CN114210259B - Gallium trichloride granulating and packaging device and method - Google Patents
Gallium trichloride granulating and packaging device and method Download PDFInfo
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- CN114210259B CN114210259B CN202111349636.3A CN202111349636A CN114210259B CN 114210259 B CN114210259 B CN 114210259B CN 202111349636 A CN202111349636 A CN 202111349636A CN 114210259 B CN114210259 B CN 114210259B
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- inert gas
- gallium trichloride
- pressure balancer
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- UPWPDUACHOATKO-UHFFFAOYSA-K gallium trichloride Chemical compound Cl[Ga](Cl)Cl UPWPDUACHOATKO-UHFFFAOYSA-K 0.000 title claims abstract description 84
- 238000004806 packaging method and process Methods 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 27
- 239000011261 inert gas Substances 0.000 claims abstract description 71
- 238000007789 sealing Methods 0.000 claims abstract description 44
- 238000005469 granulation Methods 0.000 claims abstract description 18
- 230000003179 granulation Effects 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims description 19
- 239000002245 particle Substances 0.000 claims description 13
- 239000007787 solid Substances 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 8
- 238000003825 pressing Methods 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims description 2
- 238000010923 batch production Methods 0.000 abstract 1
- 230000007613 environmental effect Effects 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 16
- 229910052757 nitrogen Inorganic materials 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 4
- 210000005239 tubule Anatomy 0.000 description 4
- 238000004891 communication Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000011521 glass Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000005388 borosilicate glass Substances 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- XOYLJNJLGBYDTH-UHFFFAOYSA-M chlorogallium Chemical compound [Ga]Cl XOYLJNJLGBYDTH-UHFFFAOYSA-M 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 210000001503 joint Anatomy 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
Classifications
-
- 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
- B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
- B01J2/02—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops
- B01J2/06—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops in a liquid medium
-
- 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
- B01J19/14—Production of inert gas mixtures; Use of inert gases in general
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65B—MACHINES, APPARATUS OR DEVICES FOR, OR METHODS OF, PACKAGING ARTICLES OR MATERIALS; UNPACKING
- B65B1/00—Packaging fluent solid material, e.g. powders, granular or loose fibrous material, loose masses of small articles, in individual containers or receptacles, e.g. bags, sacks, boxes, cartons, cans, or jars
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65B—MACHINES, APPARATUS OR DEVICES FOR, OR METHODS OF, PACKAGING ARTICLES OR MATERIALS; UNPACKING
- B65B39/00—Nozzles, funnels or guides for introducing articles or materials into containers or wrappers
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Packages (AREA)
Abstract
The invention discloses a gallium trichloride granulating and packaging device, which comprises: the device comprises a reactor, a granulating hose, a pressure balancer, an inert gas unit, a vacuum unit and a product packaging bottle, wherein the granulating hose is detachably arranged in the pressure balancer, the reactor is communicated with the granulating hose through a diversion pipe, the vacuum unit is respectively communicated with the granulating hose and the pressure balancer through a vacuumizing pipeline, the inert gas unit is respectively communicated with the pressure balancer and the granulating hose through an inert gas pipeline, the granulating hose comprises a hose body, an opening at one end of the hose body is provided with an adapter connector which is in sealing fit with the opening of the hose body, the adapter connector can be in sealing connection with the diversion connector, a plug or a bottle opening of the product packaging bottle, and the diversion connector is in sealing connection with the diversion pipe and the vacuumizing pipeline. Also provided is a gallium trichloride granulation packaging method. The method has the advantages of low cost, simple and convenient operation, safety, environmental protection, high productivity, high efficiency, stable and reliable operation, easy batch production, and high and stable product purity.
Description
Technical Field
The invention belongs to the field of fine chemical production, and particularly relates to a gallium trichloride granulating and packaging device and method.
Background
Anhydrous gallium trichloride has a molecular formula of GaCl 3 Density of 2.47g/cm 3 (25 ℃ C.), the melting point is 78 ℃ C. And the boiling point is 201.3 ℃ C. Gallium trichloride is white or colorless needle crystal, and is easy to absorb moisture and deliquesce in air, and its operation and preservation need to be carried out under anhydrous and anaerobic condition. Gallium trichloride has strong corrosiveness and has corrosiveness to most of organic polymer materials and metal materials, and the production, preparation, granulation and packaging and preservation of the gallium trichloride need to use corrosion-resistant materials.
The existing gallium trichloride granulating and packaging method has less report and mainly comprises the following steps: gallium trichloride was put into a flask with a tubule, the flask was heated to 85 ℃ or higher to melt gallium trichloride, gallium trichloride in the flask was dropped into liquid nitrogen through the tubule and cooled to solid particles, and liquid nitrogen was removed in a dry atmosphere to obtain granular gallium trichloride.
According to the gallium trichloride granulating and packaging method, gallium trichloride is required to be filled into a flask and heated for melting, then the gallium trichloride in the flask is dripped into liquid nitrogen through the tubule to be cooled into solid particles, the operation is complex, the productivity is low, the tubule dripped with the gallium trichloride is arranged above the liquid nitrogen, the cooling is very easy to be carried out, the pipeline is blocked, the production is unstable, and the method cannot be suitable for large-scale production.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide the gallium trichloride granulating and packaging device which has the advantages of simple component, low cost, simple and convenient operation, safe and environment-friendly operation, high productivity, high efficiency and stable and reliable operation, and also provides the gallium trichloride granulating and packaging method which has the advantages of low cost, simple and convenient operation, safe and environment-friendly process, high productivity, high efficiency, stable and reliable operation, low safety risk, easy mass production, sustainability and high and stable product purity.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a gallium trichloride granulation packaging device comprising:
the granulating device comprises a reactor, a granulating hose, a pressure balancer, an inert gas unit, a vacuum unit and a product packaging bottle, wherein the granulating hose is detachably arranged in the pressure balancer, the reactor is communicated with the granulating hose through a flow guide pipe, the vacuum unit is respectively communicated with the granulating hose and the pressure balancer through a vacuumizing pipeline, the inert gas unit is respectively communicated with the pressure balancer and the granulating hose through an inert gas pipeline, the granulating hose comprises a hose body, two ends of the hose body are opened, one end of the hose body is sealed by a plug, the other end of the hose body is opened and is provided with an adapter connector in sealing fit with the opening of the hose body, the adapter connector can be in sealing connection with a flow guide connector, the plug or the bottle mouth of the product packaging bottle, and the flow guide connector is in sealing connection with the flow guide pipe and the vacuumizing pipeline communicated with the granulating hose.
The two ends of the hose body are opened, one end opening is sealed by the plug, the other end opening is provided with a diversion joint or an adapter joint which is in sealing fit with the opening of the hose body, the diversion joint is in sealing connection with the diversion pipe and a vacuumizing pipeline which is communicated with the granulating hose, and the adapter joint can be in sealing connection with the plug and the bottle mouth of the product packaging bottle.
Preferably, the inert gas unit comprises an inert gas buffer tank, and the inert gas buffer tank is respectively connected with an inert gas source, a pressure balancer and a granulating hose through inert gas pipelines;
the vacuum unit comprises a vacuum buffer tank and a vacuum pump, and the vacuum buffer tank is connected with the vacuum pump, the pressure balancer and the granulating hose through vacuumizing pipelines respectively.
Preferably, the inert gas buffer tank is connected with the vacuum buffer tank through a pipeline, and an on-off valve is arranged on the pipeline.
Preferably, the inert gas pipeline comprises an inert gas main pipeline and an inert gas branch pipeline, the outlet of the inert gas buffer tank is communicated with the inert gas main pipeline, the inert gas main pipeline is communicated with the pressure balancer through an inert gas branch pipeline, and is communicated with the flow guide pipe through another inert gas branch pipeline.
Preferably, the pressure balancer comprises a pressure balancer body and a detachable cap, wherein one end of the pressure balancer body is opened and sealed by the detachable cap; the detachable cap is provided with a through hole for accommodating the honeycomb duct and the vacuumizing pipeline communicated with the granulating hose.
Preferably, two openings are arranged on the side wall of the pressure balancer body, and the two openings are respectively communicated with the vacuumizing pipeline and the inert gas pipeline.
As a general inventive concept, the present invention also provides a gallium trichloride granulation packaging method, which adopts the aforementioned granulation device to carry out granulation packaging, comprising the following steps:
s1, charging: controlling the temperature of the reactor to be 85-140 ℃, placing a granulating hose in a pressure balancer, connecting other parts according to the connection relation, controlling the granulating hose and the pressure balancer to be in a negative pressure state by controlling a vacuum unit to vacuumize, opening a valve of a flow guide pipe, introducing gallium trichloride liquid in the reactor into the granulating hose by using the pressure difference, closing the flow guide pipe valve after the introduction is finished, closing the vacuum unit, controlling an inert gas unit, filling inert protective gas into the granulating hose and the pressure balancer, and recovering the granulating hose and the pressure balancer to normal pressure;
s2, opening a pressure balancer, taking down a diversion connector, taking out a granulating hose filled with gallium trichloride, immediately sealing the adapter connector by a plug, transferring the granulating hose to a cooling area, and cooling the gallium trichloride into solid;
s3, extruding the granulating hose by using a pipe pressing device with matched pipe diameters, so that gallium trichloride solids in the hose are broken into blocks, and the breaking granulating process is completed;
s4, taking down the plug of the sealed granulating hose, quickly connecting the adapter into a packaging bottle, enabling gallium trichloride particles to flow into the product packaging bottle completely, removing the granulating hose, and sealing the product packaging bottle.
Preferably, in step S1, the negative pressure state in the granulating hose and the pressure balancer is controlled to be: the pressure of the granulating hose and the pressure balancer is controlled to be-0.06 to-0.02 MPa.
Preferably, the granulating hose is made of PFA or FEP; the granulating hose is cylindrical, the diameter is 10-100 mm, and the height is 200-2000 mm.
Preferably, in step S1, when the gallium trichloride liquid is introduced into the granulating tube, the gallium trichloride liquid level in the granulating tube is controlled to be 1/2 to 3/4 of the height thereof.
Preferably, in step S2, after the granulating hose filled with gallium trichloride is taken out, if charging is to be continued, an empty granulating hose is connected, and the charging operation in step S1 is repeated.
Compared with the prior art, the invention has the following advantages:
1. the device can directly transfer gallium trichloride from the gallium trichloride reactor without adding a transit storage tank or container, the operation flow is short, gallium trichloride is led into a granulating hose through negative pressure, the leakage risk generated by positive pressure operation can be reduced (the gallium trichloride reactor is generally made of borosilicate glass or quartz, and is easy to break under positive pressure to generate leakage accidents), the device can ensure the balance of the internal pressure and the external pressure of the hose, nitrogen (or other inert gases) is filled into the device, the granulating hose and the pressure balancer are at normal pressure, the formed inert atmosphere can avoid moisture absorption of gallium trichloride products, the leakage risk caused by external force knocking damage can be avoided in subsequent granulation, the whole process is safe and environment-friendly, the productivity is high, the operation is stable and reliable, and the safety risk is low; in the device, the granulating hose can realize internal and external pressure balance, so that the granulating hose is prevented from deforming due to the fact that the external pressure of the granulating hose is higher than the internal pressure of the granulating hose, and the granulating hose can be in sealing butt joint with a packaging bottle through the customized adapter and the detachable plug, so that a gallium trichloride particle product can be rapidly filled into the packaging bottle, and the operation is simple and convenient; the granularity of gallium trichloride products can be easily controlled by selecting granulating hoses and tube presses with different tube diameters, and the method is simple and reliable; the device can avoid introducing impurities, the purity of the prepared gallium trichloride particle product can reach 5N, and the product quality is stable and reliable.
2. The gallium trichloride granulating and packaging method has the advantages of low cost, simple and convenient operation, safe and environment-friendly process, high productivity and efficiency, stable and reliable operation, low safety risk, easy mass production, sustainability and high and stable granulating product purity.
Drawings
Fig. 1 is a schematic structural view of a gallium trichloride granulation packaging device of the present invention.
Reference numerals:
1. a reactor; 2. a pressure balancer; 21. a removable cap; 211. sealing buckle; 212. an O-shaped sealing ring; 3. a granulating hose; 31. a diversion joint; 32. an adapter; 33. a plug; 4. an inert gas buffer tank; 5. a vacuum buffer tank; 6. a vacuum pump; 7. packaging the product; 71. GL45 threaded bottle cap; 8. a ball valve; 9. sealing the joint.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
A gallium trichloride granulating and packaging device, the structural schematic diagram of which is shown in fig. 1, comprising:
the granulating device comprises a reactor 1, a granulating hose 3, a pressure balancer 2, an inert gas unit, a vacuum unit and a product packaging bottle 7, wherein the granulating hose 3 is detachably arranged in the pressure balancer 2, the reactor 1 is in sealing communication with the granulating hose 3 through a flow guide pipe, the vacuum unit is respectively in sealing communication with the granulating hose 3 and the pressure balancer 2 through vacuumizing pipes, the inert gas unit is respectively in sealing communication with the pressure balancer 2 and the granulating hose 3 through inert gas pipes, the granulating hose 3 comprises a hose body 31, two ends of the hose body are opened, one end of the hose body is opened and provided with a plug 33 for sealing the opening, the other end of the hose body is opened and provided with an adapter 32 in sealing connection with the opening of the granulating hose 3, and the adapter 32 can be in sealing connection with the flow guide joint 31, the detachable plug 33 or the bottle mouth of the product packaging bottle 7. The diversion joint 31 is in sealing connection with the diversion pipe and the vacuumizing pipeline communicated with the granulating hose 3. The diversion connector 31, the adapter connector 32 and the plug 33 are made of polytetrafluoroethylene.
When gallium trichloride solution is led into the granulating hose 3 from the reactor 1, an opening of the granulating hose 3 is provided with an adapter connector 32, the adapter connector is sealed by a diversion connector 31, the diversion connector 31 is respectively and hermetically connected with a diversion pipe and a vacuumizing pipe, specifically, a through hole is formed in the diversion connector 31 for the passage of the diversion pipe and the vacuumizing pipe, and the through hole is sealed by a sealing connector 9; after the gallium trichloride solution is introduced, the diversion connector 31 is taken down, the diversion connector 32 is replaced by a plug 33 for sealing the transfer connector 32, the diversion connector 32 is transferred to a cooling area, and after the granulation is completed, the transfer connector 32 is in sealing connection with the bottleneck of the product packaging bottle 7 in the process of transferring gallium trichloride particles to the product packaging bottle 7, so that the transfer of gallium trichloride particles under the sealing condition is completed.
The granulating hose 3 is made of PFA or FEP, and the granulating hose 3 has good elasticity and restorability, and can be restored to the original state even after extrusion deformation; the granulating hose 3 is cylindrical, has the diameter of 10-100 mm and the height of 200-2000 mm. The adapter 32 can be customized to be in sealing engagement with schottky bottles with bottle mouth threads GL25, GL32, GL45 or GL80, or can be customized to be in sealing engagement with product packaging bottles 7 with threads of other types.
The inert gas unit comprises an inert gas buffer tank 4, and the inert gas buffer tank 4 is respectively connected with an inert gas source, a pressure balancer 2 and a granulating hose 3 through pipelines; specifically, the inlet of the inert gas buffer tank 4 is connected with an inert gas source, such as nitrogen source, through an inlet pipe, and a ball valve 8 is arranged on the inlet pipe close to the inert gas buffer tank 4; the outlet of the inert gas buffer tank 4 is connected with an inert gas pipeline, the inert gas pipeline comprises an inert gas main pipeline and an inert gas branch pipeline, specifically, the outlet of the inert gas buffer tank 4 is connected with the inert gas main pipeline, the inert gas main pipeline is connected with the pressure balancer 2 through a branch pipeline, is communicated with the guide pipe through a branch pipeline and is connected with the granulating hose 3 through the guide pipe, on-off valves are arranged on two branch pipelines close to the main pipeline, and on-off valves (ball valves) are arranged on the main pipeline close to the outlet of the inert gas buffer tank 4.
The vacuum unit comprises a vacuum buffer tank 5 and a vacuum pump 6, the vacuum pump 6 adopts a water ring vacuum pump, and the vacuum buffer tank 5 is respectively connected with the vacuum pump 6, the pressure balancer 2 and the granulating hose 3 through pipelines. Specifically, the outlet of the vacuum buffer tank 5 is connected with the vacuum pump 6 through a pipeline, and a switch valve (ball valve) is arranged on the pipeline close to the vacuum buffer tank 5, the inlet of the vacuum buffer tank 5 is connected with a main vacuumizing pipeline, the main vacuumizing pipeline is respectively connected with the pressure balancer 2 and the granulating hose 3 through two vacuumizing pipelines, and the main vacuumizing pipeline is provided with the switch valve (ball valve).
The inert gas buffer tank 4 is connected with the vacuum buffer tank 5 through a pipeline, and an on-off valve (ball valve) is arranged on the pipeline.
The pressure balancer 3 comprises a body and a detachable cover cap 21, the body of the pressure balancer 3 is a plastic glass tube, one end of the pressure balancer is opened and is sealed by the detachable cover cap 21, the detachable cover cap 21 comprises a cover cap body, a sealing buckle 211 and an O-shaped sealing ring 212, and the detachable cover cap 21 is sealed with the opening of the pressure balancer body through the sealing buckle 211 and the O-shaped sealing ring 212; more specifically, the sealing buckle 211 is disposed on the outer circumferential surface of the cap body, and is used for realizing the buckle connection between the cap body and the pressure balancer body, and the O-shaped sealing ring 212 is disposed inside the cap body, and is used for realizing the sealing between the cap body and the pressure balancer body. The pressure balancer body is respectively connected with the inert gas buffer tank 4 and the vacuum buffer tank 5 through pipelines; the nut cap body is provided with two through holes which are respectively used for accommodating the passage of the honeycomb duct and the vacuumizing tube communicated with the granulating hose, and the through holes are sealed by a sealing joint 9; two openings are arranged on the side wall of the pressure balancer 3 body, and the two openings are respectively communicated with the vacuumizing pipeline and the inert gas pipeline.
The pressure balancer 3 body is made of organic glass, so that the internal state can be clearly observed, and when gallium trichloride is led into the granulating hose 2 by utilizing vacuum, the internal and external pressure balance of the granulating hose 2 can be realized, and the granulating hose 2 is prevented from being deformed due to the high pressure in the pipe outside the pipe.
In the invention, the pipelines of all the components are connected in a sealing way by using Teflon pipes, so that the introduction of other metal impurities is avoided, and the purity of the product reaches 5N.
Example 2
The granulating and packaging method for gallium trichloride adopts a granulating and packaging device shown in figure 1 to carry out granulating and packaging, and comprises the following steps:
(1) Controlling the pressure of the reactor 1 to be normal pressure, controlling the temperature to be 85-140 ℃, controlling the temperature of gallium trichloride liquid to be 85-140 ℃, putting a granulating hose 3 with the diameter of 80mm and the adapter of GL80 internal threads into a pressure balancer 2, butting with a diversion joint 31, tightly covering the pressure balancer 2, starting a vacuum pump 6, controlling the pressures in a vacuum buffer tank 5, the granulating hose 3 and the pressure balancer 2 to be minus 0.06-minus 0.02MPa, opening a flow guide valve, leading 5N gallium trichloride liquid in the reactor 1 into the granulating hose 3 by utilizing the pressure difference, controlling the gallium trichloride liquid level in the granulating hose 3 to be at a position of one half to three quarters of the height of the gallium trichloride liquid, closing the flow guide valve, closing the valve of the vacuum buffer tank 5 and the vacuum pump 6 after the leading-in is finished, opening an inert gas valve, and filling nitrogen (or other inert gas) into the inert gas buffer tank 4, the granulating hose 3 and the pressure balancer 2 to be recovered to normal pressure;
(2) Opening the detachable cap 21 of the pressure balancer 2, taking down the diversion joint 31, taking out the granulating hose 3 filled with gallium trichloride, immediately sealing the adapter joint 32 by the plug 33, putting the granulating hose 3 filled with gallium trichloride liquid into a tool vehicle, and transferring to a cooling area to cool the gallium trichloride into solid;
(3) Extruding the granulating hose 3 by using a pipe pressing device with matched pipe diameters, so that gallium trichloride solids in the hose are broken into blocks, and the breaking granulating process is completed; in the operation, a granulating hose 3 and a tube pressing device with different diameters can be used to control the granularity of the formed gallium trichloride so as to meet the requirements of customers on different particle sizes;
(4) And (3) a granulating hose 3 is vertically arranged, one end with a detachable plug 33 is arranged above, the plug 33 is detached, a GL80 threaded product packaging bottle 7 is quickly connected, the granulating hose 3 is inverted, gallium trichloride particles completely flow into the product packaging bottle 7, the granulating hose 3 is detached, a bottle cap with a tetrafluoro gasket is immediately covered on the product packaging bottle 7, and then a gallium trichloride product with the granularity of 40-60 mm large particles can be obtained, and the product purity reaches 5N.
Example 3
The granulating and packaging method for gallium trichloride adopts a granulating and packaging device shown in figure 1 to carry out granulating and packaging, and comprises the following steps:
(1) Controlling the pressure of the reactor 1 to be normal pressure, controlling the temperature to be 85-140 ℃, controlling the temperature of gallium trichloride liquid to be 85-140 ℃, putting a granulating hose 3 with the diameter of 30mm and the internal thread of GL25 into a pressure balancer 2, butting with a diversion joint 31, tightly covering the pressure balancer 2, starting a water ring vacuum pump 6, controlling the pressures of a vacuum buffer tank 5, the granulating hose 3 and the pressure balancer 2 to be minus 0.06-minus 0.02MPa, opening a flow guide valve, utilizing the pressure difference to lead 5N gallium trichloride liquid in the reactor into the granulating hose 3, controlling the gallium trichloride liquid level in the granulating hose 3 to be at a position of one half to three quarters of the height of the granulating hose, closing a flow guide valve, closing the vacuum buffer tank valve and the water ring vacuum pump 6, opening an inert gas valve, and filling nitrogen (or other inert gas) into the inert gas buffer tank 4, the granulating hose 3 and the pressure balancer 2 to restore the normal pressure;
(2) Opening a pressure balancer cap, taking down the diversion joint 31, taking out the granulating hose 3 filled with gallium trichloride, immediately sealing the adapter joint 32 by the plug 33, putting the granulating hose 3 filled with gallium trichloride liquid into a tool car, and transferring to a cooling area to cool the gallium trichloride into solid;
(3) Extruding the granulating hose 3 by using a pipe pressing device with matched pipe diameters, so that gallium trichloride solids in the hose are broken into blocks, and the breaking granulating process is completed;
(4) And (3) vertically granulating the hose 3, wherein one end with the detachable plug 33 is arranged above, the plug 33 is detached, the GL25 threaded product packaging bottle 7 is quickly connected, the granulating hose 3 is inverted, all gallium trichloride particles flow into the product packaging bottle 7, the granulating hose 3 is detached, the product packaging bottle 7 is immediately covered with a bottle cap with a gasket, and the gallium trichloride product with the granularity of 10-20 mm small particles can be obtained, and the purity of the product reaches 5N.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (8)
1. A gallium trichloride granulation packaging device, characterized by comprising:
the granulating device comprises a reactor (1), a granulating hose (3), a pressure balancer (2), an inert gas unit, a vacuum unit and a product packaging bottle (7), wherein the granulating hose (3) is detachably arranged in the pressure balancer (2), the reactor (1) is communicated with the granulating hose (3) through a flow guide pipe, the vacuum unit is respectively communicated with the granulating hose (3) and the pressure balancer (2) through a vacuumizing pipeline, the inert gas unit is respectively communicated with the pressure balancer (2) and the granulating hose (3) through inert gas pipelines, the granulating hose (3) comprises a hose body, two ends of the hose body are opened, one end of the hose body is sealed by a plug, the other end of the hose body is opened and is provided with an adapter (32) which is in sealing fit with the opening of the hose body, the adapter (32) can be in sealing connection with a flow guide joint (31), a plug (33) or a bottle opening of the product packaging bottle (7), and the flow guide joint (31) is in sealing connection with the flow guide pipe and the vacuumizing pipeline communicated with the granulating hose (3); the inert gas unit comprises an inert gas buffer tank (4), the inert gas pipeline comprises an inert gas main pipeline and an inert gas branch pipeline, an outlet of the inert gas buffer tank (4) is communicated with the inert gas main pipeline, the inert gas main pipeline is communicated with the pressure balancer (2) through an inert gas branch pipeline, and is communicated with the flow guide pipe through another inert gas branch pipeline; the pressure balancer (2) comprises a pressure balancer body and a detachable cap (21), wherein one end of the pressure balancer body is opened and sealed by the detachable cap (21); the detachable cap (21) is provided with a through hole for accommodating the honeycomb duct and passing through a vacuumizing pipeline communicated with the granulating hose (3); two openings are arranged on the side wall of the pressure balancer body and are respectively communicated with the vacuumizing pipeline and the inert gas pipeline.
2. The gallium trichloride granulating and packaging device according to claim 1, wherein the inert gas buffer tank (4) is connected with an inert gas source, a pressure balancer (2) and a granulating hose (3) through inert gas pipelines respectively;
the vacuum unit comprises a vacuum buffer tank (5) and a vacuum pump (6), and the vacuum buffer tank (5) is connected with the vacuum pump (6), the pressure balancer (2) and the granulating hose (3) through vacuumizing pipelines respectively.
3. The gallium trichloride granulation packaging device as set forth in claim 2, wherein the inert gas buffer tank (4) is connected with the vacuum buffer tank (5) through a pipe, and an on-off valve is provided on the pipe.
4. A method for granulating and packaging gallium trichloride, characterized in that the granulating and packaging are carried out by adopting the granulating device as claimed in any one of claims 1 to 3, comprising the following steps:
s1, charging: controlling the temperature of the reactor (1) to be 85-140 ℃, placing a granulating hose (3) in a pressure balancer (2), connecting other components according to the connection relation of any one of claims 1-3, controlling the granulating hose (3) and the pressure balancer (2) to be in a negative pressure state by controlling a vacuum unit to vacuumize, opening a valve of a flow guide pipe, introducing gallium trichloride liquid in the reactor into the granulating hose (3) by utilizing the pressure difference, closing the flow guide pipe valve after the introduction is finished, closing the vacuum unit, and controlling an inert gas unit to charge inert protective gas into the granulating hose (3) and the pressure balancer (2), so that the granulating hose (3) and the pressure balancer (2) are restored to normal pressure;
s2, opening the pressure balancer (2), taking down the diversion connector (31), taking out the granulating hose (3) filled with gallium trichloride, immediately sealing the adapter connector (32) by using the plug (33), transferring the granulating hose (3) to a cooling area, and cooling the gallium trichloride into solid;
s3, extruding a granulating hose (3) by using a pipe pressing device with matched pipe diameters, so that gallium trichloride solids in the hose are broken into blocks, and the breaking granulating process is completed;
s4, taking down a plug (33) of the sealed granulating hose (3), quickly connecting the adapter (32) into a product packaging bottle (7), enabling gallium trichloride particles to flow into the product packaging bottle (7), removing the granulating hose (3), and sealing the product packaging bottle (7).
5. The gallium trichloride granulation packaging method as defined in claim 4, wherein in step S1, the negative pressure state in the granulation control hose (3) and the pressure balancer (2) is: the pressure of the granulating hose (3) and the pressure balancer (2) is controlled to be-0.06 to-0.02 MPa.
6. Gallium trichloride granulation packaging method as defined in claim 4, wherein the material of the granulation hose (3) is PFA or FEP; the granulating hose (3) is cylindrical, the diameter is 10-100 mm, and the height is 200-2000 mm.
7. The gallium trichloride granulation packaging method as defined in claim 4, wherein in step S1, when the gallium trichloride liquid is introduced into the granulation tube (3), the gallium trichloride liquid level in the granulation tube (3) is controlled to be 1/2 to 3/4 of the height thereof.
8. The gallium trichloride granulating and packaging method as defined in claim 4, wherein in step S2, after the granulating tube (3) containing gallium trichloride is taken out, if the charging is to be continued, an empty granulating tube (3) is connected, and the charging operation of step S1 is repeated.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105731525A (en) * | 2014-12-12 | 2016-07-06 | 清远先导材料有限公司 | Preparation method of gallium trichloride granules |
| CN206642695U (en) * | 2016-04-22 | 2017-11-17 | 大连科利德光电子材料有限公司 | A kind of prilling granulator of gallium trichloride |
| CN109939667A (en) * | 2018-01-26 | 2019-06-28 | 中国科学院大连化学物理研究所 | A kind of method that catalyst and synthesis gas directly convert producing light olefins |
| CN113102763A (en) * | 2021-04-12 | 2021-07-13 | 清远先导材料有限公司 | Preparation method of high-purity gallium particles |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105731525A (en) * | 2014-12-12 | 2016-07-06 | 清远先导材料有限公司 | Preparation method of gallium trichloride granules |
| CN206642695U (en) * | 2016-04-22 | 2017-11-17 | 大连科利德光电子材料有限公司 | A kind of prilling granulator of gallium trichloride |
| CN109939667A (en) * | 2018-01-26 | 2019-06-28 | 中国科学院大连化学物理研究所 | A kind of method that catalyst and synthesis gas directly convert producing light olefins |
| CN113102763A (en) * | 2021-04-12 | 2021-07-13 | 清远先导材料有限公司 | Preparation method of high-purity gallium particles |
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