CN118084000A - Purification method and device of boron trichloride - Google Patents
Purification method and device of boron trichloride Download PDFInfo
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- CN118084000A CN118084000A CN202410006338.1A CN202410006338A CN118084000A CN 118084000 A CN118084000 A CN 118084000A CN 202410006338 A CN202410006338 A CN 202410006338A CN 118084000 A CN118084000 A CN 118084000A
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- boron trichloride
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- FAQYAMRNWDIXMY-UHFFFAOYSA-N trichloroborane Chemical compound ClB(Cl)Cl FAQYAMRNWDIXMY-UHFFFAOYSA-N 0.000 title claims abstract description 102
- 238000000034 method Methods 0.000 title claims abstract description 28
- 238000000746 purification Methods 0.000 title claims abstract description 20
- 238000001179 sorption measurement Methods 0.000 claims abstract description 57
- 239000002994 raw material Substances 0.000 claims abstract description 34
- 239000012043 crude product Substances 0.000 claims abstract description 31
- 239000013118 MOF-74-type framework Substances 0.000 claims abstract description 21
- 239000000047 product Substances 0.000 claims abstract description 18
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000002808 molecular sieve Substances 0.000 claims abstract description 6
- 239000002245 particle Substances 0.000 claims abstract description 6
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000012856 packing Methods 0.000 claims abstract description 5
- 239000003507 refrigerant Substances 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 7
- 238000003825 pressing Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 3
- 238000001914 filtration Methods 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 16
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 16
- 239000012535 impurity Substances 0.000 description 10
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 8
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 8
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 8
- 229910002092 carbon dioxide Inorganic materials 0.000 description 8
- 239000001569 carbon dioxide Substances 0.000 description 8
- 229910002091 carbon monoxide Inorganic materials 0.000 description 8
- 239000000460 chlorine Substances 0.000 description 8
- 229910052801 chlorine Inorganic materials 0.000 description 8
- MROCJMGDEKINLD-UHFFFAOYSA-N dichlorosilane Chemical compound Cl[SiH2]Cl MROCJMGDEKINLD-UHFFFAOYSA-N 0.000 description 8
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 8
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 8
- 229910052757 nitrogen Inorganic materials 0.000 description 8
- 239000001301 oxygen Substances 0.000 description 8
- 229910052760 oxygen Inorganic materials 0.000 description 8
- 239000005049 silicon tetrachloride Substances 0.000 description 8
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 8
- 239000005052 trichlorosilane Substances 0.000 description 8
- 239000000945 filler Substances 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 2
- 239000013114 Co-MOF-74 Substances 0.000 description 1
- 239000013115 Zn-MOF-74 Substances 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000005468 ion implantation Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 238000001020 plasma etching Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/06—Boron halogen compounds
- C01B35/061—Halides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
- B01D3/146—Multiple effect distillation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/002—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by condensation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention provides a purification method of boron trichloride, which comprises the following steps: filtering raw material boron trichloride through a filter to remove size particles in the raw material, removing water through a primary adsorption tower, removing phosgene through a secondary adsorption tower, collecting and boosting the raw material through a crude product tank, introducing the raw material into a primary rectifying tower to remove light components, removing heavy components through the secondary rectifying tower, detecting the boron trichloride, collecting qualified products to a product storage tank, and returning unqualified products to the primary adsorption tower for continuous purification; the invention also provides a purification device of the boron trichloride, which removes water and phosgene in the crude boron trichloride through an adsorption tower containing a 4A molecular sieve and MOF-74 series packing, and purifies the boron trichloride through secondary rectification, wherein the process flow is simple, and the product purity can reach 6N level.
Description
Technical Field
The invention belongs to the technical field of chemical industry, and particularly relates to a purification method and device of boron trichloride.
Background
In the production of semiconductor integrated circuits, electron gas is an indispensable core support gas. Boron trichloride is an important electron gas, and can be formed into a film by chemical vapor deposition, so that the boron trichloride is a basic substance for manufacturing optical fiber and integrated circuit BPG materials. In the plasma etching process, boron trichloride is an important gas for etching metal aluminum, and can be used in the processes of doping, ion implantation and the like in IC manufacture.
With the development of the semiconductor industry, the condition control of the semiconductor process is finer and finer, and higher requirements are also put on the purity of the boron trichloride. Only by using high-purity boron trichloride, the chip manufacturing process can be controlled. To achieve sufficient purity of the boron trichloride, it is most critical to remove the harmful, most difficult to remove impurities therein.
Impurities of crude boron trichloride generally include: water, phosgene, chlorine, carbon monoxide, carbon dioxide, hydrogen chloride, dichlorosilane, trichlorosilane, silicon tetrachloride, nitrogen and oxygen. Wherein the boiling points of phosgene and boron trichloride are quite close, and particularly difficult to remove. There is an urgent need for a simple process to purify crude boron trichloride to obtain high quality boron trichloride.
Disclosure of Invention
The invention aims to provide a purification method and device of high-purity boron trichloride, which have simple process and convenient operation.
In order to achieve the aim of the invention, the invention adopts the following technical scheme:
a method for purifying boron trichloride, comprising the steps of:
S1, pressing a boron trichloride raw material in a raw material tank into a first-stage adsorption tower after passing through a filter, removing particles in the raw material through the filter, and removing water in the boron trichloride raw material through the first-stage adsorption tower;
S2, introducing the boron trichloride treated in the S1 into a secondary adsorption tower to remove phosgene in the boron trichloride;
s3, introducing the boron trichloride treated in the step S2 into a crude product tank for collection, and boosting the pressure of the crude product tank after the boron trichloride is collected to the liquid level of 3/4;
s4, introducing boron trichloride in the boosted crude product tank into a first-stage rectifying tower;
S5, after the working pressure and the operating temperature of the primary rectifying tower are stabilized for at least 3 hours, introducing the boron trichloride treated by the S4 into the secondary rectifying tower;
S6, after the working pressure and the operating temperature of the secondary rectifying tower are stable for at least 3 hours, analyzing boron trichloride extracted from the secondary rectifying tower, collecting the boron trichloride to a finished product tank after the boron trichloride is qualified, and returning the boron trichloride to the primary adsorption tower after the boron trichloride is unqualified.
Preferably, the filter diameter is 3-30nm in size.
Preferably, the packing of the first-stage adsorption tower is a 4A molecular sieve, the working pressure of the first-stage adsorption tower is 0.4MPa, the packing of the second-stage adsorption tower is MOF-74 series, and the working pressure of the second-stage adsorption tower is 0.3MPa.
Preferably, the MOF-74 series material is one or a combination of any several of Mg-MOF-74, zn-MOF-74, ni-MOF-74, co-MOF-74, cu-MOF-74, mn-MOF-74 and Cr-MOF-74.
Preferably, the crude product tank is provided with a refrigerant refrigerating device and a heating device, refrigerant is introduced during collection to adjust the pressure of the crude product tank to 0.0-0.1MPa, and the crude product tank is heated to 0.6-1.0MPa after the crude product tank is collected to a certain liquid level;
The finished product tank is provided with a refrigerant refrigerating device and a heating device, and refrigerant is introduced during collection to adjust the pressure of the finished product tank to 0.0-0.1MPa.
Preferably, the working pressure of the primary rectifying tower is 0.5MPa-0.6MPa, the operating temperature is 50-60 ℃, and the number of tower plates is 50-70.
Preferably, the working pressure of the secondary rectifying tower is 0.4MPa-0.5MPa, the operating temperature is 40-50 ℃, and the number of tower plates is 70-100.
Preferably, the top discharge of the secondary rectifying tower is returned to the primary adsorption tower after being analyzed.
Preferably, the purity of the acceptable product is 6N.
A purification device of boron trichloride comprises a raw material tank, a filter, a primary adsorption tower, a secondary adsorption tower, a crude product tank, a primary rectifying tower, a secondary rectifying tower and a finished product tank which are sequentially communicated;
The bottom of the primary rectifying tower is connected with a first heater, the top of the primary rectifying tower is connected with a first condenser, the bottom of the secondary rectifying tower is connected with a second heater, the top of the secondary rectifying tower is connected with a second condenser, the temperature in the rectifying tower is controlled by the first heater and the second heater, and gaseous boron trichloride is condensed and reflowed by the first condenser and the second condenser;
And the top discharge of the secondary rectifying tower is communicated with the primary adsorption tower through a valve, and after the valve is opened, unqualified gas in the finished product tank enters the primary adsorption tower for purification again.
The invention has the beneficial effects that:
According to the purification method of boron trichloride, the impurities such as water, phosgene, chlorine, carbon monoxide, carbon dioxide, hydrogen chloride, dichlorosilane, trichlorosilane, silicon tetrachloride, nitrogen and oxygen in the boron trichloride are removed by adopting a mode of combining secondary adsorption and secondary rectification, the impurity content of the purified boron trichloride is less than 1ppm, and the purity of the boron trichloride can reach 6N levels.
Drawings
FIG. 1 is a schematic diagram of a boron trichloride purification apparatus of the present invention:
Wherein, 1-raw material tank, 2-first-stage adsorption tower, 3-second-stage adsorption tower, 4-crude product tank, 5-first-stage rectifying tower, 6-second-stage rectifying tower, 7-finished product tank, 8-filter.
Detailed Description
The invention will be further described in detail by way of specific examples to enable one skilled in the art to practice the invention by reference to the specification, but the scope of the invention is not limited to the description.
The embodiments 1-3 all adopt a purification device of boron trichloride, which comprises a raw material tank 1, a filter 8, a primary adsorption tower 2, a secondary adsorption tower 3, a crude product tank 4, a primary rectifying tower 5, a secondary rectifying tower 6 and a finished product tank 7 which are communicated in sequence;
The bottom of the primary rectifying tower 5 is connected with a first heater, the top of the primary rectifying tower is connected with a first condenser, the bottom of the secondary rectifying tower 6 is connected with a second heater, the top of the secondary rectifying tower 6 is connected with a second condenser, the temperature in the rectifying tower is controlled through the first heater and the second heater, and gaseous boron trichloride is condensed and reflowed through the first condenser and the second condenser;
And the top discharge of the secondary rectifying tower 6 is communicated with the primary adsorption tower 2 through a valve, and after the valve is opened, unqualified gas in the finished product tank 7 enters the primary adsorption tower 2 for purification again.
Example 1:
the purification method of the boron trichloride, wherein the purity of the boron trichloride raw material is 90%, and raw material impurities comprise moisture, phosgene, chlorine, carbon monoxide, carbon dioxide, hydrogen chloride, dichlorosilane, trichlorosilane, silicon tetrachloride, nitrogen and oxygen, and the method comprises the following specific steps of:
S1, pressing a boron trichloride raw material in a raw material tank 1 into a first-stage adsorption tower 2, removing particles in the raw material through a filter 8 with the diameter of 30nm, removing water in the boron trichloride raw material through the first-stage adsorption tower 2, wherein the working pressure of the first-stage adsorption tower is 0.4MPa, and the filler of the first-stage adsorption tower 2 is a 4A molecular sieve.
S2, introducing the boron trichloride treated by the S1 into a secondary adsorption tower 3 to remove phosgene in the boron trichloride, wherein the working pressure of the secondary adsorption tower 3 is 0.3MPa, and the filler of the secondary adsorption tower 3 is Mg-MOF-74.
S3, introducing boron trichloride treated in the step S2 into a crude product tank 4, wherein the crude product tank 4 is provided with a refrigerant and heating, introducing the refrigerant during collection to adjust the pressure of the crude product tank 4 to 0.05MPa, heating the crude product tank 4 to 0.6MPa after collecting to the liquid level of 3/4,
S4, introducing the boron trichloride treated by the step S3 into a primary rectifying tower 5, wherein the working pressure of the primary rectifying tower 5 is 0.55MPa, the operating temperature is 50 ℃, and the number of tower plates is 50;
s5, after the working pressure and the operating temperature of the primary rectifying tower 5 are stabilized for at least 3 hours, introducing the boron trichloride treated by the S4 into a secondary rectifying tower 6, wherein the working pressure of the secondary rectifying tower 6 is 0.45MPa, the operating temperature is 40 ℃, and the number of tower plates is 100;
S6, analyzing the boron trichloride extracted from the secondary rectifying tower, wherein the content of phosgene, chlorine, carbon monoxide, carbon dioxide, hydrogen chloride, dichlorosilane, trichlorosilane, silicon tetrachloride, nitrogen, oxygen and other impurities in the boron trichloride is 0.62ppm, and obtaining the boron trichloride with the purity of 99.99993 percent through the device.
Example 2:
The purification method of the boron trichloride, wherein the purity of the boron trichloride raw material is 95%, and raw material impurities comprise moisture, phosgene, chlorine, carbon monoxide, carbon dioxide, hydrogen chloride, dichlorosilane, trichlorosilane, silicon tetrachloride, nitrogen and oxygen, and the method comprises the following specific steps of:
S1, pressing the boron trichloride raw material in a raw material tank 1 into a first-stage adsorption tower 2, removing particles in the raw material through a filter 8 with the diameter of 3nm, removing water in the boron trichloride raw material through the first-stage adsorption tower 2, wherein the working pressure of the first-stage adsorption tower is 0.4MPa, and the filler of the first-stage adsorption tower 2 is a 4A molecular sieve.
S2, introducing the boron trichloride treated by the S1 into a secondary adsorption tower 3 to remove phosgene in the boron trichloride, wherein the working pressure of the secondary adsorption tower 3 is 0.3MPa, and the filler of the secondary adsorption tower 3 is Zn-MOF-74.
S3, introducing boron trichloride treated in the step S2 into a crude product tank 4, wherein the crude product tank 4 is provided with a refrigerant and heating, introducing the refrigerant during collection to adjust the pressure of the crude product tank 4 to 0MPa, heating the crude product tank 4 to 0.7MPa after collecting to the liquid level of 3/4,
S4, introducing the boron trichloride treated by the step S3 into a primary rectifying tower 5, wherein the working pressure of the primary rectifying tower 5 is 0.55MPa, the operating temperature is 55 ℃, and the number of tower plates is 60;
s5, after the working pressure and the operating temperature of the primary rectifying tower 5 are stabilized for at least 3 hours, introducing the boron trichloride treated by the S4 into a secondary rectifying tower 6, wherein the working pressure of the secondary rectifying tower 6 is 0.4MPa, the operating temperature is 45 ℃, and the number of tower plates is 85;
S6, analyzing the boron trichloride extracted from the secondary rectifying tower, wherein the content of phosgene, chlorine, carbon monoxide, carbon dioxide, hydrogen chloride, dichlorosilane, trichlorosilane, silicon tetrachloride, nitrogen, oxygen and other impurities in the boron trichloride is 0.45ppm, and the boron trichloride with the purity of 99.99995% is obtained through the device.
Example 3:
The purification method of the boron trichloride, wherein the purity of the boron trichloride raw material is 99%, and raw material impurities comprise phosgene, chlorine, carbon monoxide, carbon dioxide, hydrogen chloride, dichlorosilane, trichlorosilane, silicon tetrachloride, nitrogen and oxygen, and the method comprises the following specific steps:
S1, pressing a boron trichloride raw material in a raw material tank 1 into a first-stage adsorption tower 2, removing particles in the raw material through a filter 8 with the diameter of 10nm, removing water in the boron trichloride raw material through the first-stage adsorption tower 2, wherein the working pressure of the first-stage adsorption tower is 0.4MPa, and the filler of the first-stage adsorption tower 2 is a 4A molecular sieve.
S2, introducing the boron trichloride treated by the S1 into a secondary adsorption tower 3, and removing phosgene in the boron trichloride, wherein the working pressure of the secondary adsorption tower 3 is 0.3MPa, and the filler of the secondary adsorption tower 3 is 50wt% of Ni-MOF-74 and 50wt% of Co-MOF-74.
S3, introducing boron trichloride treated in the step S2 into a crude product tank 4, wherein the crude product tank 4 is provided with a refrigerant and heating, introducing the refrigerant during collection to adjust the pressure of the crude product tank 4 to 0.1MPa, heating the crude product tank 4 to 1.0MPa after collecting to the liquid level of 3/4,
S4, introducing the boron trichloride treated by the step S3 into a primary rectifying tower 5, wherein the working pressure of the primary rectifying tower 5 is 0.6MPa, the operating temperature is 60 ℃, and the number of tower plates is 70;
S5, after the working pressure and the operating temperature of the primary rectifying tower 5 are stabilized for at least 3 hours, introducing the boron trichloride treated by the S4 into a secondary rectifying tower 6, wherein the working pressure of the secondary rectifying tower 6 is 0.5MPa, the operating temperature is 50 ℃, and the number of tower plates is 70;
S6, analyzing the boron trichloride extracted from the secondary rectifying tower, wherein the content of phosgene, chlorine, carbon monoxide, carbon dioxide, hydrogen chloride, dichlorosilane, trichlorosilane, silicon tetrachloride, nitrogen, oxygen and other impurities in the boron trichloride is 0.31ppm, and the boron trichloride with the purity of 99.99996% is obtained through the device.
The foregoing is merely a preferred embodiment of the present application 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 application, which are intended to be comprehended within the scope of the present application.
Claims (10)
1. A method for purifying boron trichloride, comprising the steps of:
S1, pressing a boron trichloride raw material in a raw material tank (1) into a first-stage adsorption tower (2) after passing through a filter (8), removing particles in the raw material through the filter (8), and removing water in the boron trichloride raw material through the first-stage adsorption tower (2);
s2, introducing the boron trichloride treated by the S1 into a secondary adsorption tower (3) to remove phosgene in the boron trichloride;
s3, introducing the boron trichloride treated in the step S2 into a crude product tank (4) for collection, and boosting the pressure of the crude product tank (4) after the boron trichloride is collected to the liquid level of 3/4;
S4, introducing boron trichloride in the boosted crude product tank (4) into a first-stage rectifying tower (5);
s5, after the working pressure and the operating temperature of the primary rectifying tower (5) are stabilized for at least 3 hours, introducing the boron trichloride treated by the S4 into the secondary rectifying tower (6);
s6, after the working pressure and the operating temperature of the secondary rectifying tower (6) are stable for at least 3 hours, analyzing boron trichloride extracted by the secondary rectifying tower (6), collecting the boron trichloride to a finished product tank (7) after the boron trichloride is qualified, and returning the boron trichloride to the primary adsorption tower (2) after the boron trichloride is unqualified.
2. A method of purifying boron trichloride according to claim 1, characterized in that the filter (8) has a diameter size ranging from 3 to 30nm.
3. The purification method of boron trichloride according to claim 1, wherein the packing of the primary adsorption tower (2) is a 4A molecular sieve, the working pressure of the primary adsorption tower (2) is 0.4MPa, the packing of the secondary adsorption tower (3) is MOF-74 series, and the working pressure of the secondary adsorption tower (3) is 0.3MPa.
4. A method of purifying boron trichloride according to claim 3, wherein the MOF-74 series material is one or a combination of any of Mg-MOF-74, zn-MOF-74, ni-MOF-74, co-MOF-74, cu-MOF-74, mn-MOF-74 and Cr-MOF-74.
5. The purification method of boron trichloride according to claim 1, wherein the crude product tank (4) is equipped with a refrigerant refrigerating device and a heating device, refrigerant is introduced during collection to adjust the pressure of the crude product tank (4) to 0.0-0.1MPa, and the crude product tank (4) is heated to 0.6-1.0MPa after the crude product tank is collected to a certain liquid level;
the finished product tank (7) is provided with a refrigerant refrigerating device and a heating device, and refrigerant is introduced during collection to adjust the pressure of the finished product tank (7) to 0.0-0.1MPa.
6. The method for purifying boron trichloride according to claim 1, wherein the operating pressure of the primary rectifying column (5) is 0.5MPa to 0.6MPa, the operating temperature is 50 ℃ to 60 ℃ and the number of trays is 50 to 70.
7. The method for purifying boron trichloride according to claim 1, wherein the operating pressure of the secondary rectifying column (6) is 0.4MPa to 0.5MPa, the operating temperature is 40 ℃ to 50 ℃ and the number of trays is 70 to 100.
8. The purification method of boron trichloride according to claim 1, wherein the top discharge of the secondary rectifying tower (6) is returned to the primary adsorption tower (2) after being analyzed.
9. The method for purifying boron trichloride of claim 1, wherein the purity of the acceptable product is 6N.
10. The purification device of boron trichloride according to any one of claims 1 to 9, which comprises a raw material tank (1), a filter (8), a primary adsorption tower (2), a secondary adsorption tower (3), a crude product tank (4), a primary rectifying tower (5), a secondary rectifying tower (6) and a finished product tank (7) which are communicated in sequence;
The bottom of the primary rectifying tower (5) is connected with a first heater, the top of the primary rectifying tower is connected with a first condenser, the bottom of the secondary rectifying tower (6) is connected with a second heater, and the top of the secondary rectifying tower (6) is connected with a second condenser;
and the top discharge of the secondary rectifying tower (6) is communicated with the primary adsorption tower (2) through a valve.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410006338.1A CN118084000A (en) | 2024-01-03 | 2024-01-03 | Purification method and device of boron trichloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410006338.1A CN118084000A (en) | 2024-01-03 | 2024-01-03 | Purification method and device of boron trichloride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN118084000A true CN118084000A (en) | 2024-05-28 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202410006338.1A Pending CN118084000A (en) | 2024-01-03 | 2024-01-03 | Purification method and device of boron trichloride |
Country Status (1)
| Country | Link |
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| CN (1) | CN118084000A (en) |
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- 2024-01-03 CN CN202410006338.1A patent/CN118084000A/en active Pending
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