CN106766910A - High temperature corrosion resistant vacuum synthesis stove and its process - Google Patents
High temperature corrosion resistant vacuum synthesis stove and its process Download PDFInfo
- Publication number
- CN106766910A CN106766910A CN201611173329.3A CN201611173329A CN106766910A CN 106766910 A CN106766910 A CN 106766910A CN 201611173329 A CN201611173329 A CN 201611173329A CN 106766910 A CN106766910 A CN 106766910A
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- Prior art keywords
- boiler tube
- vacuum
- reaction
- tube
- corrosion resistant
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Classifications
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B17/00—Furnaces of a kind not covered by any preceding group
-
- 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
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/006—Processes utilising sub-atmospheric pressure; Apparatus therefor
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D17/00—Arrangements for using waste heat; Arrangements for using, or disposing of, waste gases
- F27D17/008—Arrangements for using waste heat; Arrangements for using, or disposing of, waste gases cleaning gases
Abstract
The present invention provides a kind of high temperature corrosion resistant vacuum synthesis stove and its process, it includes 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 present invention 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 present invention relates to a kind of high temperature corrosion resistant vacuum synthesis stove and its process.Belong 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
Obtained in solution.Wherein anhydrous InCl3Used as 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 produced anhydrous InCl3
Legacy equipment there are problems that small yield, high cost, 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 patent of invention《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, but the device are proposed in one text without equipment of crystallisation by cooling, nothing is washed
Device of air, body of heater cannot be opened when reacting and be unable to observing response situation, it is impossible to for anhydrous InCl3Production.
The content of the invention
Present invention deficiency regarding to the issue above proposes a kind of high temperature corrosion resistant vacuum synthesis stove and its process, can be effective
Carry out heating in vacuum to reactant, the synthetic product of reaction collects convenient, can carry out situation by observing response at any time, can adopt
The mordant poisonous reacting gas of apparatus, and safety and environmental protection.
The present invention is achieved by the following technical programs：
High temperature corrosion resistant 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, and body of heater is divided into upper and lower two parts, and 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 with vertical boiler tube by horizontal boiler tube, and 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
Import sealing flange, import coolant jacket are provided with, reaction boat is placed with the horizontal boiler tube；The lower end of the vertical boiler tube sets
Outlet coolant jacket, exit seal flange are equipped with, the exit seal flange lower end is provided with discharging opening, and the discharging opening is by 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, insertion is provided with the end cap
Two air inlets and a thermocouple port.
The exit seal flange is provided with gas outlet, and the gas outlet connects vacuum tube, is provided with the vacuum tube
Vacuum meter and vacuum valve, the vacuum tube is by connecting 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
Reaction boat lower section.
Further, the air-washer includes surge flask, No. 1 Drexel bottle, No. 2 Drexel bottles, No. 1 Drexel bottle and 2
Number Drexel bottle built with concentration for 5 ~ 15% NaOH solution.
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, also it is connected with the electric heater unit including temperature controller.
A kind of high temperature corrosion resistant vacuum synthesis stove and its process can improve yield, improve synthetic purity, accurate control
Reaction process processed, production process safety and environmental protection, the process are as follows：
Charging aperture end cap is first turned on, the reaction boat of reactant is will be equipped with, the front of the perpendicular end opening in end of horizontal boiler tube is put into
Position, is then shut off end cap and seals tight；Open vacuum extractor to vacuumize boiler tube, technological requirement is reached in vacuum
Afterwards, stop vacuumizing, the inert gas needed for starting to be passed through reaction to micro-vacuum state；Start to warm up synthesis needed for being heated to anti-
Temperature is answered, is started simultaneously at and is passed through cooling medium in feed end coolant jacket and discharge end coolant jacket boiler tube is cooled down；Work as boiler tube
When temperature reaches the reaction temperature of technological requirement, start to be passed through reacting gas, synthetic reaction is proceeded by；In entering for synthetic reaction
During row, open body of heater observation synthetic reaction situation, and control to react by the flow of reacting gas that adjustment is passed through into
Journey；The operation that can be vacuumized during the course of the reaction, so that the sublimation gases that synthetic reaction is produced flow to vertical boiler tube, when
Gas by vertical boiler tube coolant jacket when will crystallisation by cooling, produced crystalline solid dropped in receiving flask naturally, by receiving
Collection bottle collects most synthetic product, opens body of heater observing response synthesis situation, after reactant reacts completely, closes reaction
Air inlet device closes air inlet pipe, and last time vacuum pumping is carried out to boiler tube, is then shut off gas outlet, and by inertia
Flue stops being passed through after being passed through inert gas to micro-vacuum state, closes intensification heater and starts cooling, when temperature is down to
During technological requirement temperature, open boiler tube and remove receiving flask, start to collect synthetic product.
A kind of high temperature corrosion resistant vacuum synthesis stove of the invention and its process, with existing for synthesizing anhydrous chlorine
The device for changing indium is compared, and is had the advantages that：
（1）Boiler tube and reaction boat are all quartz glass, and import sealing flange, exit seal flange, end cap are all polytetrafluoroethylene (PTFE),
Connecting pipe is all polyvinyl chloride, vacuum meter, and valve etc. is all anticorrosive material, has strong corruption when reacting gas is that hydrogen chloride is this
During corrosion gas, it is also ensured that the normal of equipment is used, prevent from corroding the hydrogen chloride leakage for causing, it is ensured that synthetic product
Quality 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, and 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 is divided into upper and lower two parts, and observing response situation can be opened in reaction, controls the process of reaction.
（5）Boiler tube is furnished with cooling device, can accelerate the crystallisation by cooling of anhydrous indium chloride, and 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 synthetic furnace of the present invention.
Fig. 2 is air-washer structural representation of the invention.
In accompanying drawing：1st, boiler tube；2nd, body of heater；3rd, electric heater unit；4 reaction boats；5th, reactant；61st, import coolant jacket；62、
Outlet coolant jacket；71st, silicagel pad；72nd, exit seal circle；73rd, receiving flask sealing ring；8th, vacuum valve；9th, escaping 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, heat
Galvanic couple；15th, receiving flask；16th, glove box；17th, support；18th, vacuum meter；19th, wireway；20th, surge flask；21st, No. 1 Drexel bottle；
22nd, No. 2 Drexel bottles；23rd, NaOH solution.
Specific embodiment
In order that technical problem solved by the invention, technical scheme and beneficial effect become more apparent, below in conjunction with
Drawings and Examples, are described in further detail to the present invention.It should be appreciated that specific embodiment described herein is only
It is used to explain the present invention, is not intended to limit the present invention.
Refer to Fig. 1, the specific embodiment of the invention provides a kind of high temperature corrosion resistant vacuum synthesis stove, including tube type high-temperature furnace,
Glove box 16, air-washer, tube type high-temperature furnace includes body of heater 2 and boiler tube 1, and the inwall of the body of heater 2 is provided with electric heater unit
3.The electric heater unit 3, can use Resistant heating device or Elema heater.The synthetic furnace also includes temperature
Degree controller, 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 with vertical boiler tube by horizontal boiler tube, and the horizontal boiler tube is positioned in body of heater 2, and quilt
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 within transverse direction
The outside of boiler tube, import sealing flange 101 is adopted with the left end of horizontal boiler tube and inlays or be glued or interference fit 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 be provided with charging aperture end cap 11, 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 passes through thermocouple port and is deep into
In boiler tube 1, and it is made using high temperature resistant quartz glass positioned at the lower section of reaction boat 4, the boiler tube 1 and reaction boat 4.
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, exit seal flange 102 adopted with the lower end of vertical boiler tube inlay or be glued or interference fit 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
Support receiving flask 15, 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 connects vacuum tube 9, pacifies on 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 by connecting air-washer after vacuum valve 8, by connecting vacuum extractor 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 wireway 19.
The process of the present embodiment high temperature corrosion resistant vacuum synthesis stove, 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, vertical stove
The anterior position of pipe upper opening, is then shut off end cap 11 and seals tight.
Second step, opens vacuum extractor and boiler tube 1 is vacuumized, and after vacuum reaches technological requirement, stops vacuumizing,
The inert gas needed for inert gas inleting pipe 13 is passed through 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
End coolant jacket 62, is passed through cooling medium 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 carrying out of synthetic reaction, opens the observation synthetic reaction situation of body of heater 2, and logical by adjustment
The flow of the reacting gas for entering controls reaction process.
6th step, the operation that can be vacuumized during the course of the reaction, so that the sublimation gases that synthetic reaction is produced are to perpendicular
Flowed to boiler tube, when gas is by discharging opening coolant jacket 62 will crystallisation by cooling, produced crystalline solid drops to receipts naturally
In collection 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, and last time vacuum pumping is carried out to boiler tube 1, is then shut off escaping pipe 9, and by indifferent gas
Body pipe 13 stops being passed through after being passed through inert gas to micro-vacuum state, closes intensification heater and starts cooling, when temperature is down to
During technological requirement temperature, boiler tube 1 is opened, remove receiving flask 15, start 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%.
It is described be only presently preferred embodiments of the present invention, be not intended to limit the invention, it is all it is of the invention spirit and
Any modification, equivalent and improvement for being made within principle etc., should be included within the scope of the present invention.
Claims (10)
1. high temperature corrosion resistant vacuum synthesis stove, it is characterised in that：It includes tube type high-temperature furnace, air-washer, the tube type high-temperature furnace
Including body of heater and boiler tube, the inwall of the body of heater is provided with electric heater unit, and body of heater is divided into upper and lower two parts, lower volume right-hand member
The circular hole through body of heater is provided with, the boiler tube is perpendicular type bend pipe, is connected as one with vertical boiler tube by horizontal boiler tube, the horizontal stroke
It is positioned in body of heater to boiler tube, and between electric heater unit, the vertical boiler tube runs through lower volume by circular hole；It is described
The left end of horizontal boiler tube is provided with import sealing flange, import coolant jacket, and reaction boat is placed with the horizontal boiler tube；It is described perpendicular
The lower end of boiler tube is provided with outlet coolant jacket, exit seal flange, the exit seal flange lower end is provided with discharging opening, described
Discharging opening 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 two of insertion are provided with the end cap
Individual air inlet and a thermocouple port；
The exit seal flange is provided with gas outlet, and the gas outlet connects vacuum tube, vacuum is provided with the vacuum tube
Table and vacuum valve, the vacuum tube is by connecting air-washer, the air-washer and vacuum extractor phase after vacuum valve
Even.
2. high temperature corrosion resistant vacuum synthesis stove according to claim 1, it is characterised in that measurement stove is provided with the boiler tube
The temperature sensor of interior temperature, the temperature sensor is thermocouple, and the thermocouple is wrapped in a quartz ampoule, the heat
Galvanic couple is goed deep into boiler tube by thermocouple port, and positioned at reaction boat lower section.
3. high temperature corrosion resistant vacuum synthesis stove according to claim 1, it is characterised in that the air-washer includes buffering
Bottle, 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. high temperature corrosion resistant vacuum synthesis stove according to claim 1, it is characterised in that the exit seal flange and gloves
Case is connected, and the receiving flask is located in glove box.
5. high temperature corrosion resistant vacuum synthesis stove according to claim 1, it is characterised in that the boiler tube and reaction boat are using resistance to
High quartz glass is made, and receiving flask is simple glass bottle.
6. high temperature corrosion resistant vacuum synthesis stove according to claim 1, it is characterised in that the import sealing flange, end cap,
Exit seal flange and vacuum valve are made using polytetrafluoroethylene (PTFE).
7. high temperature corrosion resistant vacuum synthesis stove according to claim 1, it is characterised in that the electric heater unit is Elema
Electric heater unit.
8. high temperature corrosion resistant vacuum synthesis stove according to claim 1, it is characterised in that the vacuum meter is stainless steel barrier film
Pressure gauge.
9. high temperature corrosion resistant vacuum synthesis stove according to claim 1, it is characterised in that described also including temperature controller
Temperature controller is connected with electric heater unit.
10. the process of the high temperature corrosion resistant vacuum synthesis stove according to claim any one of 1-8, it is characterised in that press
Following steps are carried out：
（1）Charging aperture end cap is opened, will be equipped with the reaction boat of reactant, be put into the end of horizontal boiler tube, vertical boiler tube opening
Anterior position, is then shut off end cap and seals tight；
（2）Open vacuum extractor to vacuumize boiler tube, after vacuum reaches technological requirement, stop vacuumizing, start to be passed through
Inert gas needed for reaction is to micro-vacuum state；
（3）Start to warm up and be heated to required synthesis reaction temperature, start simultaneously at logical in feed end coolant jacket and discharge end coolant jacket
Enter cooling medium to cool down boiler tube；
（4）When furnace tube temperature reaches the reaction temperature of technological requirement, start to be passed through reacting gas, synthetic reaction is proceeded by；
（5）During the carrying out of synthetic reaction, body of heater observation synthetic reaction situation, and the reaction gas being passed through by adjustment are opened
The flow of body controls reaction process；
（6）The operation that can be vacuumized during the course of the reaction, so that the sublimation gases that synthetic reaction is produced are to vertical boiler tube stream
It is dynamic, when gas is by vertical boiler tube coolant jacket will crystallisation by cooling, produced crystalline solid drops in receiving flask, leads to naturally
Cross receiving flask and collect most synthetic product；
（7）Open body of heater observing response synthesis situation, after reactant reacts completely, close reacting gas inlet duct close into
Tracheae, last time vacuum pumping is carried out to boiler tube, is then shut off gas outlet, and be passed through inert gas by inert gas tube
Stop being passed through after to micro-vacuum state, close intensification heater and start cooling, when temperature is down to technological requirement temperature, open
Boiler tube removes receiving flask, starts to collect synthetic product.
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| CN201611173329.3A CN106766910B (en) | 2016-12-18 | 2016-12-18 | High-temperature corrosion-resistant vacuum synthesis furnace and process method thereof |
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| CN201611173329.3A CN106766910B (en) | 2016-12-18 | 2016-12-18 | High-temperature corrosion-resistant vacuum synthesis furnace and process method thereof |
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| CN106766910A true CN106766910A (en) | 2017-05-31 |
| CN106766910B CN106766910B (en) | 2023-01-10 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107983291A (en) * | 2017-10-28 | 2018-05-04 | 株洲冶炼集团股份有限公司 | A kind of devices and methods therefor for preparing anhydrous gallium chloride |
| CN108217669A (en) * | 2018-01-08 | 2018-06-29 | 北京工业大学 | A kind of gas-solid reaction synthesizes MgB2The method of superconductor |
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| CN106766910B (en) | 2023-01-10 |
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