CN115385374A - Preparation device and preparation method of gallium trichloride - Google Patents
Preparation device and preparation method of gallium trichloride Download PDFInfo
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- CN115385374A CN115385374A CN202211035391.1A CN202211035391A CN115385374A CN 115385374 A CN115385374 A CN 115385374A CN 202211035391 A CN202211035391 A CN 202211035391A CN 115385374 A CN115385374 A CN 115385374A
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- UPWPDUACHOATKO-UHFFFAOYSA-K gallium trichloride Chemical compound Cl[Ga](Cl)Cl UPWPDUACHOATKO-UHFFFAOYSA-K 0.000 title claims abstract description 214
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 239000007789 gas Substances 0.000 claims abstract description 259
- 238000006243 chemical reaction Methods 0.000 claims abstract description 153
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 102
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims abstract description 102
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims abstract description 102
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 100
- 239000010453 quartz Substances 0.000 claims abstract description 98
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 37
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims description 24
- 238000004519 manufacturing process Methods 0.000 claims description 15
- 239000000126 substance Substances 0.000 claims description 15
- 239000011261 inert gas Substances 0.000 claims description 13
- 239000007787 solid Substances 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 6
- 238000011049 filling Methods 0.000 claims description 4
- 230000008901 benefit Effects 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 230000036632 reaction speed Effects 0.000 abstract description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 76
- 229910052786 argon Inorganic materials 0.000 description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 17
- 229910001868 water Inorganic materials 0.000 description 17
- 230000001681 protective effect Effects 0.000 description 16
- 238000010438 heat treatment Methods 0.000 description 15
- 239000007788 liquid Substances 0.000 description 14
- 239000013078 crystal Substances 0.000 description 12
- 229920001971 elastomer Polymers 0.000 description 12
- 239000005060 rubber Substances 0.000 description 12
- 229910052751 metal Inorganic materials 0.000 description 9
- 239000002184 metal Substances 0.000 description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 8
- 239000002253 acid Substances 0.000 description 5
- 230000009467 reduction Effects 0.000 description 5
- 238000005070 sampling Methods 0.000 description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 239000003513 alkali Substances 0.000 description 4
- 229910001338 liquidmetal Inorganic materials 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- 230000002194 synthesizing effect Effects 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000012494 Quartz wool Substances 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 125000004122 cyclic group Chemical group 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000012495 reaction gas Substances 0.000 description 2
- 230000011218 segmentation Effects 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 229910002601 GaN Inorganic materials 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 1
- 229920001774 Perfluoroether Polymers 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- -1 alkyl gallium compounds Chemical class 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000005388 borosilicate glass Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- XOYLJNJLGBYDTH-UHFFFAOYSA-M chlorogallium Chemical compound [Ga]Cl XOYLJNJLGBYDTH-UHFFFAOYSA-M 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000011978 dissolution method Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 239000010881 fly ash Substances 0.000 description 1
- 150000002258 gallium Chemical class 0.000 description 1
- 229910001195 gallium oxide Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 238000006053 organic reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
Images
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
Abstract
The invention provides a preparation device and a preparation method of gallium trichloride. The device comprises a raw material supply unit, a quartz reaction unit and a gallium trichloride collecting unit. Wherein the raw material supply unit comprises a hydrogen chloride supply device. The quartz reaction unit is connected with the hydrogen chloride supply device through a feed pipeline, the quartz reaction unit comprises a gas distributor and a reaction tank, and the gallium trichloride collecting unit comprises a plurality of gallium trichloride traps which are connected in series and connected with the quartz reaction unit through a gas output pipeline. The purity of the gallium trichloride product prepared by taking high-purity gallium (4N grade) and hydrogen chloride as raw materials through the device reaches 99.9 percent, and the device has the advantages of high reaction speed, high synthesis efficiency and the like.
Description
Technical Field
The invention relates to the technical field of inorganic chemical synthesis, in particular to a preparation device and a preparation method of gallium trichloride.
Background
Gallium trichloride of the formula GaCl 3 The melting point is 78 ℃, the boiling point is 201.3 ℃, the compound is a white acicular crystal compound which is easy to deliquesce, oxidize and dissolve in water, and the compound is hydrolyzed when meeting moisture in the air to generate gallium oxide hydrate and hydrogen chloride gas. It is an important gallium salt derivative, and is one of important raw materials for synthesizing organic gallium such as alkyl gallium compounds, gallium nitride and gallium arsenide. The catalyst can be used as a catalyst in organic reaction, can also be used as a spectral analysis reagent, and has wide application.
At present, the existing method for preparing gallium trichloride is to react gallium with dry chlorine or hydrogen chloride gas at high temperature, sublimate and cool to obtain white gallium trichloride crystals; however, the disadvantages are that the hydrogen chloride gas has high purity and extremely low water content, and the method has low utilization rate of the hydrogen chloride gas and certain toxicity. According to the invention, by utilizing the device system for rapidly preparing the gallium trichloride, the problem of drying the hydrogen chloride gas can be effectively solved, and the utilization rate of the hydrogen chloride can be remarkably improved by the gas distributor in the quartz reaction unit; and the pure water absorbs the hydrogen chloride and converts the hydrogen chloride into dilute acid, and the dilute acid can return to the dissolution process in the process system for extracting the alumina from the fly ash by the one-step acid dissolution method again, so that the utilization rate of the hydrogen chloride gas is improved again.
Disclosure of Invention
The invention mainly aims to provide a preparation device and a preparation method of gallium trichloride, and aims to solve the problems that hydrogen chloride gas is easy to absorb water in a pipeline and has low utilization rate, and gallium trichloride has low production efficiency and high cost in the prior art.
In order to achieve the above object, according to one aspect of the present invention, there is provided an apparatus for preparing gallium chloride, the apparatus including a raw material supply unit including a hydrogen chloride supply device; the quartz reaction unit is connected with the hydrogen chloride supply device through a feed pipeline and comprises a gas distributor and a reaction tank; the gallium trichloride collecting unit comprises a plurality of gallium trichloride traps which are connected in series and connected with the quartz reaction unit through a gas output pipeline.
Preferably, the device further comprises a temperature control unit, wherein the temperature control unit controls the temperature of the at least one gallium trichloride trap and the gas output pipeline.
Preferably, the apparatus further comprises a temperature control device for controlling the temperature of the quartz reaction unit, and the temperature control device and the temperature control unit are independent from each other.
Preferably, the device also comprises a tail gas capturing unit and an inert gas supply unit, wherein the tail gas capturing unit is connected with the gallium trichloride collecting unit through a gas output pipeline, and the inert gas supply unit is connected with the quartz reaction unit through an inert gas supply pipeline.
Preferably, in the above apparatus, the reaction tank is a ring-shaped through-flow reaction tank.
According to another aspect of the present invention, there is provided a method for preparing gallium trichloride, which is carried out by using the above apparatus, the method comprising: step S1, filling a gallium simple substance into a reaction tank, then introducing hydrogen chloride gas into a quartz reaction unit, and dispersing the hydrogen chloride gas in the quartz reaction unit through a gas distributor; s2, reacting the gallium simple substance with hydrogen chloride gas in a quartz reaction unit at the reaction temperature of 210-500 ℃ to obtain a gas mixture of gallium trichloride and hydrogen chloride; and S3, enabling the gas mixture to sequentially enter a plurality of gallium trichloride traps which are connected in series through gas output pipelines to obtain gallium trichloride crystalline solids.
Preferably, in the above method, the temperature of at least one of the gallium trichloride trap and the gas output line is between 65 ℃ and 200 ℃.
Preferably, in the above method, the reaction temperature is 210 to 400 ℃ in step S2.
Preferably, the method further comprises a step S4 of enabling the tail gas hydrogen chloride gas released from the gallium trichloride collecting unit to enter a tail gas capturing unit, wherein the temperature of the tail gas capturing unit is 5-30 ℃.
Preferably, the method further comprises a step S0 of introducing an inert gas into the quartz reaction unit.
By applying the technical scheme of the invention, the gas distributor and the further annular through reaction tank are arranged in the quartz reaction unit, and the temperature of the quartz reaction unit and the temperature of the temperature control unit are accurately controlled, so that the utilization rate of hydrogen chloride gas and the production efficiency of gallium trichloride are effectively improved; the synthesis method remarkably reduces the cost of synthesizing the gallium trichloride by cooling, liquefying, desublimation, crystallizing, separating the gallium trichloride, packaging and storing. The purity of the gallium trichloride product prepared by taking high-purity gallium (4N grade) and hydrogen chloride as raw materials through the device reaches 99.9 percent, and the device has the advantages of high reaction speed, high synthesis efficiency and the like.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
fig. 1 shows a schematic view of a production apparatus of gallium trichloride according to the present invention.
Wherein the figures include the following reference numerals:
1: temperature control unit, 2: quartz reaction unit, 3: temperature control device, 4-tail gas trapping unit, 5-1, 5-2, 5-3: a gallium trichloride trap, 6-1: gas distributor, 6-2: annular middle-through reaction tank, 7-1, 7-2: a plugging rubber plug, 8-1, 8-2, 8-3: an inlet of the gallium trichloride trap is a long quartz tube, 9-1, 9-2 and 9-3: the outlet of the gallium trichloride catcher is a short quartz tube, and the gas cylinder is No. 1: argon, gas cylinder No. 2: hydrogen chloride.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail below with reference to the accompanying drawings in conjunction with embodiments.
As analyzed by the background art, the existing method for preparing gallium trichloride requires high purity of hydrogen chloride gas and extremely low water content, so that the hydrogen chloride gas is easy to absorb water in a pipeline and has low utilization rate by using the existing method, and further the problems of low production efficiency and high cost of gallium trichloride are caused. In order to solve the problem, the invention provides a device and a method for preparing gallium trichloride.
In a typical embodiment of the present invention, an apparatus for preparing gallium trichloride is provided, the apparatus comprising a raw material supply unit, a quartz reaction unit and a gallium trichloride collecting unit, wherein the raw material supply unit comprises a hydrogen chloride supply device, the quartz reaction unit is connected to the hydrogen chloride supply device through a supply pipeline, the quartz reaction unit comprises a gas distributor and a reaction tank, and the gallium trichloride collecting unit comprises a plurality of gallium trichloride traps arranged in series and is connected to the quartz reaction unit through a gas output pipeline.
By applying the device, the gas distributor is arranged in the quartz reaction unit, so that the hydrogen chloride gas is uniformly dispersed by the gas distributor, and is fully contacted with the gallium simple substance in the quartz reaction unit, and the reaction can be rapidly and completely carried out, thereby improving the utilization rate of the hydrogen chloride gas and the production efficiency of gallium trichloride, and reducing the production cost of the gallium trichloride.
Further, the quartz reaction unit comprises a gas distributor at the bottom end portion, more preferably, the gas distributor is made of a porous quartz wool gas permeable sheet. By arranging the gas distributor in this way, the hydrogen chloride gas can be distributed more evenly in the quartz reaction cell before being contacted with the elemental gallium.
Further, the gallium trichloride trap is an impact type gas sampling bottle, and preferably, the impact type gas sampling bottle is made of borosilicate glass. Gallium trichloride traps include, but are not limited to, those skilled in the art can select a suitable gallium trichloride trap as desired.
Further, from the economical and easily available aspect, the gas output line is a high temperature resistant and corrosion resistant plastic tube, and preferably, the material of the plastic tube is perfluoroalkoxy vinyl ether copolymer.
Furthermore, the device also comprises a temperature control unit, wherein the temperature control unit controls the temperature of at least one gallium trichloride trap and the gas output pipeline. The temperature of the temperature control unit is controlled to convert water molecules into gaseous state, so that the solubility of hydrogen chloride in water can be reduced. Preferably, at least one of the gallium trichloride trap and the quartz reaction unit are located in the temperature control unit, so that the temperature of the gallium trichloride trap and the temperature of the gas output pipeline can be controlled simultaneously by the temperature control unit. As shown in figure 1, the device comprises three gallium trichloride traps 5-1, 5-2 and 5-3 which are connected in series, wherein the gallium trichloride traps 5-1 and 5-2 are positioned in a temperature control unit, and the gallium trichloride trap 5-3 is positioned outside the temperature control unit. In the arrangement, the temperature of the temperature control unit is adjusted to be lower than the liquefaction temperature of the generated gallium trichloride gas by 203 ℃, so that the gallium trichloride can be collected in the gallium trichloride traps 5-1 and 5-2 in a liquid form, and in the gallium trichloride trap 5-3, the temperature of the gallium trichloride gas is instantly reduced to the room temperature, and the temperature is lower than the melting point of the gallium trichloride, so that the gallium trichloride gas can be cooled and crystallized at the bottom of the gallium trichloride trap 5-3 to form a solid gallium trichloride crystal.
Further, in order to better control the temperature of the quartz reaction unit, the device of the invention also comprises a temperature control device for controlling the temperature of the quartz reaction unit, and the temperature control device and the temperature control unit are independent from each other. Because the temperature control device and the temperature control unit of the quartz reaction unit are independent of each other, the temperature of the quartz reaction unit can be controlled to be a temperature suitable for the reaction of the gallium simple substance and the hydrogen chloride gas, for example, 320-400 ℃ through the temperature control device, and the temperature of the temperature control unit is set to be lower than the liquefaction temperature of the gallium trichloride gas by 203 ℃, for example, 110-180 ℃, so that the gallium trichloride exists in a gas form in the quartz reaction unit, and the gallium trichloride is collected in a liquid form in the gallium trichloride trap positioned in the temperature control unit.
Furthermore, from the viewpoint of environmental protection and economy, the device also comprises an exhaust gas capturing unit, and the exhaust gas capturing unit is connected with the gallium trichloride collecting unit. The tail gas trapping unit is used for trapping unreacted hydrogen chloride gas, so that the cyclic utilization of the hydrogen chloride gas can be realized, the utilization rate of the hydrogen chloride gas and the production efficiency of gallium trichloride are further improved, and the production cost of the gallium trichloride is reduced. Preferably, the tail gas capturing unit is arranged outside the temperature control unit, and preferably, the tail gas capturing unit is arranged at room temperature, and as the tail gas is mainly hydrogen chloride, the hydrogen chloride has higher solubility at room temperature, and the absorption effect is better.
In addition, in order to remove air from the entire reaction system before the reaction is carried out in the quartz reaction unit, the apparatus of the present invention further comprises an inert gas supply unit connected to the quartz reaction unit through an inert gas supply line. Before the experiment, a main valve of the argon steel cylinder is opened, and further the flow rate of argon is adjusted through an adjusting valve, so that air in the connecting pipeline is exhausted. Then the argon gas cylinder is closed, the valve of the hydrogen chloride gas cylinder is opened, and the flow rate of the hydrogen chloride is adjusted.
Further, in the device of the present invention, the reaction tank is an annular through reaction tank. The annular middle through reaction tank is utilized, so that the liquid gallium is distributed more uniformly, and the hydrogen chloride is contacted with the liquid gallium more fully. Preferably, the quartz reaction unit comprises a reaction tank near the middle part for filling metal gallium simple substance. More preferably, the quartz reaction unit is fixed by the protruding positions around the reaction groove; preferably, the reaction tank is made of quartz.
In one embodiment, as shown in FIG. 1, the apparatus for preparing gallium trichloride comprises a temperature control unit 1, a quartz reaction unit 2, gallium trichloride traps 5-1, 5-2, 5-3 and a tail gas trap unit 4. Wherein, the upper and lower ends of the quartz reaction unit 2 are plugged, and the plugging material is silica gel, rubber, phenolic resin and other materials, preferably rubber; the top rubber plug and the bottom rubber plug both comprise quartz glass conduits, which are convenient for gas to enter, circulate andconveying the product; the quartz reaction unit 2 is used for enabling the hydrogen chloride gas of the reaction gas to react with the metal gallium contained in the preheating reaction tank; the bottom end of the quartz reaction unit 2 is provided with a reaction gas hydrogen chloride pipeline inlet and a protective gas Ar 2 A tracheal line inlet; the top end of the quartz reaction unit 2 is provided with a mixed gas outlet, the mixed gas outlet sequentially enters the gallium trichloride traps 5-1, 5-2 and 5-3 along a gas output pipeline such as a guide pipe, and the tail gas enters the tail gas trapping unit 4, wherein the gallium trichloride traps 5-1 and 5-2 are positioned inside the temperature control unit 1, the gallium trichloride trap 5-3 and the tail gas trapping unit 4 are positioned outside the temperature control unit, and the outside of the temperature control unit is at room temperature such as 5-30 ℃. The quartz reaction unit 2 is externally provided with a heating jacket and a temperature control device 3, the heat insulation material is quartz wool and the like, and the temperature control device is used for realizing accurate temperature control and controlling the reaction temperature of the reaction tank of the quartz reaction unit. The temperature control unit 1 is provided with an independent heating and temperature control system; the gallium trichloride trap is an impact type gas sampling bottle, the generated gallium trichloride is in a gaseous state at high temperature and sequentially enters the gallium trichloride trap, namely the impact type gas sampling bottle, the tail end of the tail gas is connected with a tail gas trapping unit 4, and unreacted hydrogen chloride gas coming out of the gallium trichloride trap 5-3 enters the tail gas trapping unit 4. The tail gas capturing unit 4 contains alkali liquor or water, the alkali liquor is preferably sodium hydroxide or sodium carbonate solution, hydrogen chloride gas entering the tail gas capturing unit 4 is either reacted with the alkali liquor to generate sodium chloride aqueous solution, or is dissolved in water to be converted into dilute acid.
In another embodiment, as shown in FIG. 1, the bottom of the quartz reaction unit 2 comprises 2 gas inlets, ar 2 And a hydrogen chloride gas inlet; firstly, introducing argon to discharge all air in a quartz reaction unit, a pipeline and a gallium trichloride catcher out of the device; and introducing hydrogen chloride gas to react with the metal gallium heated to the preset temperature in the reaction tank to generate gallium trichloride gas.
In the device, the generated gallium trichloride gas is gaseous in the quartz reaction unit, and the gaseous gallium trichloride gas enters the gallium trichloride trap through a gas output pipeline such as a conduit and then is changed into a liquid state due to temperature reduction; the mixed tail gas of the residual gallium trichloride and the hydrogen chloride enters the final gallium trichloride catcher to be instantly cooled and changed into gallium trichloride crystals.
In another exemplary embodiment of the present invention, there is provided a method for preparing gallium trichloride, which is performed using the above apparatus, the method including: step S1, filling a gallium simple substance into a reaction tank, then introducing hydrogen chloride gas into a quartz reaction unit, and dispersing the hydrogen chloride gas in the quartz reaction unit through a gas distributor; s2, reacting the gallium simple substance with hydrogen chloride gas in a quartz reaction unit at the reaction temperature of 210-500 ℃ to obtain a gas mixture of gallium trichloride and hydrogen chloride; and S3, enabling the gas mixture to sequentially enter a plurality of gallium trichloride traps which are connected in series through a gas output pipeline to obtain gallium trichloride crystalline solid.
By utilizing the preparation method, the gas distributor is arranged in the quartz reaction unit, so that the hydrogen chloride gas is uniformly dispersed by the gas distributor, and is fully contacted with the gallium simple substance in the quartz reaction unit, and the reaction can be rapidly and completely carried out, thereby improving the utilization rate of the hydrogen chloride gas and the production efficiency of the gallium trichloride, and reducing the production cost of the gallium trichloride.
Further, in the above method, the temperature of at least one of the gallium trichloride trap and the gas output line is 65 to 200 ℃, preferably 100 to 200 ℃, more preferably 110 to 180 ℃. In step S2, the reaction temperature is 210 to 400 ℃, preferably 320 to 400 ℃. By controlling the temperature of the quartz reaction unit and the temperature of the temperature control unit within the above range, the gallium simple substance and the hydrogen chloride gas can react more completely in the quartz reaction unit, the generated gallium trichloride can be better ensured to exist in a gaseous state in the quartz reaction unit, and the gallium trichloride is collected in a liquid form in the gallium trichloride trap in the temperature control unit. The temperature of the temperature control unit is controlled to convert water molecules into gaseous state, so that the solubility of hydrogen chloride in water can be reduced.
Further, from the viewpoint of environmental protection and economy, the method further comprises a step S4 of allowing the tail gas hydrogen chloride gas released from the gallium trichloride collecting unit to enter the tail gas trapping unit, wherein the temperature of the tail gas trapping unit is 5 ℃ to 30 ℃. The tail gas trapping unit is used for trapping unreacted hydrogen chloride gas, so that the cyclic utilization of the hydrogen chloride gas can be realized, the utilization rate of the hydrogen chloride gas and the production efficiency of gallium trichloride are further improved, and the production cost of the gallium trichloride is reduced. Preferably, the off-gas capture unit contains a lye, preferably an aqueous solution of sodium hydroxide or sodium carbonate, or water.
Further, in the above method, a step S0 of introducing an inert gas into the quartz reaction unit at a flow rate of preferably 20 to 50ml/min is further included. It will be understood by those skilled in the art that any inert gas may be used as long as the inert gas used does not react with the raw materials in the present invention, and argon is preferred from the viewpoint of economy and ready availability. The reaction can be carried out under the conditions of no water and no oxygen by flushing the quartz reaction unit, the pipeline and the gallium trichloride catcher by utilizing argon before the reaction, thereby further improving the utilization rate of hydrogen chloride gas and the production efficiency of gallium trichloride and reducing the cost for synthesizing gallium trichloride. Preferably, the purity of the argon is up to 99.99wt%.
Specifically, firstly, introducing argon to evacuate air in the connecting pipeline; then the quartz tube is heated to a preset temperature by using a heating system, then the argon gas cylinder is closed, the hydrogen chloride gas cylinder is opened, and the flow rate of hydrogen chloride is adjusted. The hydrogen chloride gas is contacted with the liquid gallium chloride in the annular tube of the quartz tube to react. The gallium trichloride gas enters a gallium trichloride catcher, the gallium trichloride is converted into liquid gallium trichloride from the gas due to the temperature reduction, and the residual gaseous gallium trichloride is further cooled to room temperature and directly converted into solid gallium trichloride. The tail gas hydrogen chloride enters a tail gas trapping unit, and the tail gas is purified, absorbed and then emptied; and after the reaction, the gallium trichloride solid or liquid gallium trichloride is directly sealed at the inlet and the outlet, and is sealed for later use.
In one embodiment, as shown in FIG. 1, the method of the present invention comprises the steps of: solid gallium simple substances are filled into an annular middle through reaction tank 6-2 in a quartz reaction unit in advance, the gallium simple substances are preferably uniformly distributed in the reaction tank, a gas cylinder 1 filled with protective gas argon is opened, argon is introduced, the argon is uniformly dispersed in the quartz reaction unit through a gas distributor 6-1, the introduction time of the argon is about 10min to 30min until all impurities such as air in the quartz reaction unit 2, a pipeline and gallium trichloride traps 5-1, 5-2 and 5-3 are emptied. Closing the gas cylinder 1 filled with protective gas argon, opening the gas cylinder 2 filled with hydrogen chloride gas at the flow rate of 20-60 ml/min, feeding the hydrogen chloride gas into the quartz reaction unit 2 along a feeding pipeline, heating the quartz reaction unit 2 to 210-500 ℃, and reacting high-purity hydrogen chloride with metal gallium to generate gallium trichloride gas. The temperature of the temperature control unit 1 is adjusted to 65-200 ℃, so that the temperature of the temperature control unit 1 is lower than that of the quartz reaction unit 2, and the gallium trichloride gas enters the gallium trichloride trap 5-1 and the gallium trichloride trap 5-2 through the output pipeline and then is liquefied; unreacted hydrogen chloride gas and residual unliquefied gallium trichloride gas leave the temperature control unit 1 through an output pipeline such as a conduit pipeline and enter a gallium trichloride trap 5-3 under the room temperature condition, and the residual gallium trichloride gas is rapidly desublimated and crystallized due to temperature shock, so that gallium trichloride crystals are generated; the tail gas hydrogen chloride gas enters the tail gas trapping unit 4 through an output pipeline such as a guide pipe, and reacts with alkali liquor or water in the tail gas trapping unit 4 to generate sodium chloride water solution or dilute acid; after the gallium simple substance and the hydrogen chloride gas are reacted, closing the gas cylinder No. 2 filled with the hydrogen chloride gas, opening the gas cylinder No. 1 filled with the protective gas argon, and leading the argon to empty the quartz reaction unit 2, the pipeline and the residual hydrogen chloride in the gallium trichloride traps 5-1, 5-2 and 5-3, wherein the time for introducing the argon is about 10min to 30min; after the reaction is finished, under the condition of introducing argon, isolating and sealing the gallium trichloride trap in sections, preferably sequentially sealing a terminal gallium trichloride trap 5-3, a terminal gallium trichloride trap 5-2 and a terminal gallium trichloride trap 5-1 by using balloons in sections; preferably, the sealed gallium trichloride traps 5-1, 5-2 and 5-3 are transferred into a vacuum glove box for operation, the vacuum glove box is transferred into the glove box, the top device of the impact type gas sampling bottle is replaced by a rubber plug, sealing and storage are carried out, and after cooling, white needle-shaped crystalline solid of gallium trichloride is obtained.
The following examples are provided to further illustrate the benefits of the present application.
Examples
Preparation in the early stage of the experiment: opening a heating sleeve at the periphery of the quartz reaction unit, taking out the quartz reaction unit, pulling out plugging rubber plugs 7-1 and 7-2 at the top and the bottom of the quartz reaction unit, putting a small amount of elemental gallium into a beaker, and heating the beaker by hot water to liquefy the gallium; liquid gallium is sucked by a quartz suction pipe and is uniformly placed in an annular middle through reaction tank 6-2; at the moment, the quartz reaction unit is fixed in the heating sleeve, and the quartz reaction unit is blocked by the blocking rubber plugs 7-1 and 7-2.
When the reactor is operated, opening the gas cylinder No. 1 filled with protective gas argon, and introducing argon to discharge air in the quartz reaction unit, the pipeline and the gallium trichloride catcher out of the reaction device; opening the temperature control unit to raise the temperature to 65-200 ℃ of the target temperature; then opening a temperature control device of a quartz reaction unit heating sleeve, and heating to a reaction temperature of 210-500 ℃; closing the gas cylinder 1 filled with protective gas argon and opening the gas cylinder 2 filled with hydrogen chloride gas; the hydrogen chloride is uniformly dispersed by the gas distributor and contacts with the metal gallium in the reaction tank to generate gallium trichloride gas; the gallium trichloride gas and unreacted hydrogen chloride enter the gallium trichloride trap 5-1 through an outlet at the top end of the quartz reaction unit and a gas output pipeline such as a conduit, and because the temperature of the gallium trichloride trap 5-1 is lower than the liquefaction temperature of the gallium trichloride gas by 203 ℃, liquid of gallium trichloride can appear at the bottom of the gallium trichloride trap 5-1; the unliquefied gallium trichloride gas continuously enters the gallium trichloride trap 5-2 along a gas output pipeline such as a conduit and is continuously liquefied at the bottom of the gallium trichloride trap 5-2; at the moment, the residual gallium trichloride gas and hydrogen chloride gas continuously leave the temperature control unit along an output pipeline such as a guide pipe and enter the gallium trichloride catcher 5-3 along the output pipeline such as the guide pipe; because the temperature of the residual gas is instantly reduced to the room temperature, the gallium trichloride gas is cooled and crystallized at the bottom of the gallium trichloride catcher 5-3 to form a solid gallium trichloride crystal; the incompletely reacted hydrogen chloride gas will pass along an output line, such as a conduit, into the tail gas capture unit 4.
When the reaction is finished, the gallium simple substance is reacted, at the moment, the gas cylinder No. 2 filled with hydrogen chloride gas is closed, and the gas cylinder No. 1 filled with protective gas argon is opened; and completely removing hydrogen chloride and gallium trichloride gas remained in the quartz reaction unit, the pipeline and the gallium trichloride catcher. At the moment, the drying oven is opened, the gallium trichloride traps 5-3, 5-2 and 5-1 are sequentially blocked in a segmented mode, and the gallium trichloride traps are transferred to the interior of the vacuum glove box. Then, a rubber plug is adopted to seal the gas collecting bottle, and white needle-shaped crystalline solid of gallium trichloride is obtained.
Example 1
2g of metal gallium with the purity of 99.99wt% is transferred to an annular hollow reaction tank of a quartz reaction unit and is uniformly distributed on the annular hollow reaction tank; opening a gas cylinder 1 filled with protective gas argon, introducing argon at a gas flow rate of 80ml/min, and continuing for 15min to remove all air in a quartz reaction unit, a conduit and a gallium trichloride catcher out of a reaction system; then, closing the gas cylinder No. 1 filled with protective gas argon, opening the gas cylinder No. 2 filled with hydrogen chloride gas, heating a heating jacket of the quartz reaction unit to 220 ℃, introducing the hydrogen chloride gas at a gas flow rate of 40ml/min, and continuing for 120min to enable the hydrogen chloride gas and metal gallium to fully react to generate gaseous gallium trichloride;
then, the temperature of the temperature control unit is controlled at 200 ℃, gaseous gallium trichloride is liquefied in the gallium trichloride catcher 5-1 and the gallium trichloride catcher 5-2 due to temperature reduction, and liquid gallium trichloride is formed at the bottom of the gallium trichloride catcher; the residual gallium trichloride gas enters a gallium trichloride trap 5-3 through a gas output pipeline, and the gallium trichloride gas is crystallized to form a gallium trichloride crystal due to desublimation because the temperature is reduced to room temperature;
after the reaction is finished, closing the gas cylinder No. 2 filled with hydrogen chloride gas, opening the gas cylinder No. 1 filled with protective gas argon, introducing argon at the gas flow rate of 60ml/min, continuing for 30min, and removing all residual gallium trichloride gas and hydrogen chloride gas in a quartz reaction unit, a pipeline and a gallium trichloride trap out of a reaction system; then, the gallium trichloride catcher 5-3, the gallium trichloride catcher 5-2 and the gallium trichloride catcher 5-1 are sequentially isolated and sealed in a segmentation way, and the gallium trichloride catcher is transferred into a vacuum glove box, a gas collection bottle is sealed by a rubber plug and stored, and the purity of white crystals of gallium trichloride is more than 99.90wt% through ICP-Mas and ICP-OES analysis.
Example 2
Transferring 2g of liquid metal gallium with the purity of 99.99wt% to an annular hollow reaction tank of a quartz reaction unit, and uniformly distributing the liquid metal gallium on the annular hollow reaction tank; opening a gas cylinder 1 filled with protective gas argon, introducing argon at the gas flow rate of 100ml/min, and continuing for 30min to remove all air in the quartz reaction unit, the conduit and the gallium trichloride catcher out of the reaction system; then, heating a heating jacket of the quartz reaction unit to 320 ℃, closing the gas cylinder No. 1 filled with the protective gas argon, opening the gas cylinder No. 2 filled with the hydrogen chloride gas, introducing the hydrogen chloride gas at a gas flow rate of 40ml/min, and continuing for 120min to ensure that the hydrogen chloride gas and the metal gallium are fully reacted to generate gaseous gallium trichloride;
then, the temperature of the temperature control unit is controlled at 180 ℃, gaseous gallium trichloride is liquefied in the gallium trichloride catcher 5-1 and the gallium trichloride catcher 5-2 due to temperature reduction, and liquid gallium trichloride is formed at the bottom of the gallium trichloride catcher; the residual gallium trichloride gas enters a gallium trichloride trap 5-3 through a gas output pipeline, and the gallium trichloride gas is crystallized to form a gallium trichloride crystal due to desublimation because the temperature is reduced to room temperature;
after the reaction is finished, closing the gas cylinder No. 2 filled with hydrogen chloride gas, opening the gas cylinder No. 1 filled with protective gas argon, introducing argon at a gas flow rate of 60ml/min, continuing for 30min, and removing all residual gallium trichloride gas and hydrogen chloride gas in a quartz reaction unit, a pipeline and a gallium trichloride trap out of a reaction system; then, the gallium trichloride catcher 5-3, the gallium trichloride catcher 5-2 and the gallium trichloride catcher 5-1 are sequentially isolated and sealed in a segmentation way, and the gallium trichloride catcher is transferred into a vacuum glove box, a gas collecting bottle is sealed by a rubber plug and stored, and the purity of white needle-shaped gallium trichloride crystals obtained by ICP-Mas and ICP-OES analysis is more than 99.99wt%.
Example 3.
Transferring 2g of liquid metal gallium with the purity of 99.99wt% to an annular hollow reaction tank of a quartz reaction unit, and uniformly distributing the liquid metal gallium on the annular hollow reaction tank; opening a gas cylinder No. 1 filled with protective gas argon, introducing argon at the gas flow rate of 120ml/min, and continuing for 20min to remove all air in a quartz reaction unit, a conduit and a gallium trichloride catcher out of a reaction system; then, heating a heating jacket of the quartz reaction unit to 420 ℃, closing the gas cylinder No. 1 filled with protective gas argon, opening the gas cylinder No. 2 filled with hydrogen chloride gas, and introducing the hydrogen chloride gas at a gas flow rate of 60ml/min to ensure that the hydrogen chloride gas and the metal gallium are fully reacted to generate gaseous gallium trichloride;
then, the temperature of the temperature control unit is controlled at 110 ℃, gaseous gallium trichloride is liquefied in the gallium trichloride catcher 5-1 and the gallium trichloride catcher 5-2 due to temperature reduction, and liquid gallium trichloride is formed at the bottom of the gallium trichloride catcher; the residual gallium trichloride gas enters a gallium trichloride catcher 5-3 through a gas output pipeline, and the gallium trichloride gas is crystallized to form a gallium trichloride crystal due to sublimation when the temperature is reduced to room temperature;
after the reaction is finished, closing the gas cylinder No. 2 filled with hydrogen chloride gas, opening the gas cylinder No. 1 filled with protective gas argon, introducing argon at the gas flow rate of 80ml/min, continuing for 20min, and removing all residual gallium trichloride gas and hydrogen chloride gas in a quartz reaction unit, a pipeline and a gallium trichloride trap out of a reaction system; then, the gallium trichloride catcher 5-3, the gallium trichloride catcher 5-2 and the gallium trichloride catcher 5-1 are sequentially isolated and sealed in a subsection mode, the gallium trichloride catcher is transferred into a vacuum glove box, a rubber plug is used for sealing a gas collecting bottle, the gas collecting bottle is stored, and white needle-shaped gallium trichloride crystal purity higher than 99.99wt% is obtained through ICP-Mas and ICP-OES analysis.
From the above description, it can be seen that the above-described embodiments of the present invention achieve the following technical effects: by applying the technical scheme of the invention, the gas distributor and the further annular middle through reaction tank are arranged in the quartz reaction unit, and the temperature of the quartz reaction unit and the temperature of the temperature control unit are accurately controlled, so that the utilization rate of hydrogen chloride gas and the production efficiency of gallium trichloride are effectively improved; the synthesis method remarkably reduces the cost for synthesizing the gallium trichloride by cooling, liquefying, sublimating, crystallizing, separating the gallium trichloride, packaging and storing.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. An apparatus for producing gallium trichloride, comprising:
a raw material supply unit including a hydrogen chloride supply device;
the quartz reaction unit is connected with the hydrogen chloride supply device through a feed pipeline and comprises a gas distributor and a reaction tank;
the gallium trichloride collecting unit comprises a plurality of gallium trichloride traps which are connected in series, and the quartz reaction unit is connected with the gas output pipeline.
2. The apparatus of claim 1, further comprising a temperature control unit that controls the temperature of at least one of the gallium trichloride trap and the gas output line.
3. The apparatus of claim 2, further comprising a temperature control device for controlling the temperature of the quartz reaction unit, and the temperature control device and the temperature control unit are independent from each other.
4. The apparatus according to claim 1 or 2, further comprising a tail gas capturing unit and an inert gas supply unit, wherein the tail gas capturing unit is connected with the gallium trichloride collecting unit through a gas output pipeline, and the inert gas supply unit is connected with the quartz reaction unit through an inert gas supply pipeline.
5. The apparatus of claim 1 or 2, wherein the reaction tank is an annular through-channel reaction tank.
6. A method for producing gallium trichloride, characterized in that the method is carried out using the device according to any one of claims 1 to 5, and comprises:
step S1, filling a gallium simple substance into the reaction tank, and then introducing hydrogen chloride gas into the quartz reaction unit, wherein the hydrogen chloride gas is dispersed in the quartz reaction unit through the gas distributor;
s2, reacting the gallium simple substance with hydrogen chloride gas in the quartz reaction unit at the reaction temperature of 210-500 ℃ to obtain a gas mixture of gallium trichloride and hydrogen chloride;
and S3, enabling the gas mixture to sequentially enter a plurality of gallium trichloride traps which are arranged in series through the gas output pipeline to obtain gallium trichloride crystalline solids.
7. The method of claim 6, wherein at least one of the gallium trichloride trap and the gas outlet line has a temperature of 65 ℃ to 200 ℃.
8. The method according to claim 6, wherein the reaction temperature in step S2 is 210 to 400 ℃.
9. The method according to any one of claims 6 to 8, further comprising a step S4 of feeding the off-gas hydrogen chloride gas released from the gallium trichloride collecting unit into an off-gas capturing unit, wherein the temperature of the off-gas capturing unit is 5 ℃ to 30 ℃.
10. The method according to any one of claims 6 to 8, further comprising a step S0 of introducing an inert gas into the quartz reaction unit.
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Application publication date: 20221125 |