum reaches technological requirement, stop vacuumizing,
Inert gas that inert gas inleting pipe 13 is passed through needed for reaction is begun through to micro-vacuum state.
3rd step, starts to warm up and is heated to required synthesis reaction temperature, starts simultaneously in feed end coolant jacket 61 and discharging
Coolant jacket 62 is held, cooling medium is passed through and boiler tube 1 is cooled down.
4th step, when the temperature of boiler tube 1 reaches the reaction temperature of technological requirement, begins through reacting gas air inlet pipe 12 and leads to
Enter reacting gas, synthetic reaction is proceeded by.
5th step, during the progress of synthetic reaction, opens the observation synthetic reaction situation of body of heater 2, and logical by adjustment
The flow of the reacting gas entered controls reaction process.
6th step, the operation that can be vacuumized during the course of the reaction, so that the sublimation gases that produce of synthetic reaction are to perpendicular
Flowed to boiler tube, when gas passes through discharging opening coolant jacket 62 will crystallisation by cooling, produced crystalline solid drops to receipts naturally
Collect in bottle 15, most synthetic product is collected by receiving flask 15.
Final step, opens the observing response of body of heater 2 synthesis situation, after reactant 5 reacts completely, closes reacting gas and enters
Device of air closes air inlet pipe 12, carries out last time vacuum pumping to boiler tube 1, is then shut off escape pipe 9, and pass through indifferent gas
Body pipe 13, which is passed through after inert gas to micro-vacuum state, to be stopped being passed through, and is closed heating heater and is started cooling, when temperature is down to
During technological requirement temperature, boiler tube 1 is opened, receiving flask 15 is removed, starts to collect synthetic product.
Result of laboratory test shows that the synthetic product purity of gained can reach more than 99.99%, and yield can reach more than 95%.
Described is only preferred embodiment of the present utility model, all in this practicality not to limit the utility model
Any modifications, equivalent substitutions and improvements made within new spirit and principle etc., should be included in guarantor of the present utility model
Within the scope of shield.
Claims (9)
1. a kind of vacuum synthesis stove, it is characterised in that：It includes tube type high-temperature furnace, air-washer, and the tube type high-temperature furnace includes
Body of heater and boiler tube, the inwall of the body of heater are provided with electric heater unit, body of heater be divided into above and below two parts, lower volume right-hand member is provided with
Through the circular hole of body of heater, the boiler tube is perpendicular type bend pipe, is connected as one by horizontal boiler tube with vertical boiler tube, the horizontal stove
Pipe is positioned in body of heater, and between electric heater unit, the vertical boiler tube runs through lower volume by circular hole；The transverse direction
The left end of boiler tube is provided with import sealing flange, import coolant jacket, the horizontal boiler tube and is placed with reaction boat；The vertical stove
The lower end of pipe is provided with outlet coolant jacket, exit seal flange, and the exit seal flange lower end is provided with discharging opening, the discharging
Mouth is closely coupled with receiving flask by sealing ring, and the receiving flask has support；
The import sealing flange is provided with charging aperture, and the charging aperture is provided with end cap, the end cap and is provided with the two of insertion
Individual air inlet and a thermocouple port；
The exit seal flange is provided with gas outlet, and the gas outlet connects and is provided with vacuum on vacuum tube, the vacuum tube
Table and vacuum valve, the vacuum tube connect air-washer, the air-washer and vacuum extractor phase after vacuum valve
Even.
2. a kind of vacuum synthesis stove according to claim 1, it is characterised in that temperature in measurement stove is provided with the boiler tube
The temperature sensor of degree, the temperature sensor is thermocouple, and the thermocouple is wrapped in a quartz ampoule, the thermocouple
Goed deep into by thermocouple port in boiler tube, and below reaction boat.
3. a kind of vacuum synthesis stove according to claim 1, it is characterised in that the air-washer include surge flask, No. 1
Drexel bottle, No. 2 Drexel bottles, No. 1 Drexel bottle and No. 2 Drexel bottles are built with the NaOH solution that concentration is 5 ~ 15%.
4. a kind of vacuum synthesis stove according to claim 1, it is characterised in that the exit seal flange and glove box phase
Even, the receiving flask is located in glove box.
5. a kind of vacuum synthesis stove according to claim 1, it is characterised in that the boiler tube and reaction boat use high temperature resistant
Quartz glass is made, and receiving flask is simple glass bottle.
6. a kind of vacuum synthesis stove according to claim 1, it is characterised in that the import sealing flange, end cap, outlet
Sealing flange and vacuum valve are made using polytetrafluoroethylene (PTFE).
7. a kind of vacuum synthesis stove according to claim 1, it is characterised in that the electric heater unit is that Elema electricity adds
Thermal.
8. a kind of vacuum synthesis stove according to claim 1, it is characterised in that the vacuum meter is stainless steel diaphragm pressure
Table.
9. a kind of vacuum synthesis stove according to claim 1, it is characterised in that also including temperature controller, the temperature
Controller is connected with electric heater unit.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201621388951.1U CN206362178U (en) | 2016-12-18 | 2016-12-18 | A kind of vacuum synthesis stove |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201621388951.1U CN206362178U (en) | 2016-12-18 | 2016-12-18 | A kind of vacuum synthesis stove |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN206362178U true CN206362178U (en) | 2017-07-28 |
Family
ID=59374749
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201621388951.1U Expired - Fee Related CN206362178U (en) | 2016-12-18 | 2016-12-18 | A kind of vacuum synthesis stove |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN206362178U (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106766910A (en) * | 2016-12-18 | 2017-05-31 | 株洲冶炼集团股份有限公司 | High temperature corrosion resistant vacuum synthesis stove and its process |
| CN114480800A (en) * | 2022-01-11 | 2022-05-13 | 武汉理工大学 | Vertical high-temperature reaction quenching furnace for phase diagram determination |
-
2016
- 2016-12-18 CN CN201621388951.1U patent/CN206362178U/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106766910A (en) * | 2016-12-18 | 2017-05-31 | 株洲冶炼集团股份有限公司 | High temperature corrosion resistant vacuum synthesis stove and its process |
| CN114480800A (en) * | 2022-01-11 | 2022-05-13 | 武汉理工大学 | Vertical high-temperature reaction quenching furnace for phase diagram determination |
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| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20170728 |