CN107983291A - A kind of devices and methods therefor for preparing anhydrous gallium chloride - Google Patents
A kind of devices and methods therefor for preparing anhydrous gallium chloride Download PDFInfo
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- CN107983291A CN107983291A CN201711030890.0A CN201711030890A CN107983291A CN 107983291 A CN107983291 A CN 107983291A CN 201711030890 A CN201711030890 A CN 201711030890A CN 107983291 A CN107983291 A CN 107983291A
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- UPWPDUACHOATKO-UHFFFAOYSA-K gallium trichloride Chemical compound Cl[Ga](Cl)Cl UPWPDUACHOATKO-UHFFFAOYSA-K 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 68
- 239000000460 chlorine Substances 0.000 claims abstract description 38
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 38
- 238000002425 crystallisation Methods 0.000 claims abstract description 27
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 19
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 61
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 41
- 239000010453 quartz Substances 0.000 claims description 40
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 37
- 229910052757 nitrogen Inorganic materials 0.000 claims description 31
- 239000007789 gas Substances 0.000 claims description 25
- 230000008025 crystallization Effects 0.000 claims description 22
- 239000007788 liquid Substances 0.000 claims description 20
- 230000004044 response Effects 0.000 claims description 15
- 238000010521 absorption reaction Methods 0.000 claims description 13
- 241001411320 Eriogonum inflatum Species 0.000 claims description 7
- 230000001681 protective effect Effects 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 238000005070 sampling Methods 0.000 claims description 4
- 238000000605 extraction Methods 0.000 claims description 3
- -1 reaction tube Chemical compound 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 3
- 239000012535 impurity Substances 0.000 abstract description 2
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 3
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000036632 reaction speed Effects 0.000 description 2
- 239000002341 toxic gas Substances 0.000 description 2
- 229910005267 GaCl3 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- 238000004442 gravimetric analysis Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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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
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/2415—Tubular reactors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/002—Avoiding undesirable reactions or side-effects, e.g. avoiding explosions, or improving the yield by suppressing side-reactions
-
- 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
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
-
- 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
- B01J4/008—Feed or outlet control devices
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G15/00—Compounds of gallium, indium or thallium
-
- 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
- B01J2204/00—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
- B01J2204/002—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices the feeding side being of particular interest
-
- 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
- B01J2204/00—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
- B01J2204/005—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices the outlet side being of particular interest
-
- 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
- B01J2204/00—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
- B01J2204/007—Aspects relating to the heat-exchange of the feed or outlet devices
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
- B01J2219/00094—Jackets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00162—Controlling or regulating processes controlling the pressure
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00245—Avoiding undesirable reactions or side-effects
- B01J2219/00252—Formation of deposits other than coke
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The present invention provides a kind of device for preparing anhydrous gallium chloride, including reaction tube, heating mantle, temperature control device, vacuum plant, collection device and exhaust gas processing device.Gallium is placed in the bottom of reaction tube, and air inlet pipe is connected with pressure gauge and vacuum plant, and the air outlet pipe of reaction tube is enclosed with muff, and connects collection device and exhaust gas processing device.Chlorine is dried by drying equipment, is then passed to reaction tube and is reacted with gallium, and the gas after reaction enters collection device and carries out crystallisation by cooling collection, and tail gas is discharged after treatment.The present apparatus have the advantages that rational technology, be easy to collect, the introducing of impurity easy to control, pollution-free, product purity is high.
Description
Technical field
The invention belongs to compound synthesis apparatus field, and in particular to a kind of device for preparing anhydrous gallium chloride.
Background technology
Anhydrous gallium trichloride, molecular formula：GaCl3, white, needle-shaped crystals, 2 .47g/cm3 of density (25 DEG C).Fusing point 78
DEG C, 201 .3 DEG C of boiling point.Easy deliquescence, oxidizable, soluble easily in water in atmosphere.It is extremely dry at one to prepare anhydrous gallium trichloride needs
It is dry, completely cut off air and have and carry out under conditions of inert protective gas.
Prepare the common method of anhydrous gallium trichloride：Dry hydrogen chloride gas or chlorine are passed through the stone equipped with gallium
Ying Guan, after air discharge in pipe, temperature is delayed and rises to 200 DEG C and makes its reaction.After the completion of question response, begin to cool down and lead to
Enter inert gas to discharge hydrogen chloride gas.The product of distillation is sealed from reaction tube, and with general gravimetric analysis chlorine
With the content of gallium, the amount according to gallium used calculates yield.
The prior art is disadvantageous in that, is passed through hydrogen chloride gas or chlorine and is reacted with gallium surface, reaction speed is slow,
Efficiency is low, and the utilization rate of gas is low, and discharge gas has certain toxicity；Easily crystallisation by cooling blocks up during the collection of gaseous state gallium trichloride
Fill in collection conduit.
The content of the invention
In order to overcome the existing appeal shortcoming for preparing anhydrous gallium chloride, the present invention provides one kind to prepare anhydrous gallium chloride
Device, have rational technology, reaction fully, be easy to collection, be the introducing of impurity easy to control, low manufacture cost, pollution-free, nontoxic
Evil, the advantages that yield and product purity are high.
Technical solution is as follows used by the present invention solves above-mentioned technical problem：
A kind of device for preparing anhydrous gallium chloride, including reaction tube, pressure gauge, nitrogen tube valve, nitrogen tube, chlorine tube valve,
Vacuum tube valves, quartz cover, air inlet pipe, air outlet pipe, crystallization receiving flask, the first connecting tube, collection liquid bottle, collection liquid, second connect
Adapter, absorption bottle and tail gas absorption liquid, the right end of the reaction tube are equipped with quartz cover, air inlet pipe, and the left end of the air inlet pipe is worn
Quartz cover is crossed to extend into reaction tube and close to reaction bottom of the tube, the right end of the air inlet pipe respectively with nitrogen tube, chlorine tube, true
Blank pipe is connected, and the air inlet pipe, nitrogen tube, chlorine tube, be respectively equipped with air inlet pipe valve, nitrogen tube valve, chlorine on vacuum tube
Tube valve, vacuum tube valves, are additionally provided with pressure gauge in the air inlet pipe；The left end of the reaction tube is connected with air outlet pipe, described
Air outlet pipe is extend into crystallization receiving flask, and the crystallization receiving flask is connected with one end of the first connecting tube, first connecting tube
The other end extend into the collection liquid of collection liquid bottle.The collection liquid bottle top is connected with one end of the second connecting tube, described
The other end of second connecting tube is extend into the tail gas absorption liquid of absorption bottle.
Further, the outside of reaction tube is enclosed with muff, and the heating mantle is equipped with thermometric bar, the thermometric bar with
Temperature control device connects；The outside of the air outlet pipe is uniformly enclosed with muff, prevents the gallium chloride that reaction produces in air outlet pipe
Crystallisation by cooling blocks air outlet pipe.
Further, the quartz cover is with reaction tube using being tightly connected, and the quartz cover is linked up with equipped with quartz cover, institute
State reaction tube to link up with equipped with inlet end, the quartz cover hook is connected by fixed coil with inlet end hook, makes quartz cover
It is close with the reaction seal of tube.
Further, described device further includes glove box, is full of inert protective gas, the air outlet pipe in the glove box
Left end portion, crystallization receiving flask, the right end portion of the first connecting tube be respectively positioned in glove box, after gallium crystallization completely to be chlorinated,
Bottle stopper is opened by glove box and is collected sampling.
Further, the air inlet pipe, nitrogen tube, chlorine tube, vacuum tube are orthogonal connects or is connected by four-way valve,
The vacuum tube is connected with exterior vacuum equipment.
A kind of method for preparing anhydrous gallium chloride, comprises the following steps：
The first step：Open right side quartz cover, it would be desirable to the metal derby gallium reacted is placed in reaction tube, covers quartz cover,
Linked up with fixed coil connection quartz cover hook and inlet end, make quartz cover and the reaction seal of tube close；
Second step：Vacuum tube valves are opened, air inlet pipe valve, opens vacuum equipment and reaction tube and crystallization receiving flask take out very
Do-nothing operation, passes through the vacuum condition of pressure gauge observing response pipe；
3rd step：After air extraction in question response pipe, vacuum valve is closed, chlorine tube valve is opened, chlorine is passed through to reaction tube
Gas, while connection tube valve is opened, and beginning to warm up carries out reaction；
4th step：After gallium reaction completely in question response pipe, chlorine tube valve is closed, nitrogen tube valve is opened, into reaction tube
Nitrogen is passed through, after question response pipe and the chlorine crystallized in receiving flask are completely exhausted out, nitrogen tube valve are closed and simultaneously closes air inlet pipe valve
Door, simultaneously closes off connection tube valve；
5th step：Inert protective gas is filled with into glove box, after gallium crystallization completely to be chlorinated, opening bottle stopper, which is collected, to be taken
Sample.
The present invention has the advantages that：
（1）Equipped with pressure vacuum meter can at any time in observing response pipe pressure situation.Vacuum pumping can be fully drawn out instead
Should manage can control reaction speed and ensure the steady progress of reaction with the gas in receiving flask, control pressure.
（2）Air inlet pipe stretches into reaction tube and close to reaction bottom of the tube.It can ensure the chlorine that is passed through completely and gallium
Reacted.
（3）The air outlet pipe of reaction tube is enclosed with muff.It can prevent the gallium chloride that reaction produces from being cooled down in air outlet pipe
Crystallization Plugging air outlet pipe.
（4）Air outlet pipe is connected with collection device, and crystallized product is collected convenient.
（5）Air outlet pipe has device for absorbing tail gas, for absorbing the toxic gases such as chlorine.Safe preparation process environmental protection.
Brief description of the drawings
Fig. 1 is the reaction unit structure diagram of the present invention.
Fig. 2 is the collection device and exhaust gas processing device structure diagram of the present invention.
Reference numeral in attached drawing is as follows：1st, reaction tube；2nd, inlet end is linked up with；3rd, fixed coil；4th, quartz cover is linked up with；5、
Pressure gauge；6th, nitrogen tube valve；7th, nitrogen tube；8th, chlorine tube valve；9th, chlorine tube；10th, vacuum tube valves；11st, vacuum tube；
12nd, air inlet pipe valve；13rd, quartz cover；14th, air inlet pipe；15th, heating mantle；16th, outlet side is linked up with；17th, air outlet pipe；18th, thermometric fills
Put；19th, thermometric bar；20th, metal derby；21st, muff；22nd, bottle stopper；23rd, connection tube valve；24th, the first connecting tube；25th, collect
Liquid bottle；26th, the second connecting tube；27th, exhaust pipe；28th, absorption bottle；29th, tail gas absorption liquid；30th, collection liquid；31st, receiving flask is crystallized；
32nd, glove box.
Embodiment
In order to which technical problem, technical solution and beneficial effect solved by the invention is more clearly understood, below in conjunction with
Accompanying drawings and embodiments, are described in further detail the present invention.It should be appreciated that specific embodiment described herein is only
To explain the present invention, it is not intended to limit the present invention.
Fig. 1, Fig. 2 are refer to, the embodiment provides a kind of device for preparing anhydrous gallium chloride, including reaction tube
1st, pressure gauge 5, nitrogen tube valve 6, nitrogen tube 7, chlorine tube valve 8, vacuum tube valves 10, quartz cover 13, air inlet pipe 14, outlet
Pipe 17, temperature control device 18, collection device and exhaust gas processing device.
The reaction tube 1 uses high temperature resistant quartz glass tube, is hardly damaged, reacting phenomenon is easy to observe, and gallium 20 is put
In the bottom of reaction tube 1.The outside of reaction tube 1 is enclosed with muff 15, and the heating mantle 15 is equipped with thermometric bar 19, the survey
Warm bar 19 is connected with temperature control device 18.The right end of reaction tube 1 is equipped with quartz cover 13 and air inlet pipe 14, the left end of the air inlet pipe 14
Extend into through quartz cover 13 in reaction tube 1 and close to 1 bottom of reaction tube, the right end of the air inlet pipe 14 respectively with nitrogen tube 7,
Chlorine tube 9, vacuum tube 11 are connected, and the air inlet pipe 14, nitrogen tube 7, chlorine tube 9, be respectively equipped with air inlet pipe valve on vacuum tube 11
Door 12, nitrogen tube valve 6, chlorine tube valve 8, vacuum tube valves 10, are additionally provided with pressure gauge 5 in the air inlet pipe 14.
The orthogonal connection of the air inlet pipe 14, nitrogen tube 7, chlorine tube 9, vacuum tube 11 is mutually connected by four-way valve
Logical, the vacuum tube 11 is connected with exterior vacuum equipment, and the nitrogen tube 7 is connected with exterior nitrogen cylinder, the chlorine tube 9
It is connected with exterior chlorine cylinder.When opening vacuum equipment, vacuum pumping can be carried out to reaction tube 1 and crystallization receiving flask 31,
Pass through the vacuum condition of 5 observing response pipe 1 of pressure gauge.
The left end of reaction tube 1 is connected with air outlet pipe 17, and the air outlet pipe 17 is connected with collection device, exhaust gas processing device,
For absorbing the toxic gases such as chlorine.Air outlet pipe 17 is extend into crystallization receiving flask 31, and the crystallization receiving flask 31 and first connects
One end of adapter 24 is connected, and the other end of first connecting tube 24 is extend into the collection liquid 30 of collection liquid bottle 25.The receipts
25 top of liquid-collecting bottle is connected with one end of the second connecting tube 26, and the other end of second connecting tube 26 extend into absorption bottle 28
In tail gas absorption liquid 29, exhaust pipe 27 is additionally provided with the absorption bottle 28.The outside of the air outlet pipe 17 is uniformly enclosed with insulation
Set 21, to prevent the gallium chloride of reaction generation crystallisation by cooling in air outlet pipe from blocking outlet.
Reaction tube 1 is sealed with quartz cover 13 using ground, and the quartz of quartz material is welded with the quartz cover 13
Lid links up with 4, and the inlet end hook 2 of quartz material is welded with the reaction tube 1, and the quartz cover hook 4 passes through fixation
Coil 3 is connected with inlet end hook 2, quartz cover 13 is sealed closely with reaction tube 1.Reaction tube can so born stronger
Pressure.
A kind of device for preparing anhydrous gallium chloride of the present invention, further includes glove box 32, is full of inertia in the glove box 32
Protective gas, left end portion, crystallization receiving flask 31, the right end portion of the first connecting tube 24 of the air outlet pipe 17 are respectively positioned on gloves
In case 32, after gallium crystallization completely to be chlorinated, bottle stopper 22 can be opened by glove box 32 and be collected sampling.
A kind of method for preparing anhydrous gallium chloride, comprises the following steps：
The first step：Open right side quartz cover 13, it would be desirable to which the metal derby 20 reacted is placed in reaction tube 1, covers quartz
Lid 13, connects quartz cover hook 4 and inlet end hook 2 with fixed coil 3, quartz cover 13 is sealed closely with reaction tube 1.
Second step：Vacuum tube valves 10 are opened, air inlet pipe valve 12, opens vacuum equipment and reaction tube 1 and crystallization are collected
Bottle 31 carries out vacuum pumping, passes through the vacuum condition of 5 observing response pipe 1 of pressure gauge.
3rd step：After air extraction in question response pipe 1, vacuum valve 10 is closed, chlorine tube valve 8 is opened, to reaction
Pipe 1 is passed through chlorine, while opens connection tube valve 23, and beginning to warm up carries out reaction.
4th step：After the reaction completely of gallium in question response pipe 1, chlorine tube valve 8 is closed, opens nitrogen tube valve 6, to anti-
Nitrogen should be passed through in pipe 1, after question response pipe 1 and the chlorine crystallized in receiving flask 31 are completely exhausted out, close nitrogen tube valve 6 and simultaneously close
Air inlet pipe valve 12 is closed, simultaneously closes off connection tube valve 23.
Final step：Be filled with inert protective gas into glove box 32, after gallium crystallization completely to be chlorinated, open bottle stopper 22 into
Row collecting and sampling.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement made within refreshing and principle etc., should all be included in the protection scope of the present invention.
Claims (6)
- A kind of 1. device for preparing anhydrous gallium chloride, it is characterised in that：Including reaction tube, pressure gauge, nitrogen tube valve, nitrogen Pipe, chlorine tube valve, vacuum tube valves, quartz cover, air inlet pipe, air outlet pipe, crystallization receiving flask, the first connecting tube, collection liquid bottle, Collection liquid, the second connecting tube, absorption bottle and tail gas absorption liquid, the right end of the reaction tube are equipped with quartz cover, air inlet pipe, it is described into The left end of tracheae extend into reaction tube through quartz cover and close to reaction bottom of the tube, the right end of the air inlet pipe respectively with nitrogen Pipe, chlorine tube, vacuum tube are connected, and the air inlet pipe, nitrogen tube, chlorine tube, be respectively equipped with air inlet pipe valve, nitrogen on vacuum tube Tube valve, chlorine tube valve, vacuum tube valves, are additionally provided with pressure gauge in the air inlet pipe；The left end and outlet of the reaction tube Pipe is connected, and the air outlet pipe is extend into crystallization receiving flask, and the crystallization receiving flask is connected with one end of the first connecting tube, described The other end of first connecting tube is extend into the collection liquid of collection liquid bottle, the collection liquid bottle top and one end of the second connecting tube It is connected, the other end of second connecting tube is extend into the tail gas absorption liquid of absorption bottle.
- A kind of 2. device for preparing anhydrous gallium chloride according to claim 1, it is characterised in that：The exterior parcel of reaction tube There is muff, the heating mantle is equipped with thermometric bar, and the thermometric bar is connected with temperature control device；The outside of the air outlet pipe is uniform Muff is enclosed with, prevents that reacting the gallium chloride produced crystallisation by cooling in air outlet pipe blocks air outlet pipe.
- A kind of 3. device for preparing anhydrous gallium chloride according to claim 1, it is characterised in that：The quartz cover and reaction Pipe using being tightly connected, equipped with quartz cover link up with by the quartz cover, and the reaction tube is linked up with equipped with inlet end, the quartz Lid hook is connected by fixed coil with inlet end hook, makes quartz cover and the reaction seal of tube close.
- A kind of 4. device for preparing anhydrous gallium chloride according to claim 1, it is characterised in that：Described device further includes hand Casing, inert protective gas, left end portion, crystallization receiving flask, the first connecting tube of the air outlet pipe are full of in the glove box Right end portion be respectively positioned in glove box, after gallium to be chlorinated crystallization completely, bottle stopper is opened by glove box and is collected sampling.
- A kind of 5. device for preparing anhydrous gallium chloride according to claim 1, it is characterised in that：The air inlet pipe, nitrogen The orthogonal connection of pipe, chlorine tube, vacuum tube is connected by four-way valve, and the vacuum tube is connected with exterior vacuum equipment.
- A kind of 6. method for preparing anhydrous gallium chloride, it is characterised in that it comprises the following steps：The first step：Open right side quartz cover, it would be desirable to the metal derby gallium reacted is placed in reaction tube, covers quartz cover, Linked up with fixed coil connection quartz cover hook and inlet end, make quartz cover and the reaction seal of tube close；Second step：Vacuum tube valves are opened, air inlet pipe valve, opens vacuum equipment and reaction tube and crystallization receiving flask take out very Do-nothing operation, passes through the vacuum condition of pressure gauge observing response pipe；3rd step：After air extraction in question response pipe, vacuum valve is closed, chlorine tube valve is opened, chlorine is passed through to reaction tube Gas, while connection tube valve is opened, and beginning to warm up carries out reaction；4th step：After gallium reaction completely in question response pipe, chlorine tube valve is closed, nitrogen tube valve is opened, into reaction tube Nitrogen is passed through, after question response pipe and the chlorine crystallized in receiving flask are completely exhausted out, nitrogen tube valve are closed and simultaneously closes air inlet pipe valve Door, simultaneously closes off connection tube valve；5th step：Inert protective gas is filled with into glove box, after gallium crystallization completely to be chlorinated, opening bottle stopper, which is collected, to be taken Sample.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711030890.0A CN107983291A (en) | 2017-10-28 | 2017-10-28 | A kind of devices and methods therefor for preparing anhydrous gallium chloride |
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| CN201711030890.0A CN107983291A (en) | 2017-10-28 | 2017-10-28 | A kind of devices and methods therefor for preparing anhydrous gallium chloride |
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| CN107983291A true CN107983291A (en) | 2018-05-04 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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